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P754: Metal Accounting

Code of Practice and Guidelines: Release 3

February 2007

© AMIRA International

AMIRA International Africa Registration No. 2002/011077/08


88 Studio Office Park, 5 Concourse Crescent, Lonehill, South Africa. Phone: +27 11 745 1522, Facsimile: +27 21 467
0021
Email: AMIRA@amira.com.au Website: www.amira.com.au
To the Sponsors of the AMIRA P754 Project
The third formal release of the Code of Practice for Metal Accounting, dated February
2007, is attached for your attention. Also attached is the third release of the
Guidelines Document, which supports the Code of Practice.

These documents have been prepared in consultation with representatives of the


sponsor companies, particularly those who serve on the Project Steering Committee.

Following the first release of these documents in October 2005, extensive feedback
and comments were received from Dr GJ Lyman, Sampling Consultant to Anglo
Platinum, which mainly affected the sections of the documents related to sampling,
and which were incorporated into Release 2 of the Code and Guidelines.

The content of Release 2 has undergone a comprehensive professional editing


process during 2006, while feedback and comments have been received from
several of the sponsors’ operating companies, as well as from a number of experts in
the field of sampling and of statistics. These have been incorporated into the
documents, where appropriate, and mainly affect the Guidelines.

Further contributions have also been received from the P754 Research Teams at the
Universities of Cape Town, Queensland, and Stellenbosch and these have assisted
the team preparing the Code and the Guidelines.

During the drafting of these documents, regular discussions were held with
representatives of the South African Accounting Profession and their suggestions
and comments have been incorporated.

On behalf of the members of the P754 Code Development Team, I would like to
express our sincere thanks to all those listed above for their help in compiling the
Code of Practice and the Guidelines.

This release is an update of Release 2 which was seen as a trial or ‘beta’ version of
what we hope will become a set of documents which can be applied throughout the
minerals industry to assist operating management in the design, installation and
operation of sound metal accounting systems, which will meet the requirements of
corporate governance. To achieve this, Release 3 of this Code of Practice and
Guidelines must be introduced and applied in the operating environment of
companies, so that any flaws in the documents can be identified and eliminated as
rapidly as possible.

In addition to the sponsors of P754, Release 3 will also be distributed to people who
have expressed interest in participating in the evaluation of the documents, and to a
wider group of potentially interested parties at workshops provisionally scheduled to
be held in Australia and South Africa during 2007. A further review and revision of
the documents is planned for the end of 2007, after which Release 4 is expected to
be distributed to a wider group of interested parties, including mining companies in
North America, during the first quarter of 2008.

Following the distribution of Release 4, it is hoped that sufficient interest in the


documents and support for them will have been generated to justify the
establishment of an international coordinating body, through the appropriate

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professional societies, to maintain the documents and incorporate further
improvements as they are identified, so that the Code of Practice and the Guidelines
can become living documents and can be accepted as a basis for Metal Accounting
in the global minerals industry.

We look forward to your feedback and comments, which should be addressed to Ms


Tess Chalk, AMIRA International Africa, at tess.chalk@amira.com.au

Peter Gaylard

Convenor, P754 Code Development Team

2007-02-19

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Code of Practice for Metal Accounting
Developed in terms of the AMIRA P754 Project:

Metal Accounting and Reconciliation

Preface to the Code on Metal Accounting


Historically, in the Mining and Metallurgical industry, the accounting for
metals/commodities across processing plants has not generally been performed at a
level required by currently acceptable corporate governance practices. A number of
factors have contributed to this, primarily a lack of knowledge and understanding of
the principles of mass balancing and metal accounting. However, other factors have
also played a major role; for example, the equipment required to achieve an
acceptable level of accountability is often a last minute addition to a new plant design
and as a result, it can be inadequately designed and installed. In addition, the
installed equipment is often poorly maintained and operated. Capacity and staffing of
laboratory facilities are also frequently insufficient to allow for the accurate and timely
reporting of metal accounting results.

These drawbacks, together with the need for metal accounting to be conducted to the
level of “financial accounting” standards with respect to auditability and transparency,
for example, have been recognised for some time. Following the symposium entitled
“Challenges in Metallurgical Accounting & Information Management” held in Cape
Town in August 2001 under the auspices of the SAIMM, several interested parties
held discussions on how the situation could be improved. The outcome of these
discussions was a proposal for a project to be coordinated by AMIRA International
entitled “P754 – Metal Accounting and Reconciliation” which was subsequently
accepted and sponsored by Anglo American, Anglo Platinum, BHP Billiton, Kumba
Resources and Rio Tinto. The objective of the project was to develop a Code of
Practice for Metal Accounting, which would be similar in concept to the JORC and
SAMREC Codes produced for the reporting of mineral resources and ore reserves.
At the same time, research projects were established at several universities in South
Africa and Australia, which, in collaboration with industry, will aim to provide solutions
to some of the more intractable aspects of metal accounting.

A team under the leadership of Professor Peter Gaylard, UCT, was commissioned in
August 2004 to develop the Code, which focuses on the need for all activities in the
areas of mass measurement, sampling, sample preparation and analysis to be
carried out accurately and with an acceptable level of precision. In addition,
wherever possible the Code recommends the use of International Standards as the
basis for all evaluation activities. Calculations and reports must be on a full “Check
in-Check out” basis and must be prepared in a completely transparent manner with
clearly defined audit trails. During its development, the Code has been discussed on
many occasions with representatives of the financial auditing profession, who have
offered many helpful suggestions on its content and who are in general agreement
with its aims.

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Although it is accepted that the Code will be a living document, it has now reached a
stage where it can be endorsed for use by the Industry. At the heart of the proposed
Code are the following ten Principles:

1 The metal accounting system must be based on accurate measurements of


mass and metal content. It must be based on a full Check in-Check out system
using the Best Practices as defined in this Code, to produce an on-going
metal/commodity balance for the operation. The system must be integrated
with management information systems, providing a one-way transfer of
information to these systems as required.

2 The system must be consistent and transparent and the source of all input data
to the system must be clear and understood by all users of the system. The
design and specification of the system must incorporate the outcomes of a risk
assessment of all aspects of the metal accounting process.

3 The accounting procedures must be well documented and user friendly for easy
application by plant personnel, to avoid the system becoming dependent on
one person, and must incorporate clear controls and audit trails. Calculation
procedures must be in line with the requirements set out in this Code and
consistent at all times with clear rules for handling the data.

4 The system must be subject to regular internal and external audits and reviews
as specified in the relevant sections of the Code to ensure compliance with all
aspects of the defined procedures. These reviews must include assessments
of the associated risks and recommendations for their mitigation, when the
agreed risk is exceeded.

5 Accounting results must be made available timeously, to meet operational


reporting needs, including the provision of information for other management
information systems, and to facilitate corrective action or investigation. A
detailed report must be issued on each investigation, together with
management’s response to rectify the problem. When completed, the plan and
resulting action must be signed-off by the Competent Person.

6 Where provisional data has to be used to meet reporting deadlines, such as at


month ends when analytical turn-around times could prevent the prompt issuing
of the monthly report, clear procedures and levels of authorisation for the
subsequent replacement of the provisional data with actual data must be
defined. Where rogue data is detected, such as incorrect data transfer or
identified malfunction of equipment, the procedures to be followed together with
the levels of authorisation must be in place.

7 The system must generate sufficient data to allow for data verification, the
handling of metal/commodity transfers, the reconciliation of metal/commodity
balances, and the measurement of accuracies and error detection, which
should not show any consistent bias. Measurement and computational
procedures must be free of a defined critical level of bias.

8 Target accuracies for the mass measurements and the sampling and analyses
must be identified for each input and output stream used for accounting

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purposes. The actual accuracies for metal recoveries, based on the actual
accuracies, as determined by statistical analysis of the raw data, achieved over
a company’s reporting period must be stated in the report to the Company’s
Audit Committee. Should these show a bias that the Company considers
material to its results, the fact must be reported to shareholders.

9 In-process inventory figures must be verified by physical stock-takes at


prescribed intervals, at least annually, and procedures and authority levels for
stock adjustments and the treatment of unaccounted losses or gains must be
clearly defined.

10 The metal accounting system must ensure that every effort is made to identify
any bias that may occur, as rapidly as possible and eliminate or reduce to an
acceptable level the source of bias from all measurement, sampling and
analytical procedures, when the source is identified.

It is possible that, in older metallurgical operations, it may be physically impossible or


very expensive to implement all of the above principles, in which case the Code
stipulates that an Exception Report must be submitted for approval by a Competent
Person as well as by management.

In addition to those already mentioned, the Code covers areas such as Safety,
Training, Data Management and Design of Metal Accounting Systems. Two further
very important sections cover the appointment of a Competent Person to coordinate
implementation of the Code and the requirements for internal and external audits of
the Metal Accounting system.

The recipients of the Code and its attachments should include independent Directors,
members of the Risk/Audit Committee, senior corporate and operational
management, project design staff (including outside contractors) and plant operation
and laboratory staff.

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Disclaimer
The attached Code, including its supporting Guidelines, (the “Code”) has been
developed by and on behalf of certain sponsor companies and organisations (the
“Sponsors”) pursuant to the AMIRA P754 Project on Metal Accounting and
Reconciliation. While it is the intention of AMIRA and the Sponsors that the Code (or
subsequent revisions of the Code) will ultimately achieve global and industry wide
acceptance as a code of best practice in relation to metal accounting, the following
points should be noted:

• The Code has not at this stage been formally adopted, for internal purposes,
by any of the Sponsors or by any industry associations and hence it is not
binding on any such companies, organisations, associations or on any
directors, officers, agents, employers, advisors or members thereof
• The Code has not been adopted by any legislative or regulatory bodies
(including any stock exchanges), nor has it been incorporated into the listing
or other rules of such exchanges
• The Code does not purport to be, nor should it be construed as constituting,
any form of legal or other standard in relation to metal accounting
• Neither AMIRA, nor the Sponsors nor any of their directors, officers, agents,
employees and advisors make any representation or warranty regarding, nor
shall they have any liability whatsoever in respect of any statement,
recommendation, advice, opinion or information contained in the Code
• To the extent that the Code is made available to third parties by or on behalf
of the Sponsors, such action (or any subsequent interactions) shall not be
construed as giving rise to any contractual relationship or any duty of care, of
whatsoever nature, between AMIRA, the Sponsors (and/or their directors,
officers, agents, employees or advisors) and such third parties.

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TABLE OF CONTENTS
Page

Preface to the Code on Metal Accounting iii

Disclaimer vi

TABLE OF CONTENTS vii

1 INTRODUCTION .................................................................................1
1.1 SAFETY AND HEALTH 2
1.2 PRINCIPLES OF METAL ACCOUNTING 2
1.3 STANDARDS 3
1.4 TRACEABILITY 3
1.5 ACCURACY AND PRECISION IN METAL ACCOUNTING 4
1.6 ERROR TYPES 4
1.7 METAL ACCOUNTING RISK 4
1.8 TRAINING 5
2 DATA MANAGEMENT........................................................................6
2.1 INTRODUCTION 6
2.2 DATA ACQUISITION / ENTRY 6
2.3 DATA DOCUMENTATION 6
3 MASS MEASUREMENT .....................................................................7
3.1 INTRODUCTION 7
3.2 ACCURACY AND PRECISION OF MASS MEASUREMENT 8
3.2.1 Scales / Weighing Equipment 8
3.2.2 Flow Meters 9
3.3 METHODS OF MEASURING MASS 9
4 SAMPLING........................................................................................ 11
4.1 INTRODUCTION 11
4.2 ACCURACY AND PRECISION OF THE SAMPLING SYSTEM 11
4.3 MULTI-STAGE SAMPLING SYSTEMS 12
4.4 SAMPLE STORAGE 12
4.5 SAMPLE LABELLING 12
5 SAMPLE PREPARATION AND ANALYSIS ..................................... 13
5.1 INTRODUCTION 13
5.2 SAMPLE PREPARATION 13
5.2.1 Moisture determination 13
5.2.2 Sample Reduction 13

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5.2.3 Sample Mixing 13
5.2.4 Sample Division 14
5.2.5 Sample Storage After Sample Preparation 14
5.3 ANALYSIS 14
6 STOCK-TAKES................................................................................. 15
7 METAL BALANCING........................................................................ 17
7.1 INTRODUCTION 17
7.2 THE METAL ACCOUNTING PROCESS 17
7.3 METAL BALANCING APPLICATIONS 19
7.3.1 Concentrators with minimal accumulation 19
7.3.2 Concentrators with intermediate accumulation 19
7.3.3 Coal treatment plants 19
7.3.4 Pyrometallurgical plants 19
7.3.5 Hydrometallurgical plants 20
7.3.6 Heap leaching 21
7.3.7 Bench scale, pilot and demonstration plants 22
7.4 MASS BALANCING FOR ENVIRONMENT AND HEALTH MONITORING 23
7.5 MINE TO PRODUCT BALANCING AND RECONCILIATION 23
8 REPORTING ..................................................................................... 24
9 SELECTION AND USE OF A COMPETENT PERSON .................... 25
10 DESIGN OF METAL ACCOUNTING SYSTEMS .............................. 26
11 METAL ACCOUNTING AUDITING RULES...................................... 27
11.1 INTRODUCTION 27
11.2 AUDIT TEAM AND ITS RESPONSIBILITY 27
11.3 METAL ACCOUNTING REVIEW 27
11.4 PHYSICAL AUDITS 27
CODE GLOSSARY 28

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1 INTRODUCTION
This Code document has been developed as one of the deliverables of the AMIRA
P754 Project on Metal Accounting and Reconciliation and it is supported by a Metal
Accounting Guidelines Document, to which are attached Appendices containing
glossaries of relevant technical terms, lists of references, and illustrative examples of
metal accounting procedures. The Guidelines Document is intended to serve as a
manual for plant operating and metal accounting personnel. Further deliverables of
the P754 project are the outcomes of site based research projects on metal
balancing and reconciliation, which will be incorporated in the Guidelines Document
as they become available.

Where words are highlighted in bold lettering in the Code, their definitions in terms of
Metal Accounting are included in the Glossary to this Code Document.

This document is intended to serve as a Metal Accounting Code of Practice, which


will become the provenance of suitable groups of industry organisations, as a way to
gain broad industry acceptance worldwide as the Industry Code for best practice in
metal accounting. It should also be regarded as a living document, which will be
revised through contributions from sponsoring companies, the related research
program and other initiatives.

Metal Accounting is defined as the system whereby selected process data (pertaining
to metals of economic interest), including mass measurement and analysis are
collected from various sources and transformed into a coherent report format that is
delivered in a timely fashion in order to meet specified reporting requirements.

A Metallurgical (Metal) balance involves the determination, through measurement,


analysis and computation, of the magnitude of each component of interest across an
entire process (Primary Accounting) or across each section of a process flow sheet
(Secondary Accounting). A metallurgical balance, which is suitable for reporting of
Metal Accounting, should be supplemented by defined uncertainties associated with
each determination. In terms of this Code, a metallurgical (metal) balance
encompasses metals, minerals or commodities of interest, which can also include
species which are measured and balanced for purposes of reporting on the
environmental compliance of an operation.

The ultimate purpose of the Code is to define the best practice for creating and
reconciling process metal balances, although it does not prescribe specific valuation
methods, as these will be dependent on the practices and policies of the company or
operation concerned.

The Code is based on a set of metal accounting principles, which are set out in detail
in Section 1.2. These incorporate the use of the Check in-Check out procedure for
metal balancing, as well as the use of Exception Reports for reporting all deviations
from the Code. These reports, in turn, have to be signed off by the Competent
Person before being submitted to the Audit Committee of the company for ratification.
The Competent Person is also required to approve the final design and installation of
the metal accounting system and to conduct routine audits of its operation.

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The Code document sets out principles for use and application by operating
management for obtaining credible figures, such as the methods to be used and their
bias and precision, and they should facilitate full disclosure of operational
performance, including losses in emissions, in line with requirements for triple bottom
line reporting in financial statements.

At present, the Code does not address metal accounting in mines and open cast
operations, as it takes the feed to metallurgical treatment plants as its starting point.
It is envisaged that this aspect will be addressed as the Code is developed. However,
mass measurement in stopes and ore blocks is discussed briefly.

1.1 SAFETY AND HEALTH


The safety and health of staff involved in Metallurgical Accounting activities must
always be of primary importance. Staff must, therefore, be well trained, provided with
the necessary personal protection equipment and be fully aware of the company’s
safety and health policies and procedures. In addition, access to equipment for
inspection, cleaning and maintenance must be safe, with the appropriate work
practices, lockouts and permissions in place.

1.2 PRINCIPLES OF METAL ACCOUNTING


The basic principles of metal accounting are summarised below:

1 The metal accounting system must be based on accurate measurements of


mass and metal content. It must be based on a full Check in-Check out system
using the Best Practices, as defined in this Code, to produce an on-going
metal/commodity balance for the operation. The system must be integrated
with management information systems, providing a one-way transfer of
information to these systems as required.

2 The accounting system must be consistent and transparent and the source of
all input data to the system must be clear and understood by all users. The
design and specification of the system must incorporate the outcomes of a risk
assessment of all aspects of the metal accounting process.

3 The accounting procedures must be well documented and user friendly for easy
application by plant personnel, to avoid the system becoming dependent on
one person, and must incorporate clear controls and audit trails. Calculation
procedures must be in line with the requirements set out in this Code and must
be consistent at all times with clear rules for handling the data.

4 The system must be subject to regular internal and external audits and reviews
as specified in the relevant sections of the Code, so as to ensure compliance
with all aspects of the defined procedures. These reviews must include
assessments of the associated risks and recommendations for their mitigation,
where the agreed risk is exceeded.

5 Accounting results must be made available timeously, to meet operational


reporting needs, including the provision of information for other management
information systems, and to facilitate corrective action or investigation. A

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detailed report must be issued on each investigation, together with
management’s response to rectify the problem. When completed, the plan and
resulting action must be signed off by the Competent Person.

6 Where provisional data has to be used to meet reporting deadlines, such as at


month ends when analytical turn-around times could prevent the prompt issuing
of the monthly report, clear procedures and levels of authorisation for the
subsequent replacement of the provisional data with actual data must be
defined. Where rogue data is detected, such as incorrect data transfer or
identified malfunctioning of equipment, the procedures to be followed together
with the levels of authorisation must be in place.

7 The system must generate sufficient data to allow for data verification, handling
of metal/commodity transfers, reconciliation of metal/commodity balances, and
measurement of accuracies and error detection, which should not show any
consistent bias. Measurement and computational procedures must be free of a
defined critical level of bias.

8 Target accuracies for the mass measurements and the sampling and analyses
must be identified for each input and output stream used for accounting
purposes. The actual accuracies for metal recoveries, based on the actual
accuracies, as determined by statistical analysis of the raw data, achieved over
a company’s reporting period must be stated in the report to the Company’s
Audit Committee. Should these show a bias which the Company considers
material to its results, the fact must be reported to shareholders.

9 In-process inventory figures must be verified by physical stock-takes at


prescribed intervals, at least annually, and procedures and authority levels for
stock adjustments and the treatment of unaccounted losses or gains must be
clearly defined.

10 The metal accounting system must ensure that every effort is made to identify
any bias which may occur as rapidly as possible and to eliminate or reduce to
an acceptable level the source of the bias from all measurement, sampling and
analytical procedures, once the source has been identified.

1.3 STANDARDS
Wherever possible, procedures used in Metal Accounting must be based on the
appropriate International or National Standards.

1.4 TRACEABILITY
In the areas of mass measurement and analysis, the aim must be to establish
traceability back to the relevant international standard units of mass, distance and
time.

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1.5 ACCURACY AND PRECISION IN METAL ACCOUNTING
All of the operations and equipment used to derive data for the reporting of Metal
Accounts, which include mass measurement, sampling, sample preparation and
analysis, must be designed and conducted to achieve an accurate result.

The actual accuracy of the independent operations involved in obtaining data for the
Metallurgical Accounts must be measured on at least an annual basis or, if the nature
of one of the measurement parameters changes, e.g. particle size of the process
stream, sampler design, analytical method etc. The precision of mass measurement,
sampling and analyses must be monitored on an on-going basis by a robust
statistical method and an investigation must be commenced when the monitoring
system indicates that the precision is outside the acceptable range. The overall
expected precision of the Metallurgical Accounts must be calculated from these
values and compared to the actual metal imbalance.

1.6 ERROR TYPES


Errors in measurement can be classified into three types:

• Random Errors
• Systematic Errors
• Illegitimate (Spurious) Errors
The value of the random errors must be minimised by careful operation and the
causes of systematic and illegitimate errors identified and eliminated.

1.7 METAL ACCOUNTING RISK


Any production operation is exposed to financial risk associated with its Metal
Accounting process to the extent that there is uncertainty in the evaluation of the
quantities of metal delivered to that operation and produced by it. In addition, there is
the risk to the reputation of a company and of negative market perceptions resulting
from major Metal Accounting discrepancies. One of the prime objectives in the
design of a Metal Accounting system is to enable an operation to quantify, manage,
and minimise the level of risk to which it could become exposed, through failures or
shortcomings in its Metal Accounting system. Each operation must conduct an initial
Risk Assessment of its entire Metal Accounting system, to establish and quantify the
risks. The design of a Metal Accounting system must take these risks into
consideration and set down procedures to be followed when accounting
discrepancies are identified.

The use of statistical analysis, and check measurements and analyses provides a
database, which becomes an essential component of the risk management process.
The other fundamental component of the risk management process is regular and
frequent management reviews, incorporating Risk Assessments, of the entire Metal
Accounting system, supported by both internal audits and external audits carried out
by the Competent Person.

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The main areas of risk to which an operation could be exposed in its Metal
Accounting system are:

• Misrepresenting the performance of the operation through incorrect weighing,


sampling or analytical procedures; inaccurate weighing or sampling
equipment; incorrect stockpile estimation; incorrect calculations or the use of
arbitrary calculation methods; poor control of accounting samples and the
utilisation of illegitimate or unacceptably biased data.
• Real losses of an unknown nature, such as theft of material, through failure to
identify and investigate accountability problems promptly.

1.8 TRAINING
There must be full training procedures available to staff in line with International and
National Standards together with appropriate sections of the Metal Accounting
Guidelines. The level of training and qualification requirements of staff will obviously
vary depending on their role in the accounting system.

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2 DATA MANAGEMENT

2.1 INTRODUCTION
The operation of a Metal Accounting System represents the accumulation and
evaluation of process data (e.g. mass measurements and analyses) from various
sources. The acquisition, processing and management of data require a substantial
portion of the effort associated with Metal Accounting. Efficient, secure and reliable
data management adds considerable value to the Metal Accounting System.

The goal of data management is to create data files from data obtained from various
plant sources in such a way as to prevent systematic and spurious error. Production
(e.g. mass measurement) and laboratory data (e.g. analyses) need to be integrated
to a single user interface to facilitate Metal Accounting. At the same time, however, it
is essential that those responsible for entering plant operating data, and those
responsible for entering analytical results into the system, are able to operate
independently of each other.

2.2 DATA ACQUISITION / ENTRY


There are a number of ways of acquiring or entering information for use in a Metal
Accounting System. Data may be acquired from various plant systems such as
SCADA, Plant Historians, LIMS systems, etc.

Manual entry of data to operator log sheets and transposition to spreadsheets is


common practice on some plants. Spreadsheets do not allow for controlled data
entry and they are easily corrupted. It is easy to inadvertently type over data, lose
track of records, duplicate and improperly enter data in a spreadsheet. Further to
this, the justification of formulae in spreadsheets often lacks clarity, and is not always
recorded with the spreadsheet. Because of this, the justification can get lost,
especially if the developer of the spreadsheet moves on, thereby making
spreadsheets vulnerable to error and unjustified computations. For these reasons
spreadsheets must be avoided as a method of data entry.

2.3 DATA DOCUMENTATION


Metal Accounting systems must include sufficient documentation of the data
(metadata) that is being utilised for the various calculations so as to provide a clearly
defined audit trail.

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3 MASS MEASUREMENT

3.1 INTRODUCTION
The overriding objective of mass measurement for Metal Accounting purposes is to
establish the mass of the particular material or component present at a specific time,
or the mass flow of that component over a defined time period, to a defined accuracy
suitable for mass balancing, using procedures that take account of Best Practices.
At the same time, the cost/benefit relationship, the difficulty of measuring and
sampling the process stream and the importance of the measurement to the Metal
Balance must also be taken into consideration.

In terms of mass measurement, accuracy may be defined in several different ways,


such as maximum percentage error of reading, or maximum percentage error at full
scale of the instrument or equipment. It is critical to ensure that the definition of the
levels of accuracy in supplier’s documentation or the literature is comparable with
those used in this Code and in the applicable Standards. A fundamental requirement
for all mass or volume measurements is traceability back to the accredited standards
used for calibration and certification.

Mass measurement can be classified into three areas:

• Those measurements necessary for Custody Transfer and Primary Metal


Accounting
• Measurements required for Secondary Metal Accounting, and management
control including intra company transfers and plant area performance, which
may also be used for cross checks on Primary Accounting. This also includes
those measurements necessary for environmental monitoring
• Measurements required for plant control only
This Code is concerned only with the requirements for the measurements related to
Primary Accounting. The requirements for accuracy of the measurement are the
most stringent for the first area above requiring certified (assized) weighing
equipment and the ability to establish the distribution of the random errors associated
with the measurements.

In all weigher and flow meter installations, it is essential that the selection, system
design, installation, operation, maintenance and calibration follow the applicable
standards and manufacturers’ recommendations, in order to achieve the accuracy
and precision levels quoted in Section 3.2, as well as those required by International
and National Standards and National Metrology Acts. All the data from the checks
and calibrations must be collected and stored to enable statistical analysis and
assessment, to establish if bias exists and to calculate the variance and likely error in
the value recorded.

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3.2 ACCURACY AND PRECISION OF MASS MEASUREMENT

3.2.1 Scales / Weighing Equipment


In the weighing industry, a scale is accurate if it has been properly calibrated, it
conforms to the applicable standard, and its performance is within the permitted
tolerances (or maximum permissible errors) for initial verification and in service.
Although the maximum tolerances specified in the Standards (such as NIST 44) may
suggest 95% confidence levels, this is not actually stated.

Accuracy is generally expressed in the industry in terms of “inaccuracy” or the


amount of error, and is quoted as ± x%, usually of the full-scale value, without
defining the confidence levels. The precisions quoted in this section are percentages
of full-scale value. Often the number quoted in literature is actually precision and not
accuracy. For further discussion see the Guidelines.

The figures quoted below are expected precisions in terms of a coefficient of


variation.

Static scales provide the most accurate and precise method of measuring mass and
must be the choice, where circumstances permit, for Custody Transfer and Primary
and Secondary Metal Accounting purposes.

Certified in-motion weighing is also a suitable choice for Primary Metal Accounting
but for rail transport only.

Certified electromechanical belt weighers must be the second choice for metal
accounting purposes after static scales, if static weighing is not feasible.

Providing proper installation, operation and calibration are adhered to, precisions
obtainable generally range between ± 0.05% to ± 0.2% for platform scales and
between ± 0.1% to ± 0.5% for weighbridges on gross load measurements. For
hopper/bin scales and gantry scales the equivalent figures are ± 0.1% to ± 0.25%
and ± 0.15% to ± 0.4% respectively.

For in-motion weighing, provided that the key principles of taring each truck or
hopper on each occasion and controlling the truck speed are followed, a precision of
± 0.5 % is feasible.

A precision of ± 0.5% should be possible for conveyor belt weighing on most


applications, providing all the guidelines for selection, design, installation, operation
and calibration are followed.

Nuclear belt weighers must not be used for Primary Metal Accounting but they can
be used for Secondary Metal Accounting if the material is homogeneous in size and
composition and the belt loading is uniform.

Mass measurement equipment will measure the wet weight, therefore, accurate
determination of the moisture content is essential.

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3.2.2 Flow Meters
The accuracy of flow meters can be expressed in three different ways:

• Percentage of span
• Percentage of a rate or reading
• Percentage of the upper range limit
The accuracies quoted below are those at 95% confidence levels.

The accuracy of electromagnetic flow meters, especially on slurries, is installation


specific. Typical accuracies are ± 0.2 to ± 1% of reading and ± 0.5% is attainable on
water or clean solutions if selection, design, installation, operation and calibration
follow the applicable standards and manufacturer’s recommendations. On slurries,
however, the accuracy can be much worse and their use for Primary Metal
Accounting in these cases is not recommended unless the use of static or belt
weighing is not possible.

Coriolis mass flow meters are capable of high accuracy, ± 0.2% of reading in certain
cases, but they only have limited application in the extractive industry, as they require
low fluid velocity and they are sensitive to the amount of entrained air.

Ultrasonic transit time meters have limited applicability for specific applications and
they can give an accuracy of 0.5 to 2% of the reading.

Momentum (impact) mass flow meters can be used for free flowing solids and they
are capable of achieving an accuracy of ± 1.0% of the reading.

Differential pressure type meters are not recommended for accounting


measurements, as there are too many cumulative sources of error.

All methods utilizing a volume or volume flow determination require the measurement
of the bulk density of the material in the stockpile/bin or of the specific gravity/relative
density of the slurry or liquid. This can be performed by nuclear (gamma) gauge, or
preferably by bulk or laboratory tests which are the best methods. In a few cases,
such as for fine coal stockpiles, a penetrometer may be used. The density
determination is often a cause of error in the mass measurement calculation.

3.3 METHODS OF MEASURING MASS


The various methods of measuring mass and volume, their advantages and
disadvantages, as well as the applicable standards for design, installation, calibration,
certification, operation and maintenance, and their suitability for use in Metal
Accounting, are described in the Guidelines Section 3.3. Certain of these methods
are prescribed for the various applications in Primary Accounting.

The mass may be static in a tank, bin or stockpile or flowing on a conveyor belt, in a
conduit or in an open channel, or it may be moving in railway or road trucks.
Methods for measuring volume and volume flow, density and moisture are also
covered in the Guidelines.

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Measurement of mass in stockpiles and process inventory is subject to the highest
level of uncertainty. Use should be made of parallel streams, and stocks must
periodically be reduced to zero. Specific procedures such as Draught Surveys may
contractually apply to the mass measurement of bulk commodities. Methods for
measuring mass in gaseous and liquid effluents are specialised and they are usually
defined in environmental legislation. Measurement of mass in stopes or ore blocks is
not covered, as it is outside the scope of this Code at present.

Certification is required for all Primary Accounting mass measurement instruments.


If after due assessment of the risk, certification is considered unwarranted subject to
an evaluation of the:
• costs/benefits
• company needs
• practical limitations.
Then, suitable in-house procedures must be drawn up and applied, for the calibration,
operation and maintenance of equipment. These procedures must be based on the
appropriate standards and legal requirements and an Exception Report to the Code
motivated and agreed.

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4 SAMPLING

4.1 INTRODUCTION
Correct sampling of a particulate material from a moving stream is achieved when
the expected number fraction of the particles in the sample is equal to the average
number fraction of the particles in the process stream during the time that it takes to
extract the sample increment. To achieve this objective, the sampler must be
correctly designed, installed and operated in accordance with sampling theory. This
issue is dealt with in the Guidelines. A mechanically correct sampler is unbiased.
Where possible, the correctness of the sampler and its freedom from a specified level
of bias should be confirmed by carrying out bias tests by the stopped belt method or
another suitable reference method of sampling.

The sampling from stockpiles and bins for accounting purposes must be avoided
because of the great difficulty in obtaining an accurate sample. The sampling of
other process streams/products must be carried out according to the available
International Standards.

4.2 ACCURACY AND PRECISION OF THE SAMPLING SYSTEM


A mechanically correct sampling system cannot be biased in the long run. The most
effective manner of ensuring that sampling systems are free of bias is to design them
to be mechanically correct under all circumstances (material types and range of
mass flow). If a sampling system cannot be designed in a manner that is
unequivocally mechanically correct, provision must be made to allow accurate bias
testing. If the nature of the flow being sampled changes, a sampler that is not
mechanically correct must be tested for bias on the new material type.

A correct sampling system can show a bias over a short period of time if the sampler
takes increments at fixed time intervals, and this interval is a multiple of the period of
a periodic variation in the mass flow or quality of the process stream. To eliminate
this effect, the sampler must be operated in a random stratified sampling mode.

Sampling systems should be designed to achieve a precision that has been


determined according to the requirements of the metal accounting system. To
accomplish such a design, the process stream should be studied to determine the
nature of the solids and liquids to be sampled and to determine the statistical
variability of the measurands with time. When the samples are to be used to provide
data to a metal accounting system, the sampling accuracy and the accuracy of all
subsequent sample preparation and analysis steps should be such that the overall
accuracy is what is genuinely needed in that system.

The only unequivocal method of establishing the precision of a sampling and sample
preparation system is to ensure that the sampling system can carry out inter-leaved
sampling.

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4.3 MULTI-STAGE SAMPLING SYSTEMS
In situations where, due to high mass flow rates of the process stream, or where the
required number of increments to achieve a desired sampling variance produces an
excessive sample mass, it is necessary to install a multi-stage sampling system. In
such a system there will be a number of sampling stages that will reduce the final
sample mass to a level that can be handled by the laboratory.

The design criteria for multi-stage sampling systems must include the following:

• Each sampling stage must employ a correctly designed mechanical sampler


• There must be a storage system between each stage capable of holding the
total increments from the previous stage
• The feed rate between stages must be such that at least 30 increments are
taken by the subsequent sampler
• If there is particle size reduction in the system, this must be done to minimise
additional sampling variance. The level of variance is dependent on the
heterogeneity of the material, which in turn determines the sampling constant.
Ideally, the variance must be established by experimentation on the material
concerned. In certain cases, as an interim measure, it is possible to use a
“Sample Safety Line” such as the one described by Gy, provided the
limitations of this approach are clearly understood.

4.4 SAMPLE STORAGE


Prior to delivery to a laboratory, samples must be stored in suitable sealed
containers, so that any change to their physical or chemical parameters is minimised.
This is especially important with regard to their moisture content.

4.5 SAMPLE LABELLING


All samples must be labelled in such a way that their unique identity is unambiguous,
using a system that can withstand normal handling.

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5 SAMPLE PREPARATION AND ANALYSIS

5.1 INTRODUCTION
All operations in sample preparation and analysis must be carried out to provide
unbiased data, with a known and acceptable precision and within a time frame that is
suitable for Metal Accounting purposes.

Cross-contamination of samples during sample preparation must always be guarded


against. Samples with known differences in concentration such as feeds, tails,
concentrates, mattes and slags must be prepared in separately enclosed areas using
dedicated equipment. With underground and geological samples, where large
variations of grade are unavoidable and unknown, it must be established that there is
minimal hold-up of material within the sample reduction equipment. Frequent
cleaning of this equipment may be necessary.

5.2 SAMPLE PREPARATION

5.2.1 Moisture determination


Moisture is defined as water which can be removed from the sample by drying to
constant mass at temperatures up to 105 oC, as water can be present in the material
in different forms including water of crystallisation.

It is important to ensure that samples for moisture determination are taken in a


manner that will ensure that the moisture in the sample is representative of the
material being weighed and that no evaporation can take place, or water ingress
occur, before the determination takes place. It is also very important to ensure that
any analysis is carried out on the sample that has been used for moisture
determination or, if a nominally identical sample is used, that an appropriate
correction be made to convert the analyses from an as-received to a dry basis, in
order that the analytical result can be related directly to the dry tonnes value.

5.2.2 Sample Reduction


Sample Reduction must be carried out in equipment that does not contaminate the
sample and in which dust losses are minimal. Sample Reduction ahead of Sample
Division must always be done to a particle size that is known to minimise additional
sampling variance.

5.2.3 Sample Mixing


Sample Mixing is unnecessary during sample preparation provided that Sample
Division is carried out using correctly designed rotating sample dividers (spinning
rifflers). If mixing is carried out it must be done in sealed mechanical systems.
Paper rolling must not be used, as it generally leads to segregation of the sample by
particle size or particle density.

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5.2.4 Sample Division
Sample Division refers to the process of sub-sampling a quantity of material that is
itself a sample, or a partial sample, from a lot of material. Sample division is always
accompanied by an increase in the uncertainty associated with the sample.

The increase in variance is given by the following equation:

⎡ 1 1 ⎤
∆σ 2 = a2 K s ⎢ - ⎥
⎣ Mss Ms ⎦

where: Ks = The sampling constant for the material

a = The sample assay

Mss = The mass of the sub-sample retained

Ms = The mass of the sample before division

Sample division should be carried out wherever possible using a rotary sample
divider (spinning riffler). This recommendation extends to the extraction of the
analytical aliquot from the mass of sub-sample pulverised in the previous preparation
step. The Incremental Division procedure is acceptable. Stationary rifflers must be
avoided.

5.2.5 Sample Storage After Sample Preparation


Samples must be stored in suitable sealed containers to prevent any physical or
chemical change and to minimise the possibility of cross-contamination. If the
storage period is to be greater than three months, storage under nitrogen should be
considered.

5.3 ANALYSIS
Analysis of samples for Metallurgical Accounting must be carried out using methods
that have been accredited to ISO 17025. It is likely that such methods will involve a
twin-stream (parallel analysis) procedure and they are performed using extensive QA
and QC systems and checks. The calibration of instruments should conform to best
practice and, where appropriate, it should comply with the requirements of VAM
document LGC/VAM/2003/032. It is expected that there will be frequent use of
certified reference materials and that an Umpire Laboratory will be used on a regular
basis.

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6 STOCK-TAKES
Physical stock-takes, the determination of the Plant Stocks and the total Process
Inventory are all integral to metal accounting. The calculation of the dry mass and
content of process inventory held in stockpiles, bins, tanks or other process vessels
is subject to a high degree of uncertainty, mainly due to the difficulty in obtaining a
representative bulk density and sample. It can also be difficult to make estimates of
the volume of material that comply with the standard of accuracy needed for
metallurgical accounting. The effort put into the estimation of a particular item of
stock within the plant should be dependent on the values of the contained balance
species relative to the total input of all species that are expected to be found in the
item of stock, taking due account of the accuracy with which the balance is to be
carried out. A great deal of reliance is placed by external financial auditors on
“setting the clock to zero”; i.e. a full stock-take at regular intervals.

The frequency with which stock-takes or audits of the plant operation are carried out
is a management decision. It will relate to the value of the plant throughput, the in-
process inventories relative to the expected profit at year-end, and the cost of
execution; however, stock-takes must be conducted on at least an annual basis.
Stock-takes may be performed more frequently for plant control and these require a
lesser degree of accuracy than those used in financial reporting. The latter stock-
takes must be performed in conjunction with the company’s auditors.

The cost of executing the stock-takes increases with the demand for accuracy of the
result. The level of financial risk associated with a particular strategy will determine
the final decision regarding stock-take frequency and accuracy. The costs incurred
should be offset against the benefits of faster access to more accurate information
relating to production performance and stock shortages or excesses. The overall
confidence level in the result of the stock-take must be established from the
uncertainties in the component measurements and it must be reported with the
results.

Having developed a stock-take policy, the procedure must be documented to ensure


a clear definition of roles and responsibilities leading to the rapid and effective
execution of the stock-take and the reporting of results. Procedures for handling
differences between book and measured stocks must be fully documented. Any
adjustments must be made only after the appropriate authorisation, as defined in this
Code and the Guidelines.

It is readily demonstrated that in-process stocks and draw-down or build-up of


stockpiles are likely to represent the largest uncertainties in a Metal Balance. The
most successful strategy for the elimination of these uncertainties is to use a policy of
building parallel stockpiles, one of which can be exhausted at the end of the
accounting period. If stocks are never exhausted, measurement uncertainties will
accumulate to a point where the balances will be essentially meaningless. The policy
of eliminating stockpiles on a regular basis must be built into the general processing
strategy.

In cases in which the in-process inventory has a value that is large compared to the
value of the net input for the accounting period, the accounting strategy must involve

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an operating policy, which permits the exhaustion of the in-process inventory
immediately prior to the stock-take, such as the use of the Bubble Method.

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7 METAL BALANCING

7.1 INTRODUCTION
Metal Accounting is critical for corporate governance in monitoring, checking and
improving performance and in identifying and quantifying losses and emissions. A
satisfactory metal balance provides a convincing demonstration that:

"What comes into the operation, less any internal accumulation, plus
any draw down from internal stock, is sufficiently similar, i.e. within
acceptable limits in mass and analysed components, to what goes
out as product(s), losses and rejects". (Check in-Check out)

Using the Check in-Check out system, all streams into and out of the Process or
Plant for which the balance is being performed, are measured, sampled and
analysed. In terms of this Code, this is the standard procedure to be adopted for
Metal Accounting in all operations, and all deviations from this approach must be
justified in an Exception Report approved by company management.

The accuracy for each component measured is quantified and the resulting accuracy
of the metal balance calculated and reported in order to determine whether it is within
the acceptable limits, as defined for the operation by the company’s management.

Applying the Check in-Check out system will normally show a difference between net
input and output, due to measurement, sampling and analytical uncertainties, and
this imbalance is treated as an unaccounted gain or loss. The handling of this
unaccounted quantity and techniques for the reconciliation of the data and the
detection of errors and bias are covered in the Code Guidelines (Section 7) with the
essential overriding principles that any procedure or adjustment must be transparent,
fully documented and approved. The primary purpose of the reconciliation
techniques is to assist in pinpointing problem areas, thereby leading to improvements
in applying the Check in-Check out system.

7.2 THE METAL ACCOUNTING PROCESS


Metal Accounting involves the recording, to accounting standards, of information
relating to the flow and transfer of materials and their contained metals, while the
term “to accounting standards” includes criteria such as accuracy, integrity, security
and auditability which must be met. In turn, auditability requires that all source data
must be traceable and all changes to the data must be authorised and recorded,
together with reasons for the change and they must be filed to provide an audit trail.
Metal Accounting is based on an accounting period (typically one month), which is
usually determined by company reporting requirements, but it could also be
determined by specific reporting requirements for the operation concerned. Primary
Accounting, the focus of this Code, relates to the balance across an entire plant;
whereas Secondary Accounting involves balances across sections of the plant or
individual processes. Secondary accounting, therefore, can be used to help identify
where process inventory is occurring, where time lags are involved, or where any
measurement problems exist, thereby improving Primary Accounting.

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For custody transfers of material from one operation to another, it is common for the
material to be weighed and sampled by both sender and receiver when the transfer
takes place between corporate entities, as each entity has a requirement to complete
its own metallurgical accounting process. Although the mass measurements,
sample(s) and analyses used for settlement purposes will be defined in the
commercial agreement covering the transfer. When the transfer takes place between
business units of the same corporate entity, the double weighing, sampling and
analysis (Home and Away) system presents opportunities to monitor mass
measurement, sampling and analysis variances and bias. If there is no detectable
bias, all results should preferably be used to arrive at the values used for metal
accounting. If a bias is detected, the source of the bias must be investigated
immediately and eliminated. Such a double check system is, however, expensive,
and the resources might be better spent ensuring that the sampling at a single point
is beyond reproach and that sample preparation and analysis is done to the highest
standard, incorporating both appropriate quality assurance and control procedures.

Evaluation involves activities, some technological and some statistical, concerned


with the technical quality of the accepted data and it normally involves the
comparison of two independent measurements of the same quantity.

Recovery and Accountability are separate but related parameters, the determination
of both being necessary for the efficient monitoring, over defined boundaries, of the
performance of metallurgical plants or processes, as well as for reliable forecasting
and planning.

Although other definitions for Recovery and Accountability exist, which are currently
used in the industry, as shown in the Guidelines for this Code (Section 7), the
definition in this Code is Actual Recovery, which is calculated on the basis of all
process inputs according to the formula:

Actual Recovery (%) = (sum of all useful or desired outputs) x 100


(sum of all inputs)

Accountability is defined by the following formula:

Accountability (%) = (sum of all outputs + stock and inventory change) x 100

(sum of all inputs)

This provides a check whether over time, inputs, outputs and stock changes
reconcile.

The day-to-day data collected from a metallurgical plant is rarely consistent and it will
usually contain redundant information. In general, any two methods of calculation
will yield different results and, therefore, many factors influence the selection of a
suitable metal accounting strategy. These factors are discussed in the Guidelines
and some practical strategies for different types of metallurgical operations are
indicated.

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7.3 METAL BALANCING APPLICATIONS

7.3.1 Concentrators with minimal accumulation


As there is no significant accumulation of, or change in, process inventory in this type
of concentrator, accountability is measured by comparing all outputs with all process
inputs over the accounting period, ignoring any change in Plant Stock or Process
Inventory.

Care must be taken to ensure that the balance is not compromised by recycle
streams and the return of plant spillage to the circuit, especially if these are of higher
or lower grade than the main stream.

Typically, in concentrators, it is possible to obtain reliable measurements of the feed


and concentrate masses, but it is usually more difficult to measure the mass of the
tailings stream. Thus, in some concentrator metal accounting balances, Check in-
Check out is not carried out and the masses of the feed and concentrates, together
with the analyses of the feed, products and tailings streams, are used applying the
two-product or three-product formulae. This practice must be motivated and
approved via an Exception Report.

7.3.2 Concentrators with intermediate accumulation


Where significant accumulation or changes in plant stocks or in-process inventory
occur, the determination of the concentrator accountability has to take this into
account as per the accountability formula.

The potential impact of the measurement of plant stocks and in-process inventory on
the overall metal balance has been discussed in Section 6.

7.3.3 Coal treatment plants


In the coal industry, the practice of metal/commodity accounting, on a full Check in-
Check out basis, is not rigorously practised, in the sense of tracking a valuable
component in the plant feed/ore to a final product containing an enhanced
concentration of that valuable component. However, there are stringent
requirements regarding the mass measurement, sampling, and chemical and sizing
analysis of coal products as contained in various International Standards (Guidelines
Appendix D.2.2.)

Operating performance is monitored through the determination of the Yield of


product coal from the ROM material fed to the plant.

7.3.4 Pyrometallurgical plants


Recovery and accountability for smelters and pyrometallurgical plants are calculated
using the same formulae as shown in Section 7.2. For Check in-Check out, all input
and output streams around the plant must be measured and sampled leading to the
calculation of the material balance closure errors for the various species. These
balance closure errors reflect the material that is unaccounted. However, dust and
gas losses are normally subject to a high level of uncertainty and slag quantities are
often not accurately measured, thus Check in-Check out cannot be carried out for

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species affected by such losses and lack of measurement. Slags are not
homogeneous; they may have metal or alloy inclusions and they may contain varying
amounts of moisture, especially in the case of water-granulated slags. Fortunately,
the metal content in gases, dusts and slags is usually a small proportion of the feed
and the effect of omissions on the balance less significant. The amount of effort put
into improving the accuracy of measurement of dust and slag losses is dependent on
their magnitude and value, the risk potential and the requirements for environmental
reporting. However, it is recommended that furnace slag be weighed before disposal
or recycling.

Smelters represent a challenge in terms of metal accounting because of the difficulty


in measuring in-process inventories, intermediates and recycles, which are often
significant, including material from ladles and refractory repairs and metal/alloy build
up in furnaces. Furthermore, the materials in streams around furnaces and
converters are coarse, highly heterogeneous, variable in grade and may be molten.
They are, therefore, among the most difficult materials to sample. Nevertheless, the
accounting system must either treat these materials as in-process stock or it must
recycle them out and back into the process on a Check in-Check out basis.

7.3.5 Hydrometallurgical plants


Hydrometallurgical plants are usually relatively complicated, with multiple stages,
many circuits for purification and upgrading and several recycle streams. In addition,
Metal Accounting is often required for more components than in the earlier stages of
processing; these components include multiple products, residues, impurities,
reagents and effluents.

As process streams can be made up of either, or both, solids and liquids (organic
and/or aqueous), with both containing significant quantities of metals, the Metal
Accounting system for such plants must make adequate provision for the sampling
and mass measurement of all the components of each feed and output stream and it
must allow for the measurement and assessment of continuous recycle streams and
of process spillage, which may occur on a periodic basis.

Check in-Check out is essential for the feed and product streams including liquid and
gaseous effluents. The precise measurement for effluents is difficult but, usually, the
mass content of these streams is relatively small. Mass balancing of the individual
process steps and circuits (Secondary Accounting) is important for monitoring
process performance and it can provide checks on the Primary Accounting.

Hydrometallurgical plants usually have a significant process inventory in the form of


metals in solutions and in solids, including that in solvent extraction/electrowinning
circuits. Estimation of this inventory is complicated by the changing metal contents of
the solid and liquid phases as they progress through the plant. Estimation has to
incorporate tank level measurements, slurry relative densities as well as solution and
solids analyses at each stage of the process. In plants treating high value metals,
the process inventory estimate should be verified at prescribed intervals by physical
stock-takes, using procedures such as the bubble method, to reduce the probability
of major stock write-offs caused by undetected errors in the routine accounting
system.

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Hydrometallurgical plants are subject to losses of valuable materials in effluents and
they also normally generate various solid residues, which will contain some metal
values in both solid and solution. Besides the valuable constituents, it is necessary
to measure, account for, and report on various impurities and pollutants to ensure
conformity with environmental regulations.

7.3.6 Heap leaching


The heterogeneous (two-phase), non-steady state nature of Dump and Heap
leaching, together with a protracted leach cycle (several months) and the
consequent large process inventory all complicate metal balancing. The large
inventory also means that the effect of input or other changes is not readily apparent
and can be subject to long delays. However, the material treated is often of low
grade/value and high mass, and this must considered when assessing the cost
effectiveness of the Metal Balance methodology.

Further to this, the fact that the process inventory includes unleached, partially
leached, and fully leached ore, as well as solution with varying metal contents, and
that a significant proportion of the metal is not recoverable, raises issues that are not
encountered in other processes. The main concerns are the inventory of metal in the
leach solution and the determination and prediction of the recoverable metal in the
feed material. Often the Check in-Check out process cannot be used, especially for
Dump Leaching, as the mass and analysis of the dump is not known to a sufficient
degree of accuracy and it is impractical or not cost effective to measure the metal
remaining in the heap independently at the end of the accounting period. The metal
remaining in the heap is then determined by subtracting the quantity that has leached
into solution from the original estimate of what was deposited on the pad. If this
practice is utilised it must be approved by means of an Exception Report.

The principles in this Code thus apply to Heap Leaching only, as they are not
possible to achieve for most Dump Leaching operations.

Feed material must be weighed, sampled and analysed according to the Code and
the material must be tracked to the specific pile or pad. Drained pregnant solution
from each heap and the barren solution returned as irrigation to the heaps must be
accurately measured by suitable flow meters and sampled for analysis.
Reconciliation of these flows is important in order to provide a calculation of the
solution inventory in the leach piles, the metal extraction from all the heaps/modules
under irrigation and the total plant production. To perform this reconciliation requires
estimates to be made of the amount of rainfall, evaporation and the solution content
of each abandoned heap. Rainfall and evaporation must be based on actual site
measurements over the accounting period. The solution content of operating,
abandoned and resting heaps must be periodically established by test work, although
standard figures based on experience are often used. The metal content in the
solution in the heaps is normally the largest proportion of the total solution inventory
and it is usually equivalent to several months’ production.

However, the metal accounting is complicated further by the fact that a significant
proportion of the metal is not recoverable. Thus, it is common practice for process
control, to utilise the recoverable metal placed on the heap, rather than total metal,
for mass balance and performance calculations. If recoverable metal, as opposed to

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total metal, is being used for metal accounting, this must be approved by means of
an Exception Report. The recoverable metal in the specific material placed on the
heap must be determined by suitable laboratory tests on representative samples, for
example, using rolling bottle or shake tests, or pilot-scale column tests. These
values are adjusted by factors, based on experience with older heaps, to reflect the
predicted performance of an operating heap. The procedures and methodology for
performing these tests and calculations must be rigorously designed, documented
and monitored. Thus, the balance will reconcile the output metal in solution with the
inputted recoverable metal and it will further give the recoverable metal still in the
heap in both solid and solution forms.

To achieve a Check in-Check out balance, when a particular pile/heap has reached
the end of its life after leaching and elution has been completed, a closing balance
must be performed and the heap sampled to check the amount of total and
recoverable metal remaining. If the heap is to be left in place, this sampling should
preferably be performed by mechanical drill/augur or sonic drilling. If it is to be
moved, it must be sampled conventionally as it is moved. The metal that was not
recovered must be removed from the plant inventory when a heap is abandoned.

Sampling of heaps is subject to a high level of inaccuracy and due cognisance of this
must be taken in the use of the information generated for stock evaluation and for
use in predicting future performance.

The metal balancing from the output leach solution through the purifying and refining
steps to metal product is similar to that for Hydrometallurgical processes. General
practice is to calculate the recovery of the metal finally produced, after the
purifying/refining process, as a percentage of the metal placed on the heaps.

7.3.7 Bench scale, pilot and demonstration plants


Metal Accounting for pilot plants must embody all the principles covered in other
sections of this Code. The design and operation of the plant must allow for suitable
equipment and procedures, in line with this Code, for mass measurement, sampling
and analysis that will ensure that meaningful results can be obtained to give metal
balances to a defined accuracy, in order to facilitate the decision process. Operating
and sampling manuals are required.

• All input and output streams must be accounted for, i.e. Check in-Check out
• Accountability must be better than 100% (± 5% at 95% confidence levels) for
the product metals and 100% (±10%) for impurities, for the results to be
utilised for economic and process decisions
• As quantities are much smaller than a full-scale plant, static weighing on
certified weighers only must be used to establish feed and product weights
• Samples are a larger proportion of the process flows than in a full scale plant
and the mass and metal content of the samples must be included in the metal
balances as part of the Check in-Check out
• Similarly, spillage must be collected, weighed, analysed, and accounted for in
the balance at the appropriate stage. It should not be returned to the circuit
as it causes process disturbances. Spillage should be kept to a minimum

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• Effluents must be collected, accurately weighed and sampled
• Appropriate metal balancing methods must be used to calculate plant
performance
The entire sampling frequency and plan must be statistically designed to yield
meaningful results allowing for the fact that planned variations in operating conditions
will occur and that performance of individual process steps is required.

7.4 MASS BALANCING FOR ENVIRONMENT AND HEALTH MONITORING


For metal balance purposes, measurement of streams from operating plants only is
relevant. However, measurement and quantification of any dissolution of heavy
metals and other contaminants (such as Acid Mine Drainage) and percolation of
critical compounds into aquifers or watercourses, or gases emitted and dust blown
from slag and tailings dumps is also necessary for corporate governance purposes.

Methods of measurement, sampling, and analysis are defined by organisations such


as the Environmental Protection Agency and the National Institute for Occupational
Safety and Health in the USA, the World Health Organisation and other international
or national bodies as well as in national Air Quality and Water Quality Acts,
regulations and other legislation. Companies must adhere to the appropriate
regulations and guidelines and/or approved worldwide standards.

7.5 MINE TO PRODUCT BALANCING AND RECONCILIATION


A common terminology used, especially in the case of precious metals, for assessing
operating performance, is the ‘call’ system, in terms of which the amount of metal
that is produced as final metal and in the residues/tailings is compared to the quantity
delivered to the plant in the plant feed. This gives the plant call factor, which is
usually expressed as a percentage, and it is a measure of the accountability.

In the same way, the measured mass of metal in the ore delivered to the shaft, or the
ore dumping point, from the mining operations is compared with the estimated metal
content in the ore mined, as determined by sampling and surveying, to give the shaft
(or mine section) call factor, also expressed as a percentage. The combined plant
and shaft call factors give the mine call factor for the operation. Typically, these call
factors are calculated monthly and they form a useful means of monitoring
discrepancies between the expected and actual mine output.

However, the reconciliation of Metal Accounting back to stopes or ore blocks is


outside the scope of this Code at present.

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8 REPORTING
The Metal Accounting system must generate suitable reports, over various time
frames and accounting periods, to provide a Metal Balance of the desired
constituents timeously to Plant Management and to the Financial Accountants. The
report must highlight inconsistencies, problem areas, and indicate the confidence
levels for the reported data.

The report must include tonnage and analysis figures for all metal accounting
streams, and often a comparison of performance figures against key performance
indicators, and variance from the operating budget or business plan.

The report must contain sufficient information to assist in diagnosing plant operating
problems and for future production planning and project evaluation.

To meet the above objectives, the report must be compiled by adequately trained
personnel and it must use data which has been subjected to the minimum number of
manual entries, with clear traceability to the sources of all inputs. Compilation of the
report must be via the use of approved metal balancing procedures and no data may
be adjusted without written authorisation from the responsible person. The report
should also comply with International Auditing Standards as set out in IAS 2 and it
must be signed off by a Metal Accounting Committee, or another suitable authority,
for subsequent approval by the Audit Committee of the Company’s Board of
Directors.

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9 SELECTION AND USE OF A COMPETENT PERSON
A Competent Person, for the purposes of this Code, must be a member of the
relevant local professional registration authority, or any other statutory local or
international body that is recognised by the relevant Code administrators, and the
person should have a minimum of five years experience relevant to the type of metal
or mineral under consideration and to the type of operation involved.

The Competent Person must:

• be formally appointed by the management of the company or the operation


concerned to recommend standards for the setting-up and auditing of Metal
Accounting reporting systems
• accept responsibility for the final approval of the design of the Metal
Accounting systems
• be responsible for auditing the system once it has been installed, to assess
compliance with the design specifications
• conduct periodic reviews and audits of the system, at pre-determined
intervals, to ensure continued compliance and, as required, to investigate
problems which may occur
• submit reports to management in regard to the compliance of the system and
shall monitor the action plans periodically produced to remedy faults
The Competent Person must be independent from the operation concerned.

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10 DESIGN OF METAL ACCOUNTING SYSTEMS
The specification of the metal accounting system must be based on a study that has
the objective of quantifying the impact of the accuracy of process stream and process
stock measurement on the accuracy of the overall metal balances. Ideally the study
will estimate the probability distributions of the critical balance estimates, to permit a
full view of the financial risks associated with the balances.

The design and specification of the system must include the definition of all risks or
consequences of a degradation of the accuracy of the metal/commodity balance
process and it must specify the means by which these risks can be quantified.

The metal accounting system must comply with this Code and it must include the
following:

• A system for data acquisition and management


• An appropriate metal balancing methodology
• Reporting intervals, dates and timing, as well as reporting rules and
procedures
• Characterisation of the process streams involved in the balance, including the
nominal mass flows of balance species, heterogeneity of the solids to be
sampled from the stream and usual levels of process variability
• Sample equipment, sampling frequency, sample preparation procedures,
expected sampling and preparation accuracy and analyses required, as well
as cross-references to the required analytical procedures and the accuracy of
those analytical procedures
• Methods of monitoring the data streams of analytical results that will ensure
that the target sampling, preparation and analysis variances are maintained
• The quality control and assurance systems of all areas of metal accounting
must be included in the accounting system documentation
• Mass measurement points, type of measuring device and accuracy required
• Levels of authority for approval of the data and, where necessary, for
handling and approving changes to the data
• Accounting battery limits
• Stock-take procedures and frequencies
The design of the accounting system must form part of the design scope for new
plants and it must include careful identification of the mass measurement and
sampling points required to enable a reliable metal balance to be determined; it must
also pay careful attention to the detail of their installation, calibration, maintenance
and routine operation.

Where existing plants do not meet the requirements of this Code, either steps must
be taken to comply with these requirements, or non-compliance must be motivated
and approved via an Exception Report.

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11 METAL ACCOUNTING AUDITING RULES

11.1 INTRODUCTION
A company must have metal accounting rules and a procedure for auditing
compliance with these. These rules are primarily technical to provide management
information and to promote good Corporate Governance but they must also provide
the quantities and the reconciliation necessary for the financial reports.

11.2 AUDIT TEAM AND ITS RESPONSIBILITY


A team to audit the metal accounting system must be established, including a
financial auditor and, periodically, the Competent Person.

The responsibilities of the team are to:

• obtain a fair and soundly based analysis of the Metal Accounts


• witness stock-takes, on at least an annual basis
• verify mass flow measurements and analytical results
• assess the accuracy, precision and reconciliation of metal accounting data
• report to suit the company’s reporting period
• identify and advise on areas that are inadequate and recommend actions
• provide a support structure to the Competent Person

11.3 METAL ACCOUNTING REVIEW


On at least an annual basis, the metal accounting system methodology must be
reviewed by a team of suitably experienced staff, to ensure that it is still fulfilling its
requirements. Should this review lead to recommendations for changes to the
existing system, these must be approved by the Competent Person, prior to
incorporation in the system.

11.4 PHYSICAL AUDITS


A series of physical audits must be implemented to ensure that all aspects of the
metal accounting chain are operating as specified. Obviously, the auditing of
problem areas must be scheduled at a frequency to enable the problem to be
positively identified and eliminated.

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CODE GLOSSARY
Accountability – The ratio of the total output of a plant, or section of a plant, for a
given material balance species (element or compound), to its total input, normally
expressed as a percentage.

Accounting Period – The period in which a company would normally report its
financial results to the market. For example in the USA this is quarterly, while in
many other financial markets the requirement is bi-annually.

Accounting Standards – The financial accounting standards required by the


relevant regulatory authorities including Stock Exchanges.

Accuracy – A measurement is accurate if it, or the average of a number of


measurements, is close to the true value. In metallurgical operations this true value
is unknown. In addition, there is often misunderstanding between the terms accuracy
and precision, which is the measure of the spread of a number of measurements
around their mean value. For these reasons it has been decided to adopt the
following definition for accuracy, which incorporates the concept of precision, and it is
based on that given in ISO 3534-1:1993.

A measurement that is accurate is one that is free of bias and it has a dispersion
(standard deviation) that is lower than a defined dispersion or indeed a probability
density of a particular nature. The level of dispersion or the nature of the probability
density is defined with the purpose of separating measurements that are entirely fit
for a particular purpose or use from those that are not.

Acid Mine (Rock) Drainage – The low pH effluent which seeps from waste rock, ore
dumps or stockpiles of materials which have an insufficient capacity to neutralise the
acidic products, containing the dissolution products of minerals.

Actual Recovery – The sum of all useful or desired outputs from a process, divided
by the sum of all inputs to that process, expressed as a percentage.

Analyte – The component of a material whose concentration is determined by


chemical analysis.

Auditability – A user-oriented quality requirement specifying the degree to which an


application shall keep sufficient records to support a financial or technical audit.

Audit Trails – In metal accounting, an audit trail is a sequence of paperwork/data


entries that validates or invalidates metal accounting entries. Many metal accounting
entries are based on those made to computers and the term could also be used for
an electronic or paper log used to track computer activity.

Barren Solution (Tails Solution) – The discard solution from a metal recovery
process.

Battery Limits – The boundaries of a metal accounting system, across which all
inputs to and outputs from that system are measured and balanced.

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Best Practical Means – The most precise method of performing a measurement
taking into account the risk, degree of importance, cost and practicality for the stream
and variable being measured.

Best Practices – The most accurate method of performing a measurement with the
information and equipment available at that time.

Bias – Bias is the difference between the mean result of one or more measurements
and the true value of the quantity being measured. It also can be seen as a
consistent difference between two, or more, measuring systems. (e.g. sender’s and
receiver’s weights, the analysis of the same sample by two laboratories etc.)

Bubble Method – A method whereby the flow of material through a process plant is
interrupted to allow for equipment to be emptied in series to facilitate stock-takes
(normally applied to high value materials in the latter stages of processing).

Bulk Density – The density of a granular material normally stored in a bin, other
container or stockpile, defined as the mass of the material divided by the volume
occupied by the material (including the space between the particles).

Calibration Test (weighers) – A test, using known weights and forces to load a
scale, in order to determine the performance and operating tolerance compared to
standard values.

Certification (Test) – A calibration of a scale or flow meter in terms of accepted


standards defined by the relevant government authority to permit its use for trade
purposes and custody transfer.

Certified Weight – A weight, which has been certified by the relevant national body,
or an agent authorised by that body, to have a mass within a defined tolerance, to be
used for certifying weighing instruments.

Check in-Check out System – The system whereby all streams into and out of the
Process or Plant, for which the balance is being performed, are measured, sampled
and analysed.

Closure Errors – The difference between the inputs and outputs for a complete
metal balance (that is Check In-Check Out) over a plant or process, including
inventory and stock changes, over a prescribed period, and zero.

Coefficient of Variation – The quotient of the standard deviation and the mean
value of a measurement, expressed as a percentage.

Competent Person – A person with suitable qualifications and experience to make


recommendations for the design and to undertake reviews of the performance of the
Metal Accounting system and Balance.

Coriolis mass flow meter – A device consisting of a flow sensor and a transmitter
which primarily measures the mass flow by means of the interaction between a
flowing fluid and the oscillation of a tube or tubes; it may also provide measurements
of the density and the process temperature of the fluid.

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Corporate Governance – Is concerned with holding the balance between economic
and social goals and between individual and communal goals. The corporate
governance framework exists to encourage the efficient use of resources and equally
to require accountability for the stewardship of those resources. The aim is to align
as nearly as possible the interests of individuals, corporations and society.

Custody Transfer – The transfer of risk and/or ownership of a material from one
party to a second party. This includes ore from a mine to a processing plant,
intermediate products such as concentrate and matte from one plant to another, both
in-house and inter-company and waste products for sale or safe disposal, as well as
final products.

Data – In a metal balancing context it is almost always a numerical measurement.

Differential Pressure – The difference between the static pressures measured at


the wall pressure tappings, one of which is on the upstream side and the other on the
downstream side (or in the throat for a Venturi tube) of a primary device inserted in a
straight pipe through which flow occurs, when any difference in height between the
upstream and downstream tappings has been taken into account.

Division – The process of decreasing sample mass (without modification of the


particle size of the constituent pieces) whereby one or more representative parts of
the sample are retained. (AS 4433.2 – 1997)

Draught Survey – A mass measurement technique that is based on converting a


difference between a vessel’s displacement under different loads into a mass on the
basis of its draught tables while taking into account the density and temperature of
the water and ballast, and changes in ballast and supplies

Dump Leaching – Normally refers to a process whereby metals are extracted by


"heaping" uncrushed/broken Run of Mine ore on sloping impermeable pads (with
suitable low cost drainage of the leach solutions) and spraying the heaps with a
lixiviant, which dissolves the metal content. Sometimes the process is carried out
utilising low-grade ore which was previously stockpiled, as treatment through the
normal process route was uneconomic. Often the lixiviant used is the barren solution
from other primary leach operations. The metal-laden solution is collected for metal
recovery.

Electromagnetic flow meter – A flow meter, which creates a magnetic field


perpendicular to the flow, thereby enabling the flow rate to be deduced from the
induced electromotive force produced by the motion of a conducting fluid in the
magnetic field.

Electromechanical Belt Scale/Weigher – A mass measurement device whereby a


loaded belt is continuously weighed by mechanical means (load cells, levers) and the
measurement converted into an electronic signal that can be integrated (totalised)
and recorded.

Evaluation – The process by which the data required for Metal Accounting is
acquired.

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Exception Report – A report generated, in terms of this Code, whereby each non-
compliance with the requirements of this Code is motivated and approved.

Gantry scale – A scale where the load measuring elements are attached to a gantry
crane normally used for loading or offloading materials in bulk.

Heap Leaching – Normally refers to the leaching of ores that have been crushed (to
an economic size) prior to placement on an impermeable pad on which suitable
drainage lines have been placed for the collection of lixiviant that has been
percolated through the crushed and prepared ore. The crush size selected may vary
considerably but typically it ranges between 12 and 50 mm.

Heterogeneity – Is a measure of the dispersion of minerals/metals of interest within


a quantity of material, in terms of mass or time.

Home and Away System (Double Sampling and Analysis System) – A system
where batches/lots are weighed and sampled by both the sender and receiver. Data
from the analysis of the samples can be statistically analysed to establish the
presence of biases in the sampling and/or analytical processes. In the “Half Home
and Away System” samples from even numbered batches of material are analysed
by the sampling sites laboratory (i.e. the sender’s sample at the sender’s laboratory
and receiver’s sample at the receiver’s laboratory) and odd numbered batches are
analysed at the other laboratory (i.e. the sender’s sample at the receiver’s laboratory
and receiver’s sample at the sender’s laboratory). Statistical analysis of the data can
establish the level of bias in either the sampling or the analytical procedures.

Hopper Scale – A scale designed for the weighing of granular materials in bulk,
whose load-receiving element is a self-cleaning hopper with an outlet gate.

Illegitimate Errors (Spurious) – The error which invalidates a measurement. They


generally have a single cause such as the incorrect reading of one or more
significant digits or the malfunction of instruments.

In-motion weighing – The weighing of objects that are in-motion. Usually applied to
rail or road trucks.

In-process Inventory – The quantity of material contained in a process plant


through the various stages from the initial feed to the plant to the production of
product(s) from the plant. It does not include stocks of feed material or products
which are defined as Plant Stocks.

Inter-leaved Sampling – To carry out interleaved sampling, a sampling system must


be capable of taking increments at twice the usual rate. Odd-numbered increments
are collected into one sample and the even-numbered ones are collected into a
second sample over the sampling period of interest. Both samples are, at the end of
the sampling period, nominally identical. If they are both separately prepared and
analysed in the same way, the difference between the results is an indication of the
precision of sampling. A substantial number of results from interleaved pairs of
samples can be accumulated over a period of time to arrive at a good estimate of the
average sampling precision. It is also possible to draw certain conclusions regarding
the distribution of the assay uncertainties.

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International Unit of Mass – This is defined as the kilogram. The definitive standard
weight is held at the International Bureau of Weights and Measures in France, which
is also responsible for certifying National standards such as the National Prototype
Kilogram.

LIMS – Acronym for Laboratory Information Management System, a computer


system for gathering and analysing laboratory information. These systems are used
for:

• Automatic data collection. The LIMS may be interfaced directly to the


laboratory instruments, offering rapid data collection, while eliminating the risk
of transcription errors.
• Provision of electronic records of laboratory results. Electronic records
offer many benefits, such as the ability to link data together, search, retrieve
and report rapidly and backup and disseminate data easily through an
operation.
• Provision of a structured repository for laboratory data
Mass Balancing – The determination through measurement, analysis and
computation of the magnitude of each component of interest across an entire plant
(Primary Accounting), or across each section of a process flow sheet (Secondary
Accounting).

Materiality – It is what affects business decisions at the top level of management. It


is not a formal defined value but it should be determined by senior management for
each company and/or operation. For metal accounting, a measurement for a
process flow or in-process inventory may be regarded as material if:

• the metal content is significant in value and/or


• the content is regarded as important with respect to the company’s or
operation’s risk profile, public perceptions or reputation and/or
• it will reflect on the balance sheet and financial statements
Material-run (bulk) Test – A method of calibrating a belt scale whereby a known
weight of the material (either pre or post weighed on a test scale) being weighed is
passed on the conveyor through the mass detection system.

Measurand – The specific quantity subject to measurement.

Mechanically Correct Sampling – Correct sampling of a particulate material from a


moving stream is achieved when the expected number fraction of the particles in the
sample is equal to the average number fraction of the particles in the process stream
during the time that it takes to extract the sample increment. To achieve this
objective, the sampler must be correctly designed and operated. A sampler that is
mechanically correct is unbiased. Where possible, the correctness of the sampler
and its freedom from a specified level of bias should be confirmed by carrying out
bias tests by the stopped belt method or other suitable reference method of sampling.

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Metadata – The term used to describe data about data. It describes who collects the
data, what the data contains, where (and how) the data is stored, when (and how
often), why the data is collected and how it is processed.

Metal Accounting – The system whereby selected process data (pertaining to


metals of economic interest) is collected from various sources including mass
measurement and analysis and transformed into a coherent report format that is
delivered in a timely fashion in order to meet specified reporting requirements.

Metallurgical (Metal) balance – The determination through measurement, analysis


and computation of the magnitude of each component of interest across an entire
process (Primary Accounting) or across each section of a process flow sheet
(Secondary Accounting). (See Mass Balancing). A metallurgical balance, which is
suitable for reporting of Metal Accounting, should be supplemented by defined
uncertainties associated with each determination. In terms of this Code, a
metallurgical (metals) balance encompasses metals, minerals or commodities of
interest.

Metrology – The science of Weights and Measures.

Mine Call Factor – The ratio, expressed as a percentage, which the specific product
accounted for in the product recovered from a plant, plus that in tailings/residues,
bears to the corresponding product called for by the mine’s measuring and evaluation
methods. It is also the product of the Shaft and Plant Call Factors.

Momentum Mass Flow Meter (Impact Mass Flow Meter) – A device that detects
mass flow rate by measuring the momentum of a stream of material falling a definite
distance under gravity.

National Prototype Kilogram – The standard certified weight which is held by


individual countries and which has been certified by the International Bureau of
Weights and Measures. This standard weight is used to certify, by the national
Metrology organisation, the test weights used to certify all weighing equipment.

Nuclear Belt Scale/Weigher – A mass measurement device that continuously


integrates and records as a cumulative mass the load on a belt while it passes the
nuclear source by measuring the absorption of the gamma rays by the material on
the belt.

Nuclear Gauge – An instrument that emits a source of neutrons or radiation (usually


gamma rays) which pass through the material in a conduit, on a belt, or in a stockpile
or bin, and has a receptor that collects the radiation on the other side, thus enabling
a measurement of the radiation adsorption and hence the moisture content or density
of the material.

Penetrometer – An instrument that measures in-situ density by measuring the


backpressure resulting from the penetration of a cone into the material being
measured. Usually applied to soils but is also utilised for stockpiles of material such
as coal of a relatively fine uniform size.

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Plant Call Factor – The mass of a species recovered to product and to tailings of the
plant divided by the mass of species fed to the plant, expressed as a percentage.

Plant Historian – A computer system for accurate operational data archiving and its
rapid recovery. The data historian accepts data input only, it does not recognise
structures and procedures, and it is strictly concerned with accurate, efficient data
storage and recovery if required. Data historians perform three key functions:

• Data compression
• Rapid data recovery
• Data save-set facility
Plant Inventory – The inventory can be stockpiles of feed, intermediates or products
(plant stocks) as well as transient and long-term in-process inventory.

Plant Stocks – Any material received by a plant, from a previous processing


operation, but which has not yet entered a process stream, or any material produced
by that plant to dispatch standard quality, but which has not yet been dispatched.

Platform Scale – A compound lever scale whose load receiving element is a


platform that is supported by four or (rarely) more main bearings.

Precision – Precise measurements have a dispersion about their mean value which
is lower than a defined dispersion or indeed a probability density of a particular
nature. The level of dispersion or the nature of the probability density is defined with
the purpose of separating measurements that are entirely fit for a particular purpose
or use and those that are not. A precise measurement may not be accurate; its
mean may differ from the true value of the measured quantity by an arbitrary amount.
Standards often quantify the term precision as a value corresponding to the
magnitude of a 95% confidence interval around a result. The interval is ± ts, where t
is the two-sided Student-t value at 95% confidence and s is the estimate of the
standard deviation.

Pregnant Solution – A solution containing dissolved metals (e.g. from a leaching


operation), which is normally the feed to further processing to extract the product
metals.

Primary Accounting – The metal balance across an entire plant as determined by


Check in-Check out.

Random Errors – The component of the error of measurement, which in the course
of a number of measurements of the same measurand, varies in an unpredictable
way.

Random Stratified Sampling – The taking of increments whereby the material being
sampled is divided into strata, one increment being taken at random within each
stratum. (AS 4433.1 – 1997). For example, if the sampling interval of a cross stream
cutter is based on time, say every 5 minutes, the cutter is not triggered at 5, 10, 15
etc minutes but rather at a random time within each 5 minute interval.

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Reconciliation – A metallurgical balance which relates production of saleable and
reject or waste materials from a process back to its source as ore or other feed
material. It should be provided with defined and stated errors as for any other
metallurgical balance.

Recoverable Metal – The proportion of a metal in a feed material that has been
determined to be recoverable, by laboratory and/or pilot plant tests, by the chosen
process, with the remaining metal being defined as Non Recoverable.

Recovery – Of a particular component is defined as the proportion of that component


in the feed source, which is estimated to have reported to each process stream but
most commonly to the saleable product. Hence, recovery is a measure of
performance efficiency and it is always a key performance indicator.

Reduction – The process of decreasing the dimension of pieces constituting the


sample, without modification of mass of the sample or of its composition (AS 4433.2
– 1997).

Risk – The chance of an event occurring that will have an impact on objectives. A
risk may be quantifiable in terms of the likelihood of loss, less than expected returns
or an undesirable outcome. (The VALMIN Code, 2005 Edition)

Risk Assessment – A formal process for the identification and quantification of the
risks associated with all the processes involved in metal accounting. For example, a
decrease in accuracy of measurement may lead to the true loss of metal exceeding a
threshold value; a risk assessment will quantify the probability that the threshold is
exceeded.

Run of Mine (ROM) Ore – Ore produced from a mining operation, which has not
been subject to any beneficiation.

Sample Safety Line – Is usually constructed in a nomograph and relates the


minimum sample mass required at a particular particle size to achieve a specified
level of variance. Gy introduced the concept of a 'sampling safety line', which is
based on the relationship between the introduced variance and the particle top size.

If the sampling constant is taken to be dependent only on particle top size and the
sampling constant is known at one particular state of comminution of the material, a
'sampling safety line' can be drawn for the particular analyte to which the sampling
constant applies.

Sampling Constant – The sampling constant for a material describes its


heterogeneity with respect to a particular analyte. The sampling constant is usually
proportional to the cube of the 95% passing size of the particles in the sample, but
this is not always true. Important exceptions to this rule occur when sampling
materials that are low-grade overall but in which the valuable component occurs as
relatively large blebs or nuggets of high-grade material. Diamond ores, alluvial gold
and PGM ore containing 'metallics', where the valuable component is present at
g/tonne levels, are the most notable exceptions. Low-grade materials with small
inclusions of high-grade material can have very large sampling constants. The
sampling constant has a unit of mass, usually expressed in grams.

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SCADA – Acronym for Supervisory Control and Data Acquisition, a computer
system for gathering and analysing real time plant data. SCADA Systems are used
in industry to monitor and control plant status and provide logging facilities. As the
name indicates, it is not a full control system, but rather focuses on the supervisory
level. As such, it is a purely software package that is positioned on top of hardware
to which it is interfaced, in general via Programmable Logic Controllers (PLCs), or
other commercial hardware modules.

Secondary Accounting – Conducting mass balances over smaller sections of the


total plant circuit, to identify where lock-ups are occurring, time lags are involved or
where any measurement problems exist.

Shaft (or Mine Section) Call Factor – The mass of a species delivered to a shaft
compared to the mass of that species calculated from sampling and surveying
procedures, expressed as a percentage.

Sonic Drilling – Sonic drilling involves drilling with a drill stem that is excited at a
relatively high frequency, resulting in a standing wave being transmitted down the
drill stem and back upwards. This vibration substantially reduces the friction between
the stem and the material being drilled. It is claimed that core recovery is better for
sonic drilling than conventional coring methods.

Specific Gravity – The specific gravity of a substance is the ratio of the density of
the substance at a specified temperature to the density of a reference substance at
the same or a specified different temperature (usually the reference substance is
water at a temperature of 4 ºC). Specific gravity is a dimensionless quantity and is
also referred to as 'relative density'.

Strata – Approximately equal parts of a lot or sub-lot based on intervals of time,


mass or space (AS 4433-1:1997).

Static Scales – A mass measurement device that converts a static load on a


weighbridge or on a platform, inside a hopper or suspended from a gantry scale into
a mass.

Systematic Errors – The component of the error of measurement which, in the


course of a number of measurements of the same measurand remains constant or
varies in a predictable way.

Three-Product Formula – Used in concentrators which produce more than one


concentrate product (e.g. lead-zinc concentrators), to obtain a metallurgical balance
for process monitoring purposes, where the component analyses of the feed and
each product stream are known, as well as the mass flow of one of the streams
either entering or leaving the plant.

Tolerance – The limit of error or variance established by authority or usage or a


value fixing the limit of allowable error or departure from true performance or value.
(NIST Handbook)

Traceability – The property of the result of a measurement or the value of a


standard whereby it can be related to stated references, usually national or

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international standards, through an unbroken chain of comparisons, all having stated
uncertainties.

Transparency – Is achieved when the method of measurement, analysis and


calculation of a quantity is fully documented.

Triple bottom line reporting – The triple bottom line (TBL) focuses corporations not
just on the economic value they add, but also on the environmental and social value
they add - and destroy.

At its narrowest, the term 'triple bottom line' is used as a framework for measuring
and reporting corporate performance against economic, social and environmental
parameters.

At its broadest, the term is used to capture the whole set of values, issues and
processes that companies must address in order to minimize any harm resulting from
their activities and to create economic, social and environmental value. This involves
being clear about the company's purpose and taking into consideration the needs of
all the company's stakeholders and shareholders, customers, employees, business
partners, governments, local communities and the public.

Twin-Stream (parallel analysis) – Is a system where a sample is analysed,


preferably, by different analysts at different times using separately calibrated
instrumentation. Alternatively, if the availability of different analysts is limited, the
same analyst can repeat the analysis at different times.

Two-product formula – Used in concentrators with minimal accumulation of


inventory to calculate plant recovery, where

Plant Recovery = (Cc/Ff) x 100% = 100c(f – t)/f(c – t)

And C and F are respectively Concentrate and Feed tonnages

And c, f, and t are respectively Concentrate, Feed and Tails grades.

Ultrasonic Transit Time Flow Meters – A flow meter utilising the principle that the
propagation velocity of sound waves within a fluid is directly influenced by the
velocity of that fluid.

Umpire Laboratory – A laboratory, chosen because of its expertise, to which


samples with disputed results can be sent for arbitration.

Unaccounted Loss or Gain (Metal Accounting Variance) – Any discrepancy


between actual recovery and the accountability over an accounting period.

Uncertainty – A parameter, associated with the result of a measurement that


characterises the dispersion of the values that could reasonably be attributed to the
measurand.

Weighbridges – Weigh scales designed to weigh road trucks or rail wagons where
the lever system is usually below ground in a pit so that the vehicle or rail wagon can
pass over and stop on the scale. In a large capacity scale it also refers to the

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structural frame carried by the main bearing which supports the load-receiving
element.

Yield – The quantity of coal (of a specified quality) obtained from Run of Mine
Material expressed as a percentage. There are two subsets:

11 Theoretical Yield: obtained in laboratory from washability curves. It is


higher than practical yield.

12 Practical Yield: obtained on a plant after losses due to process inefficiency.

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AMIRA P754

Guidelines for Metal Balancing and Reconciliation –

Release 3 February 2007

Page

1 INTRODUCTION .................................................................................1
1.1 SAFETY AND HEALTH 2
1.2 PRINCIPLES OF METAL ACCOUNTING 2
1.3 STANDARDS 4
1.4 TRACEABILITY 4
1.5 ACCURACY IN METAL ACCOUNTING 4
1.6 PRECISION IN METAL ACCOUNTING 4
1.7 ERROR TYPES 6
1.7.1 Random Errors 6
1.7.2 Systematic Errors 6
1.7.3 Illegitimate (Spurious) Errors 8
1.8 METAL ACCOUNTING RISK 8
1.8.1 Introduction 8
1.8.2 Misrepresenting the Performance of the Operation 9
1.8.3 Real Losses of an Unknown Nature 10
1.9 TRAINING 10
1.9.1 Plant and Laboratory Operators 10
1.9.2 Plant and Laboratory Management 11
1.9.3 Operations Management 11
2 DATA MANAGEMENT...................................................................... 12
2.1 INTRODUCTION 12
2.2 DATA ACQUISITION AND ENTRY 12
2.3 DATA DOCUMENTATION 13
2.4 DATA PROCESSING 13
2.5 QUALITY CONTROL (QC) AND ASSURANCE (QA) 14
2.6 DATA FORMATS 14
2.7 DATA STORAGE AND BACK-UP 14
3 MASS MEASUREMENT ................................................................... 15
3.1 INTRODUCTION 15
3.2 ACCURACY AND PRECISION OF MASS MEASUREMENT 17
3.2.1 Scales/Weighing Equipment 18
3.2.2 Flow Meters 19

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3.3 METHODS OF MEASURING MASS 20
3.4 MASS FLOW MEASUREMENT 21
3.4.1 Mass Flow in Rail/Road Trucks 21
3.4.2 Mass Flow of Feed Materials, Products and Intermediates 23
3.4.3 Mass Flow on Conveyors 24
3.4.4 Mass Flow in Conduits 28
3.4.5 Mass Flow in Open Channels 32
3.4.6 Mass Flow for Bulk Commodities 32
3.4.7 Mass in Storage Areas 33
3.4.8 Mass in Stopes/ Ore Blocks 33
3.4.9 Mass in Stockpiles 34
3.4.10 Mass in Tanks and Bins 34
3.5 MASS IN PROCESS INVENTORY 35
3.5.1 Transient 35
3.6 LONG TERM 35
3.7 DENSITY AND MOISTURE MEASUREMENT 36
3.7.1 Bulk and Laboratory Tests 37
3.7.2 Nuclear Gauges 37
3.7.3 Microwave Gauges 38
3.7.4 Penetrometers 38
4 SAMPLING........................................................................................ 39
4.1 INTRODUCTION 39
4.2 SAMPLING ERRORS 40
4.3 STATISTICAL BASIS OF SAMPLING THEORY 43
4.3.1 Intrinsic heterogeneity of a particulate material 44
4.4 ACCURACY OF THE SAMPLING SYSTEM 54
4.4.1 Reference Sampling Method 56
4.4.2 Slurry Sampling 57
4.4.3 Stock-pile or Bin Sampling 57
4.4.4 Truck, Wagon, Skip and Drum Sampling 57
4.4.5 Solution Sampling 58
4.4.6 Final Metals and alloys 58
4.4.7 Scraps and residues 58
4.5 PRECISION OF THE SAMPLING SYSTEM 59
4.6 4.6 MULTI-STAGE SAMPLING SYSTEMS 61
4.7 SAMPLE STORAGE PRIOR TO DELIVERY TO A LABORATORY 62
4.8 SAMPLE LABELLING 62
5 SAMPLE PREPARATION AND ANALYSIS ..................................... 63
5.1 INTRODUCTION 63

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5.2 SAMPLE PREPARATION 63
5.2.1 Moisture Determination 63
5.2.2 Sample Reduction 63
5.2.3 Sample Mixing 64
5.2.4 Sample Division 64
5.2.5 Sample Storage After Sample Preparation 65
5.3 ANALYSIS 65
5.3.1 Laboratory Accreditation 65
5.3.2 Twin Stream (independent parallel) Analysis 65
5.3.3 Reference Materials 65
5.3.4 Instrumental Calibration (ICP, AA, UV/VIS, XRF [solutions]) 66
5.3.5 Instrumental Calibrations (XRF [Pressed Powder and Fused Bead]) 66
5.3.6 Instrumental Calibrations (Other) 66
5.3.7 On-Line Analysers 66
5.3.8 Fire assay 66
5.3.9 Mineralogical Analysis 67
5.3.10 QC Procedures 67
5.3.11 QA Procedures 67
5.3.12 Umpire Laboratory 67
6 STOCK-TAKES................................................................................. 69
7 METAL BALANCING........................................................................ 71
7.1 INTRODUCTION 71
7.2 THE METAL ACCOUNTING PROCESS 72
7.3 METAL BALANCING 75
7.4 RECONCILIATION OF METAL BALANCES 79
7.4.1 Detecting Random Error (or Illegitimate/Spurious Errors) 81
7.4.2 Bias 81
7.4.3 Estimating Flow Rate Accuracy 81
7.5 METAL BALANCING APPLICATIONS 82
7.5.1 Concentrators with minimal accumulation 82
7.5.2 Concentrators with Intermediate Accumulation 84
7.5.3 Coal Treatment Plants 84
7.5.4 Pyrometallurgical Plants 84
7.5.5 Hydrometallurgical Plants 89
7.5.6 Heap Leaching 90
7.5.7 Bench Scale, Pilot and Demonstration Plants 94
7.6 MINE TO PRODUCT BALANCING AND RECONCILIATION 98
7.7 MASS BALANCING FOR ENVIRONMENT AND HEALTH MONITORING 98
7.7.1 Gases and Dusts 99
7.7.2 Liquid Effluents 99

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8 REPORTING ................................................................................... 100
9 SELECTION AND USE OF A COMPETENT PERSON .................. 102
10 DESIGN OF METAL ACCOUNTING SYSTEMS ............................ 104
11 METAL ACCOUNTING AUDITING RULES.................................... 107
11.1 INTRODUCTION 107
11.2 AUDIT TEAM AND ITS RESPONSIBILITIES 107
11.3 METAL ACCOUNTING REVIEW 108
11.4 PHYSICAL AUDITS 108

GLOSSARY.................................................................................................... 109
LIST OF ACRONYMS AND ABBREVIATIONS ............................................. 128

APPENDICES................................................................................................. 129
APPENDIX A – ACKNOWLEDGEMENTS..................................................... 129
APPENDIX B – REFERENCES...................................................................... 131
APPENDIX C – STANDARDS........................................................................ 139
APPENDIX D – CHECK-LISTS ...................................................................... 150
APPENDIX E – MASS BALANCING TECHNIQUES ..................................... 159
APPENDIX F – DETERMINATION OF THE SAMPLING CONSTANT.......... 171
APPENDIX G – ERROR AND VARIANCE PROPAGATION IN TOLL
SMELTING OPERATIONS TREATING MULTIPLE
CONCENTRATE STOCKPILES.......................................... 174
APPENDIX H – USEFUL WEB SITES ........................................................... 192

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1 INTRODUCTION
The AMIRA P754 project has the primary objective of improving the auditability and
the transparency of Metal Accounting from mine to product, thus enhancing
corporate governance. The project is supported by five sponsor companies in
South Africa and Australia and it involves two academic supervisors and seven
students. Project areas have broad coverage from precious metals, to commodities,
and mine to product.

This document is intended to serve as a set of Guidelines for the Code on Metal
Accounting, which will in the future be controlled by suitable professional
organisations closely associated with the industry, and gain industry acceptance
worldwide. It should also be regarded as a living document which will be revised
through contributions from sponsor companies, the related research program and
other initiatives. In this Guidelines document, unless otherwise specifically stated,
references to the “Code” include both the Code and the Guidelines.

A number of sponsor companies and others involved in, or connected to, the metals
production industry have contributed to the contents of this document through the
provision of internal standard procedures and/or specifications, in assisting with
literature searches and by providing advice and information. A list of these
companies and individuals is included in the Appendix A, and their contributions are
gratefully acknowledged.

The aim of this document is to provide standard generic procedures and guidelines
for obtaining credible figures of quantities of materials processed and produced and
further, to be recognised and accepted as the Industry guidelines for best practice.
In cases where companies or operations are unable to comply with the best
practices set out in the Code and these Guidelines, the reasons for this non-
compliance must be documented in the form of an Exception Report. This must
clearly set out the reasons for the non-compliance, the steps taken to mitigate the
effects of the non-compliance, the resultant impact on the overall integrity of the
metal accounting system and plans to ensure compliance in the future. This
Exception Report must form part of the documentation of the metal accounting
system and, as such, must be approved by the Competent Person responsible for
the design of the metal accounting system, and by the Audit Committee of the
company concerned.

These Guidelines should facilitate full disclosure of operational performance,


including losses in gas emissions, (of S as SO2, for example) or other effluents from
operations, in line with requirements for triple bottom line reporting in financial
statements

There are no differences in principle between base and precious metals and
commodities, but there are differences in the way the Code/Guidelines would be
applied. These Guidelines set out principles for obtaining credible figures, such as
the methods to be used and their accuracy, recommended methods for mass
measurement, sampling and analysis and the applicable International Standards to
achieve this, as well as the basis for the design and management of a Metal
Accounting system. More details are included in the Appendices.

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The Code and Guidelines are aimed at working with quantities whereas valuation of
these quantities is a separate exercise. The Guidelines together with the appropriate
use of statistics to define confidence levels provide a framework for metal accounting.

Due to the random variations that are inherent in all measurement processes, the
values derived in metal accounting will not be exact but will have a degree of
uncertainty. However, in correctly designed and operated systems the level of
uncertainty is measurable and should be quoted in the accounting reports. If the
measured precision value is outside of the expected range, and the range will vary
depending on the materiality of the measurement concerned, its cause should be
identified and rectified.

Because of the naturally wider variations in dynamic metallurgical processes, it is


usual to use shift data for plant control purposes. The metal accounting system
combines shift data into an average, “to date”, number that is normally reconciled
and reported on a monthly basis. This data is then further combined on a quarterly
or six monthly basis to suit the company’s financial reporting requirements.

1.1 SAFETY AND HEALTH


It is expected that internal company procedures, in compliance with local laws and
regulations, will provide fully for the safety and health of all staff, which must always
be of primary importance in all of the activities involved in Metal Accounting. For
example, in the design of metallurgical plants, the positioning of weighers and
samplers should be such that access to them for routine operation, inspection and
cleaning can be done in a completely safe manner.

Staff must be trained in the safety and health aspects of their activities and supplied
with the necessary Personal Protective Equipment (PPE). The possibility of potential
exposure to hazardous dusts, gases and chemicals, as well as other hazards, must
be fully understood and adequate precautions implemented.

1.2 PRINCIPLES OF METAL ACCOUNTING


The basic principles of metal accounting are summarised below:

1 The metal accounting system must be based on accurate and precise


measurements of mass and metal content. It must be based on a full
Check in-Check out system using the Best Practices, as defined in this
Code, to produce an on-going metal/commodity balance for the operation.
The system must be integrated with management information systems,
providing a one-way transfer of information to these systems as required.
2 The system must be consistent and transparent and the source of all input
data to the system must be clear and understood by all users of the
system. The design and specification of the system must incorporate the
outcomes of a risk assessment of all aspects of the metal accounting
process.
3 The accounting procedures must be well documented and user friendly for
easy application by plant personnel, to avoid the system becoming
dependent on one person. The procedures must incorporate clear

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controls and audit trails. Calculation procedures must comply with the
requirements set out in this Code; they must be consistent at all times and
must include clear rules for handling the data.
4 The system must be subject to regular internal and external audits and
reviews as specified in the relevant sections of the Code, so as to ensure
compliance with all aspects of the defined procedures. These reviews
must include assessments of the associated risks and recommendations
for their mitigation, when the agreed risk is exceeded.
5 Accounting results must be made available timeously, to meet operational
reporting needs, including the provision of information for other
management information systems, and to facilitate corrective action or
investigation. A detailed report must be issued on each investigation,
together with management’s response to rectify the problem. When
completed, the plan and resulting action must be signed-off by the
Competent Person.
6 Where provisional data has to be used to meet reporting deadlines, such
as at month ends when analytical turn-around times could prevent the
prompt issuing of the monthly report, clear procedures and levels of
authorisation for the subsequent replacement of the provisional data with
actual data must be defined. Where rogue data is detected, such as
incorrect data transfer or identified malfunction of equipment, then the
procedures to be followed together with the levels of authorisation must
be in place.
7 The system must generate sufficient data to allow for data verification,
handling of metal/commodity transfers, reconciliation of metal/commodity
balances, and measurement of accuracies and error detection, which
should not show any consistent bias. Measurement and computational
procedures must be free of a defined critical level of bias.
8 Target accuracies for the mass measurements and the sampling and
analyses must be identified for each input and output stream used for
accounting purposes. The actual accuracies for metal recoveries, based
on the actual accuracies, as determined by statistical analysis of the raw
data, achieved over a company’s reporting period must be stated in the
report to the Company’s Audit Committee. Should these show a bias
which the Company considers material to its results, the fact must be
reported to shareholders.
9 In-process inventory figures must be verified by physical stock-takes at
prescribed intervals, at least annually, and procedures and authority levels
for stock adjustments and the treatment of unaccounted losses or gains
must be clearly defined.
10 The metal accounting system must ensure that every effort is made to
identify as rapidly as possible any bias which may occur and to eliminate
or reduce to an acceptable level the source of bias from all measurement,
sampling and analytical procedures once the source is identified.

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1.3 STANDARDS
Procedures used to provide data for Metal Accounting must be undertaken to the
requirements of the appropriate International or National Standard Institutions,
which have developed these to cover a wide range of mining and metal products.
Where these standards are not available, great care should be taken to maintain the
accuracy of procedures.

1.4 TRACEABILITY
In the areas of mass measurement and analysis, the aim should be to establish
traceability to international standard (SI) units.

1.5 ACCURACY IN METAL ACCOUNTING


All of the operations and equipment used to derive data for the reporting of Metal
Accounts, which include mass measurement, sampling, sample preparation and
analysis, should be designed and operated to achieve an accurate result.

As defined in this Code, accuracy is related both to random errors (Section 1.7.1),
which are an integral part of the measurement process, and to systematic errors
(Section 1.7.2).

Bias occurs as a result of systematic errors which occur when the mean value of the
random errors is not zero over an extended period which contains many
measurements. Bias is difficult to detect but it can and should be eliminated (or at
least minimised) because its effect accumulates in any cumulative measures of
production or performance.

Accuracy should not be confused with Certification. Certification is required to


provide an agreed basis for commercial transactions and Custody Transfer. A
certified measurement will contain random errors and it may also contain some
degree of bias. However, for the purposes of the commercial transaction, the
numerical result is considered to be an absolute value and it is used as the basis of a
monetary transfer calculation.

A metal accounting system, which is performing well, will provide good agreement
between the metal balance, calculated using many data inputs, and the commercial
values used as the basis of commercial transactions. However, the values only need
to be similar to within the precision of the Metal Accounts.

1.6 PRECISION IN METAL ACCOUNTING


The variances of independent operations during a process are additive. In Metal
Accounting this can be represented by the following equation:

VTMA = VM + VS + VSP + VA [Eqn 1.1]


where:

VTMA = the Total Metal Accounting variance

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VM = the variance due to Mass Measurement and the
determination of moisture
VS = the variance due to all of the Sampling Stages
VSP = the variance due to the Sample Preparation
VA = the variance due to the Analysis

VM can be further divided to show the variance due to the determination of the wet
mass, including the components of the mass measurement process, and that due to
the determination of the moisture of the material. In a multi-stage sampling process,
VS should be expanded to show the variance of each stage.

Where the processes are not independent, (i.e. they are related by a set of
procedures or combined calculations), it is appropriate to use a more general
relationship called the Propagation of Variance which takes covariance of quantities
into account. This relationship allows the variance of calculated values (such as
Recovery) to be estimated in a statistically correct manner.

Because variance is a squared term, (it is equal to the square of the standard
deviation) the operation with the largest variance will have the major impact on the
Total Metal Accounting variance. For this reason, it is important that the precision of
each operation is measured and that it has an acceptable value. An operation in this
context can mean any mass measurement or sampling and analytical procedure.
The precision for mass measurement, sampling and assaying can be established by
carrying out suitable experiments that are described in a number of International
Standards. The operation with the highest relative variance, i.e. the poorest
precision, can be identified and steps taken, if necessary, to reduce the value of the
variance. For example, the number of increments at a sampling stage could be
increased to reduce VS, or the number of replicates taken for the analysis could be
increased to reduce VA. If it was decided that the operation with the highest variance
could not be improved, for example, due to the cost involved, there would be no
purpose in reducing the variance of any other operation to be significantly below this
highest value.

In typical metallurgical plants, where process streams are sampled and analysed on
an 8-hour shift basis and about 90 data sets are produced per month, relative
precision levels (one standard deviation) of 3% for each measurement are
acceptable, because this equates to a monthly precision of 0.32%. However, where
individual shipments/lots are being evaluated, such as in toll treatment, individual
precision levels of < 0.5% will probably be required.

For operations generating a final metal product, commercial transfer precision will
usually be a small fraction of the above targets, but the required precision for coarse
mill feed (f80 of 100 mm or larger) may not be achievable without a substantial
investment in sampling and sample reduction.

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From the measurement of VTMA, it is possible to state the uncertainty in the Metal
Accounts, because:

VTMA = σ2TMA [Eqn 1.2]


where: σ TMA = the Standard Deviation of the Metal Accounts

and, by convention, it is usual to quote the uncertainty at the 95% confidence level,
which is equal to ± 2 × σ TMA.

It should be noted that biased measurements in the material balance calculations


would cause the final result to be biased. It is therefore very important that
measurements are accurate as well as precise.

1.7 ERROR TYPES


Errors in measurement can be classified into three types:

1.7.1 Random Errors


Random errors represent the variation in results obtained under the same or nearly
identical conditions. They are the scatter of the observed data around the actual
value and, as such, their average will tend to zero over time. They are caused by
natural fluctuations in the measurement process and cannot, therefore, be eliminated
but they can be minimised by careful operation. With mass measurement such
factors as:

• mechanical or electrical tolerances in the equipment


• fluctuations in temperature
• vibration and instrumental noise
will contribute to random error, and, because they are statistical in nature, they can
be evaluated and quantified by standard statistical methods.

Most random errors are assumed to be drawn from a normal distribution. If the
measurement in question is the mean of repeated measurements, then this
assumption will always be approximately correct, the approximation improving as the
number of repeated measurements increases.

However, if the probability distribution of random errors is highly asymmetric (i.e.


there is a chance of individual measurements being much larger numerically than
they will be smaller, or vice versa), then special techniques are required to ensure
that the metal balance will provide the most likely balance, which will not usually be
the mean balance.

1.7.2 Systematic Errors


Systematic errors result in data that is consistently higher or lower than the true
value, leading to a biased situation. Increasing the number of measurements will not
reduce the average of this type of error to zero. However, errors may arise from
more than one cause at the same time and these may be in opposite directions and
they tend to cancel one another out. This makes the detection and quantification of

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systematic errors difficult and they can only be identified and eliminated by careful
calibration and analysis of data.

Measurement error distributions can be truly random but they have an expected
value or mean that is non-zero and still cause bias as noted in the previous
paragraph. For example, in mass measurement, the most common form of bias is a
small instrument offset. If this offset is small compared with the random error of the
measurement, it is essentially impossible to detect from a single measurement.

A large quantity of redundant measurements, which contribute to the balance, may


assist in finding the bias or spurious error (Section 1.7.3).

Given a situation in which it is known that the expected value of a quantity should be
zero (e.g. the difference in assays of the same sample between two laboratories), it
is possible to detect a small bias by simply summing the differences over time. A
bias component in the difference will accumulate, while the random errors of zero
mean will tend to cancel. A plot of this cumulative sum of the differences is known as
a CUSUM graph.

CUSUM graphs are useful tools for detecting and measuring the level of the
systematic errors, especially if these are relatively small. CUSUMS, or ‘cumulative
sum’ methods, are very valuable for tracking the statistical parameters of a
measurand. They can be used to track the bias between two measured quantities
or they can be used to track the variance of a measurement. In the past, the
application of ‘cumulative sum’ methods implied that the differences between
measurements were simply summed over time. If the cumulative sum value
increased with time, it was interpreted as meaning that there was a real positive
difference between the values.

Such a simple basis for CUSUM methods does not, however, take advantage of
recent advances in statistical development. There are far better methods for
formulating CUSUM procedures. These are described in Hawkins and Olwell. They
describe methods that can be ‘tuned’ to detect changes in the statistical parameters
of measurements and they can also be tuned to provide the desired speed of
response to changes with a given level of risk of ‘false alarms’.

Even without bias, these differences are themselves subject to random error and
they can be expected to be negative or positive for a few times in succession. This
makes the recognition of a bias quite difficult.

In some measurements there are known errors within a system that cannot be
eliminated but they must be quantified and allowed for. These errors, which are
inherent in the method being used, produce a bias from the true value. For practical
reasons, these methods are utilised rather than an alternate method, which would
give a result closer to the true value. Examples in metallurgical accounting systems
are the:

• K-factor in electromechanical weighers


• Correction factors in the lead collection fire assay of the PGMs
• Silver correction in the fire assay of gold samples

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The assay factors are established by parallel analysis of samples using a superior,
more accurate method. It is important that the magnitude of these factors must be
established on at least a monthly basis by comparison to alternative measuring
procedures. The use and value of these factors must be agreed and signed-off by
the Competent Person. For metal accounting, fire assay should be avoided and if
used, it must be motivated by an Exception Report.

1.7.3 Illegitimate (Spurious) Errors


Illegitimate errors are caused by such factors as incorrect readings by the operator,
incorrect calculations or abnormal sources of disturbances. Sometimes these are
obvious because the result is far from the expected value. They can be eliminated or
reduced by careful supervision and monitoring.

A common source of spurious errors is the accidental swapping of samples (or


marked containers) during the collection or analysis program. Collecting mean and
standard deviations for each measurement point provides a simple indication of the
occurrence of errors. If any measurement is more than three standard deviations
from the long term mean, it must receive further examination.

1.8 METAL ACCOUNTING RISK

1.8.1 Introduction
Any production operation is exposed to financial risk associated with its metal
accounting process, to the extent that there is uncertainty in the evaluation of the
quantities of metal delivered to that operation and produced by it. In addition, there is
the risk to the reputation of a company and of negative market perceptions resulting
from major metal accounting discrepancies. One of the prime objectives in the
design of a metal accounting system is to enable an operation to quantify, manage,
and minimise the level of risk to which it could become exposed through failures or
shortcomings in its metal accounting system. Each operation must conduct an initial
risk assessment of its entire Metal Accounting system to establish and quantify the
risks. The design of a Metal Accounting system must take these risks into
consideration and set down procedures to be followed when accounting
discrepancies are identified.

The use of statistical analysis and check measurements and analyses provides a
database, which becomes an essential component of this risk management process.
The other fundamental component of the risk management process is regular and
frequent management reviews, incorporating risk assessment, of the entire metal
accounting system, supported by both internal audits and external audits by the
Competent Person.
The main areas of risk to which an operation could be exposed in its metal
accounting system are listed below.

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1.8.2 Misrepresenting the Performance of the Operation

1.8.2.1 Incorrect weighing, sampling and analytical procedures


These procedures need to be drawn up in line with international standard
procedures (e.g. ISO 9002) while analytical quality control procedures must
be followed and corrective action taken as appropriate. Where continued
laboratory biases are detected, independent (umpire) laboratories must be
used for verification purposes.

1.8.2.2 Inaccurate weighing equipment


Weighing equipment must be correctly installed and comply with international
or local standards and it must be routinely calibrated according to standard
procedures.

1.8.2.3 Incorrect recording of receipts or dispatches


Receivers’ weights must be checked against dispatchers’ weights with a third
scale used for arbitration purposes when necessary. Any anomalies must be
highlighted by the record-keeping system and investigated immediately and
all records must be retained for audit purposes for a pre-determined period
(usually to comply with local regulations).

1.8.2.4 Inaccurate sampling equipment


Sampling equipment must be designed, installed and operated to ensure
mechanically correct sampling and the ‘Home and Away’ (Double sampling
and analysis) statistical system must be used to identify analytical and/or
sampling biases.

1.8.2.5 Accounting samples mishandled or misplaced


Clear sample handling and preparation procedures must be in place to avoid
the risk of sample contamination or loss, or of a sample being inadvertently
substituted for another. Clear record keeping is essential to track all sample
movements and it is required as part of the metal accounting audit trail.

1.8.2.6 Incorrect estimation of stockpiles


Procedures exist for stock estimation and this topic is discussed further under
Section 3.4.9 of this document. Stockpile estimates must be based on zero
measurements taken at regular intervals (at least annually), as prescribed in
the design of the metal accounting system concerned.

1.8.2.7 Arbitrary methods to calculate metal recoveries


Standard calculation procedures must be defined in line with the principles of
metal accounting (Section 1.2), based on a full Check in-Check out system,
and they must be adhered to at all times.

1.8.2.8 Use of illegitimate or biased data


Procedures for reviewing data, in order to eliminate illegitimate or biased
entries from the metal accounting database, need to be established, with

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clearly defined levels of authority for the approval of these changes. Any
such changes must be supported by documented technical evidence showing
the reason for the proposed change(s), signed off by a suitably qualified
independent person, and submitted to the company’s Audit Committee for
final approval.

1.8.2.9 Incorrect calculations


The metal accounting system must incorporate automatic checks, to verify
calculated results and to identify areas of error or uncertainty before the
results are reported.

1.8.3 Real Losses of an Unknown Nature


Typically, these are related to:

• Theft of material from the processing operation(s)


• Theft of material while in transport
• Unauthorised dispatch of material to alternative customers
• Losses caused by wind or run off, particularly while in storage or being
handled
• Failure to identify and investigate accountability problems or anomalies
promptly
The design of a metal accounting system must take these factors into consideration,
including the operation’s security arrangements and defined procedures to be
followed in the event of accounting discrepancies being identified.

1.9 TRAINING
As stated in Section 1.1 on Safety and Health, it is expected that companies will have
full training procedures, in line with National and International Standards, such as
ISO 9000, 14001 and 17025. The training requirements of staff involved in Metal
Accounting will obviously vary depending on the role they are playing. Appropriate
sections of the Metal Accounting Guidelines must be available to staff so that they
can understand their part in the total system and the requirements necessary to
produce unbiased data to a known and acceptable precision.

1.9.1 Plant and Laboratory Operators


Plant Operators must be aware of the importance of the metal accounting system to
their operation and of the design and operating criteria of correctly installed sampling
and mass measurement systems, and especially of the need for cleanliness around
this equipment. The care required in the storage, labelling and handling of samples
before they are delivered to the laboratory must be clearly understood.

Laboratory Operators must be trained in the analytical procedures and equipment


used for the analysis of Metal Accounting samples. The importance of their
contribution to the Metal Accounting process must be emphasised. Laboratory
Operators should also understand how to use and interpret Shewhart and CUSUM
graphs.
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1.9.2 Plant and Laboratory Management
Plant Management must have a detailed knowledge of the design, installation and
operational requirements of Metal Accounting systems. They should be able to plan
and implement inter-leaved experiments to establish the precision of sampling and
mass measurement equipment and bias tests to establish their accuracy.

Laboratory Management must ensure that their analytical procedures are accurate
and that they are adequately monitored by quality assurance and quality control
procedures. There is a requirement for an in-depth understanding of statistical
analysis techniques.

It is likely that a 4-year tertiary qualification will be required for both Plant and
Laboratory management.

1.9.3 Operations Management


Operations Management, in particular the “Champion” of the Metal Accounting
system, must ensure the upfront, well-designed inclusion of evaluation systems into
processing plants and be aware of their ongoing maintenance and operational
requirements. There must be an awareness of the quality assurance data required to
confirm that the systems are operating to specification.

Liaison must be established between the various internal disciplines involved in metal
accounting and the appointed Competent Person. There must be an understanding
of the relevance of Metal Accounting, its relationship to good corporate governance
and the triple bottom line.

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2 DATA MANAGEMENT

2.1 INTRODUCTION
The operation of a Metal Accounting System requires the accumulation and
evaluation of process data (e.g. mass measurements and analyses) from various
sources (e.g. SCADA, Plant Historians, LIMS systems, etc). The acquisition,
processing and management of data require a substantial portion of the effort
associated with Metal Accounting. Efficient and reliable data management adds
considerable value to the Metal Accounting System.

The goal of data management is to create files from data obtained from various plant
sources in such a way as to prevent error during transcription and to enable analysis
of the errors inherent in the raw data. Production (e.g. mass measurement) and
laboratory data (e.g. analyses) must be integrated to a single user interface to
facilitate Metal Accounting. At the same time, it is essential that those responsible for
entering plant operating data, and those entering analytical results into the system,
operate independently of each other.

2.2 DATA ACQUISITION AND ENTRY


There are a number of ways of acquiring or entering information for use in a Metal
Accounting System. Data may be acquired from various plant systems such as the
SCADA, the Plant Historian or external systems such as a LIMS system.

Manual entry of data to operator log sheets and transposition to spreadsheets is


common practice on some plants. Spreadsheets do not allow for controlled data
entry and they are easily corrupted. It is easy to inadvertently type over data, lose
track of records, duplicate and improperly enter data in a spreadsheet. For these
reasons spreadsheets must be avoided as a method of data entry.

However, because of the possibility of rogue communication between on-plant


instrumentation and the Plant Historian, manual back up is necessary.

Many errors can occur when entering or acquiring data and these need to be
guarded against. Common examples of errors are:

• Transpositions
• Copying errors
• Routing errors (e.g. information incorrectly routed from a SCADA system)
• Consistency errors
• Range errors (e.g. a value outside the plausible range for a variable)
Methods to avoid such acquisition or input errors include:

• Manual checks during data collection (e.g. checks for completeness)


• Range and consistency checking of data
• Double entry and validation of manually inputted data

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• Data analysis for outliers
Many of these checks and balances can be incorporated in metal accounting
software systems.

2.3 DATA DOCUMENTATION


Metal Accounting systems must include sufficient documentation of the data
(metadata) that is being utilised for the various calculations. The objectives of
compiling data documentation for metal accounting data are:

• To ensure data transparency


• To ensure that the data is consistently well described
• To ensure that quality and limitations of the data are apparent
• To ensure that sufficient information is available to assess the suitability of
data obtained and to enable the accuracy to be determined

Measurement or Sample Collection


Documentation of the Sampling / Measurement System must include:

• A description of the equipment used to obtain the sample or measurement


and the manner in which it is to be operated
• Details of the calibration of the measurement device
• A description of any limitations associated with the chosen sampling or
measurement strategy

Sample Preparation and Analysis


Documentation for Sample Preparation and Analysis must include:

• How the sample is prepared


• A description of the stages of sample preparation
• A reference to the documentation of the analytical procedure
• A description of how instrumental error corrections are applied, if applicable
• A description of the expected precision, accuracy, repeatability, and
reproducibility of the method and the limits of detection
• Details of methods used to validate sample preparation methodologies
• Comments on any limitations

2.4 DATA PROCESSING


Documentation for the Data Processing System must include:

• A clear description of the different stages of how the data is processed,


including algorithms, statistical analysis, etc.
• A description of the algorithms and computer programmes used
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• Comments on limitations

2.5 QUALITY CONTROL (QC) AND ASSURANCE (QA)


This system must:

• include a description of QC and QA procedures


• document missing data or errors

2.6 DATA FORMATS


All data formats must be suitable for inclusion in computer files and they must be well
documented to be readily accessible to all authorised users, in order to avoid
misunderstandings and to prevent the data from becoming unusable. To achieve this,
the documentation must include details of the provenance of a number, including its
units of measurement, as well as the method by which it was obtained.

2.7 DATA STORAGE AND BACK-UP


Data loss can occur due to natural disasters, theft, human error and computer error.
It is therefore necessary to take adequate steps to protect/store Metal Accounting
data once it has been collected. It is essential to back-up data and documentation
files on a regular basis. Back-up systems must be thoroughly tested to ensure that
files remain uncorrupted and that they can be restored. Procedures must be written
up for personnel unfamiliar with back-up and restore methods.

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3 MASS MEASUREMENT

3.1 INTRODUCTION
The overriding objective of mass measurement for Metal Accounting purposes is to
establish the mass of the particular material or component present at a specific time,
or the mass flow of that component over a defined time period, to a defined
accuracy suitable for mass balancing.

For the purposes of these Guidelines, “mass” should be read as “mass or volume,”
as often for practical purposes, volume is measured (e.g. stockpiles or fluid flow). In
these cases the specific gravity/relative density of the slurry, and of the solids
and/or liquids, and/or bulk density, must also be determined by appropriate methods
in order to calculate the mass. Materials often contain moisture, the proportion of
which must also be established in order to obtain the dry mass.

Wherever possible the mass measurement must be:

• repeatable to within the defined error criteria


• reproducible to within a defined error criteria, using different methods or
equipment
• unbiased, or alternatively capable of being tested to establish bias over a
period of time
• traceable back to the accredited standards used for calibration and
certification
In order to achieve the above the system must be:

• carefully selected to suit the specific application


• specified, manufactured, designed and installed to appropriate guidelines
• installed in such a manner as to permit operation, maintenance and
calibration to be carried out safely
• operated and maintained in an appropriate manner
• calibrated regularly according to recommended standards and guidelines
• assessed by the collection and statistical analysis of the operating and
calibration data and checks to determine the accuracy of the measurements
• certified by the appropriate authorities or test facilities as required
The mass measurements necessary for metal accounting purposes are normally
required to measure the deportment of valuable components and/or for legal and
environmental requirements. As such, they must be within appropriate limits of
accuracy to satisfy shareholders and stakeholders. Thus, the equipment and the
calibration techniques used must be capable of producing results, which are superior
to those which may be used for management data or for plant control, where the
consistency of the measurement is more important than the absolute value and thus
some bias may be acceptable. The acceptable accuracy should also take account of
Best Practices, bearing in mind the cost/benefit relationship, the difficulty of
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measuring and sampling the process stream and the importance of the measurement
to the metal balance.

Mass measurement can be classified into three areas:

• Measurements necessary for custody transfer and Primary Metal


Accounting
• Measurements required for Secondary Metal Accounting, and management
control including intra company transfers and plant area performance, which
may also be used for cross checks on Primary Accounting. This also includes
measurements necessary for environmental monitoring
• Measurements required for plant control only.
The requirements for the accuracy of the measurement are the most stringent for
Primary Accounting, requiring certified (assized) weighing equipment and the ability
to establish the distribution of the random errors associated with the measurements.
Accuracy requirements are less for Secondary Accounting, with those for plant
control requiring the lowest level of accuracy.

This Code is concerned with the requirements for the first measurement area only.
Secondary Accounting measurements are used for checking and investigation
purposes, in conjunction with other process data, where confirmation of Primary
Accounting information is required.

Normally, final saleable products are weighed on certified (assized) weighing


equipment and sampled and analysed according to laid down procedures agreed
between seller and purchaser, usually to accepted standards for custody transfer.
The mass measurement of process streams for Primary Metal Accounting must be
carried out to the same level of accuracy as those for custody transfer or commercial
transactions. This means that certification, and the ability to establish the distribution
of the random errors associated with the measurements, are requirements.

Feed material to metallurgical plants is often ore, supplied from mining operations in
large quantities, which has a wide and variable size range and moisture content.
Mass measurement of this stream is required for Primary Accounting but, in practice,
it is often weighed in trucks or hoppers, or on conveyor belts, to a lower level of
accuracy than required for the final products. Achieving a high degree of accuracy
for this type of material is more difficult and costly and it requires appropriate design,
selection and installation as emphasised above. If it is felt that the cost and effort to
achieve certification is not justifiable, then this must be motivated by way of an
Exception Report.

In all weigher and flow meter installations, it is essential that the selection, system
design, installation, operation, maintenance and calibration follow the applicable
standards and manufacturers’ recommendations, in order to achieve the accuracy
and precision levels quoted in Section 3.2, and those which are required by
International and National Standards and National Metrology Acts.

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3.2 ACCURACY AND PRECISION OF MASS MEASUREMENT
The various possible methods of measuring mass or mass flow are described in
Section 3.3.

In terms of mass measurement, accuracy may be defined in several different ways,


such as maximum percentage error of reading, or maximum percentage error at full
scale of the instrument or equipment, and it is critical to ensure that the definition of
levels of accuracy in supplier’s documentation or the literature is comparable with
those used in this Code and in the applicable Standards.

The accuracy of mass measurement is affected by the:

• material being measured (particle size, size distribution, homogeneity,


variability in size, composition or density, etc.)
• method of measurement (static scale, belt scale, flow meter etc.)
• type of equipment being utilized (electromechanical, nuclear etc.)
• design of the measuring installation
• maintenance of the equipment
• calibration of the equipment.
The objective of mass measurement for Metal Accounting is to provide a mass in
which the random errors are reduced to within acceptable limits and bias eliminated.
Errors are possible throughout the mass measuring chain, including those introduced
by the equipment layout, the material being measured and mechanical, physical or
environmental aspects, and by the measuring source such as a load cell, or by the
various processes in the electronic circuits. The more steps in the chain, the greater
the possibility of error and the greater the magnitude, as all errors are cumulative.
The statistical methods to establish the precision and bias for mass measurement
are discussed in Merks and Merks. In addition, there are the errors in the moisture or
density measurements used to convert a wet weight or volume to a dry mass.

In general, the larger the quantity being measured and the more variable in size and
flow rate, the lower the accuracy. In addition, in the case of precious metals and
base metals, the larger the stream or quantity of material, generally the lower the
content of the constituent for which the metal balance is required, which affects the
analytical precision.

Thus, in the mining and metallurgical industry, generally the accuracy of mass
measurement will increase through the processing chain from raw feed or ore to the
final metal, as the materials become more homogeneous in size and composition,
with a higher grade, and they are present in smaller quantities.

The cost of the mass measurement device is often only a small portion of the cost of
the total system required to obtain a mass flow measurement suitable for accounting.
A total system includes equipment for calibration, such as weigh tanks or bins, or
other facilities for check weighing. However, the higher capital cost incurred due to
correct design and installation of the system will often result in a lower total cost of

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ownership because of reduced maintenance and operating costs, while also
increasing measurement precision.

3.2.1 Scales/Weighing Equipment


In the weighing industry, if a scale is accurate, it has been properly calibrated, it
conforms to the applicable standard and its performance is within the permitted
tolerances (or maximum permissible errors) for initial verification and it is in service.
Although the maximum tolerances specified in the Standards, such as NIST 44, may
suggest 95% confidence levels, this is in fact not actually stated.

Accuracy is generally expressed in the industry in terms of “inaccuracy” or the


amount of error, and it is quoted as ± x%, usually of the full-scale value, without
defining the confidence levels. The precisions quoted in this section are percentages
of full-scale value. Often the number quoted in literature is actually precision and not
accuracy. For further discussion of this see Merks15, and Colijn11.

The figures quoted below are expected precisions in terms of a coefficient of


variation.

Static scales provide the most accurate and precise method of measuring mass and
must be the choice, where circumstances permit, for custody transfer and Primary
and Secondary Metal Accounting purposes. They can be easily certified by
standardised procedures. Static scales include platform scales, road and rail
weighbridges, gantry, hopper and bin scales.

Precisions generally range between ± 0.05% to ± 0.2% for platform scales and
± 0.1% to ± 0.5% for weighbridges, on gross load measurements. For hopper/bin
scales and gantry scales the equivalent figures are ± 0.1% to ± 0.25% and ± 0.15%
to ± 0.4% respectively.

The accuracy of in-motion weighing is affected significantly by the truck speed and
acceleration. This effect is more apparent in the weighing of road trucks where the
control of speed and acceleration is much more difficult than for rail. Thus, in-motion
weighers are certifiable for rail use but not for road use. Certified in-motion weighing
is a suitable choice for Primary Metal Accounting for rail transport, provided that the
key principles of taring each truck or hopper on each occasion and controlling the
speed are adhered to. In-motion weighing should give a precision of ± 0.5%.

Certified electromechanical belt weighers must be the second choice for metal
accounting purposes after static scales or in-motion weighing, provided that the
design, installation, calibration, operation and maintenance requirements are
adhered to.

The accuracy of conveyor belt weighing is installation specific and it is affected by:

• belt effects such as tension, stiffness and misalignment of the belt or the
idlers
• flexibility of the weigh carriage
• spillage onto the weigh section

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• errors in the belt speed measurement
• calibration errors and poor calibration techniques
• errors in the other processes of the measurement chain
• belt loading (proportion of design and variability)
• changes in the material being conveyed
• external environmental factors such as wind, dust and excessive vibration or
shocks
• poor operation, housekeeping and maintenance
The majority of the error in a belt scale has normally been found to be due to
conveyor design and resulting belt effects and user practices (Colijn2). If properly
designed, installed, operated, maintained and calibrated they should achieve
operating precisions of ± 0.5%.

Nuclear belt weighers, although not subject to belt errors, are generally less
accurate because of effects related to the material conveyed. Precisions of ± 1–2%
can be achieved but, in practice, are often much worse. They should not be used for
Primary Metal Accounting but they can be used for Secondary Metal Accounting if
the material is homogeneous in size and composition and the belt loading uniform.

3.2.2 Flow Meters


The accuracy of flow meters can be expressed in three different ways:

• Percentage of span
• Percentage of a rate or reading
• Percentage of the upper range limit
The accuracies quoted below are those at 95% confidence levels.

The accuracy of electromagnetic flow meters, especially on slurries, is installation


specific. The accuracy is adversely affected by changes in the material and the fact
that the density measurement introduces another source of error. Typical accuracies
are ± 0.2 to ± 1% of reading and ± 0.5% is attainable on water or clean solutions if
selection, design, installation, operation and calibration follow the applicable
standards and manufacturer’s recommendations. On slurries, however, the accuracy
is usually much worse than the figures quoted above for the reasons discussed in
Section 3.4, and because they are seldom calibrated by material tests as
recommended. Because of this, accuracies of only 5–10 % are common. Therefore,
their use for Primary Metal Accounting is not recommended unless the use of static
weighing is not possible.

Coriolis mass flow meters are capable of high accuracy, ± 0.2% of reading in
certain cases, but they only have limited application in the extractive industry, as they
require low fluid velocity and they are sensitive to the quantity of entrained air.

Ultrasonic transit time meters have limited applicability for specific applications and
in those cases, they can give an accuracy of 0.5 to 2% of the reading.

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Momentum (impact) mass flow meters can be used for free flowing solids and they
are capable of achieving an accuracy of ± 1.0% of the reading.

Differential pressure type meters are not recommended for accounting


measurements, as there are too many cumulative sources of error.

3.3 METHODS OF MEASURING MASS


The various static and dynamic methods and equipment for measuring mass are well
covered in the literature. Colijn1 (1983) describes the equipment and gives guidelines
for selection, installation, operation, maintenance and calibration. Major suppliers
provide similar information for their equipment.

Similar information for the various types of mass and volume flow meters is given in
various textbooks and publications.

The various methods for measuring mass are listed below. Their applicability and
the recommended guidelines or Standards are covered in the sections which follow.

• Static Weighing (Platform, Truck and Rail Weighbridges)


• Static Weighing (Weigh Hoppers, Bins and Gantry Scales)
• In-Motion Weighing (Rail and Road)
• Conveyor Belt Weighers
▪ Electro Mechanical
▪ Nuclear
• Flow Meters
▪ Volume (differential pressure, turbine, electromagnetic, variable area,
vortex, positive displacement, thermal, ultrasonic – including Doppler
and transit time differential methods) all of which require measurement
of the density in order to determine mass flow
▪ Mass (momentum, impact, torque, Coriolis)
• Survey Techniques (land or aerial, photogrammetry, laser)
• Draught Surveys
Differential pressure type meters are generally not recommended for accounting
measurements, as there are too many cumulative sources of error. Flow meters,
other than electromagnetic, Coriolis, momentum, or transit time types, only have very
limited applicability for the measurement of flow in closed conduits in the
mining/metallurgical industry. They are generally not accurate enough for accounting
purposes, especially on slurries, and therefore are not covered in this Code.

All methods using volume or volume flow determination require the measurement of
the bulk density of the material in the stockpile or bin, or the specific gravity
(relative density) of the slurry or liquid. This can be performed by using a nuclear
(gamma) gauge (Section 3.7.2), in a few cases by a penetrometer (Section 3.7.4),
or preferably by bulk or laboratory tests (Section 3.7.1). The dry relative density of
the solids and the density of the carrier, in the case of slurry flow which is often water

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(which may have a density greater than 1.00), are also required. The mass flow is
computed by multiplying the flow and density signals and integrating on a continuous
basis

However, density determination can be a cause of error. In the case of stockpiles,


for example, although it is possible to measure the volume accurately, with sufficient
time and effort and with modern survey techniques, it is difficult to determine the in-
situ bulk density and even more difficult to obtain a representative sample, especially
if the pile is not homogeneous. This should be considered when stockpile surveys
are performed.

3.4 MASS FLOW MEASUREMENT

3.4.1 Mass Flow in Rail/Road Trucks

3.4.1.1 Static Weighing


Road/rail weighbridges and platform scales

Material in, or being loaded into or unloaded from, rail or road trucks is usually
weighed on static weighbridges or platform scales, as this is the most
accurate method. The equipment is described by Colijn3.

The method used is dependent on the quantity of material to be weighed,


whether it is in identifiable batches (lots) and on the packaging method
(drums, bags, bulk).

In all cases the principles are the same:

• The gross weight is established by weighing the full truck/container


• The truck/container is weighed empty and the tare is established and
then deducted (or the reverse of the these two steps for loading)
• Representative samples in terms of recognized procedures are taken to
determine moisture content by standard tests
• The dry weight is calculated
Calibration and Certification
These scales may be readily certified (assized), and in some cases have to
be so by law or contract. For the purposes of Primary Metal Accounting they
must be certified.

The design, installation, operation and calibration are covered by International


and National Standards and National Metrology Acts. For certification, these
scales have to comply with certain design specifications, permissible
acceptance tolerances or levels of accuracy when new, and maintenance
accuracy levels for equipment in use, which define the limits of allowable error
or departure from true performance or value, based on the defined test
procedures as laid out in the Standards. These accuracy levels are defined
for the various classes of scales (Appendix C.1.1.). They are calibrated by

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Certified Weights traceable back to the relevant National Prototype
Kilograms and thus to the International Unit of Mass. The test weights and
the test scales to weigh them are in turn certified in terms of National
Standards. The test equipment to weigh test weights has to be capable of a
greater degree of accuracy than the commercial scales (Appendix C.1.1)
National bodies or companies, who have been accredited by the national
authority, perform the certification. The precision and bias can be evaluated
by statistical techniques such as those detailed in ISO 3534.1.

Hopper/Bin Scales and Gantry Scales

Hopper/Bin Scales, either singly or in pairs, are also capable of good levels of
accuracy although they require a more elaborate installation for loading or
offloading of the materials. The equipment, design and installation guidelines
and calibration techniques are described by Colijn4 and in literature available
from the equipment suppliers. Gantry scales are usually used for bulk
offloading of ship cargoes. These scales can be calibrated with certified test
weights as for the platform scales and weighbridges and they can be certified
by the relevant authorities.

3.4.1.2 In-Motion Weighing


In-motion weighing is the weighing of materials in road or rail trucks or other
containers, whilst the containers are in motion.

This is usually used for large quantities such as bulk commodities transported
either by road or by rail. The various types are described in Colijn5, who also
lists installation guidelines and factors affecting the uncertainty of the
measurement.

The various possibilities for in-motion rail weighing are:

• Single Draught Gravity: the weighing of an entire uncoupled rail car


which is moving slowly by gravity down a slight decline. This requires a
long weighbridge
• Two-Draught Gravity: similar to the above, except that each bogey of
the rail car is weighed separately and thus the weighbridge is shorter
• Single Draught Coupled: the entire span of trucks moves slowly
through the weigh area. All cars have to be the same length coupler to
coupler and the weighbridge the same length as the cars
• Two-Draught Coupled: same as the above, except that the
weighbridge is shorter than the single draft coupled and each end of the
car is weighed separately
• Axle Weighing: same as the above, except that individual axles of the
wagons are weighed, using a short rail section with strain gauges which
means multiple weighings for each rail car (with the number being
dependent on the bogey design)
The accuracy of in-motion weighing for rail trucks is dependent on:

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• the track layout at both ends of the weighing section (which should be
straight and level)
• the fastening of the rails on these approaches (in concrete)
• constant speed over the weighing section (less than 8 km/hr)
• good maintenance of the track and rolling stock to reduce impacts and
vibration.
Train speed must be monitored automatically and, ideally, it should be controlled.
Where applicable, special lightning protection must also be installed.

In theory, the individual weighing of complete, uncoupled trucks should give the most
accurate result. However, modern in-motion weighers normally weigh individual
axles on a coupled basis, as this is simple, more rapid and practical to perform and
the software can compensate for coupling and speed effects. The multiple weighing
of individual axles provides a larger number of readings, which can assist in
evaluating the results and improves the average deviation over a measuring period.
For more accurate installations it is common to have four or eight strain gauges.
Previously train speeds were limited to 8km per hour for certification but with the
latest equipment it is possible to operate up to 20km per hour or higher.
Rail in-motion weighers can be calibrated and certified according to various
standards and national Trade and Metrology Regulations (in South Africa this is
covered in Regulation 61) and used for custody transfer purposes. However,
certification is not possible for road trucks at present because of the variable
accuracy due to the effect of truck speed and the acceleration or deceleration, which
is difficult to control.

If the equipment is adequately designed, installed, maintained, calibrated, and


operated (especially with respect to train speed), a precision of ± 0.5% should be
achievable, assuming that the empty trucks or trains are also weighed on the system
and the tare established on every weighing.

3.4.2 Mass Flow of Feed Materials, Products and Intermediates


Products must be weighed by one of the static methods in order to obtain the highest
accuracy. For material being packed into drums, bags, or other containers, the net
weight must be established by measuring the tare (empty weight) and the weight
after filling, by means of a platform scale. A bin scale delivering a preset weight may
also be used. In addition, the dispatch gross weight is established, after loading the
truck, on a weighbridge. As solid materials often contain some moisture it is
important that samples are taken, preferably during loading or unloading, to establish
moisture content.

The mass flow of feed materials, or inter/intra plant intermediates (e.g. matte),
required for Primary Metal Accounting, must be weighed in the same manner or by
in-motion weighing, even if not required commercially, or by belt conveyor weighing,
as specified below, with the weighing equipment certified, since these streams are
critical for Metal Accounting. However, it may be decided, after due assessment of
the risk to the company and an evaluation of the costs/benefits, company needs and
practical limitations, that certification is unwarranted. In these cases, suitable in-

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house procedures for calibration, operation and maintenance of the equipment,
based on the appropriate standards and legal requirements, must be drawn up and
applied and an Exception Report motivated and agreed in terms of Company
procedures to permit such uncertified operation.

Where a product is transferred from one plant to another, it is good practice for the
mass to be measured at both loading and unloading points for on-going comparison
and error determination.

3.4.3 Mass Flow on Conveyors


Belt scales (weighers) enable the continuous weighing of large quantities of materials
travelling on conveyor belts without the disruption to the process that batch weighing
can produce. Belt weighers are divided into three accuracy classes (OIML R50-1
1997).

These are shown below:

OIML Class Maximum Permissible Errors for the Calculated Load


Initial Verification In Service
0.5 ± 0.25 % ± 0.50 %
1 ± 0.50 % ± 1.00 %
2 ± 1.00 % ± 2.00 %

As a minimum requirement, weighers conforming to the maximum permissible errors


allowed in OIML Class 0.5, or an appropriate equivalent local national standard, must
be used for Primary Accounting, trade, commercial and custody transfer purposes
and they are the only weighers that can be certified (assized). OIML Class 1 (or
equivalent) is required for Secondary Accounting and Class 2 for less critical
applications such as plant control. Although no ISO standard exists, various other
national Standards specify the allowable precisions for the various classes of these
weighers and they are largely based on the principles in the OIML recommendation.
It should be noted that some of these Standards may refer to a different number of
classes or to no class, (there were only two classes in the previous edition of the
OIML recommendation), with JIS B 7606 having six classes and the NIST 44
handbook only referring to a single class and specifying a maximum tolerance of
0.25% of the test load for both maintenance and acceptance tolerances on material-
run tests. It is important therefore, for certification, to ensure that national
regulations are met, as specific requirements and specifications for testing can be
slightly different.

Static scales are in general more accurate than belt scales, and they are also
capable of greater sensitivity, because they weigh larger quantities of material at
one time. In addition, the accuracy of belt scales in operation is often considerably
poorer than that expected, based on the specification of the scale, because of poor
choice, system design, or bad operation or calibration.

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The weight recorded by the belt weigher is the wet weight, as most materials contain
moisture. This moisture content is often variable and it is important that samples for
moisture determination are taken at regular intervals using approved procedures, to
enable an accurate moisture determination. Moisture for a few materials (fine,
consistent) can also be determined continuously by a nuclear neutron gauge
(Section 3.7.2) or a microwave gauge (Section 3.7.3). The former is applicable
mainly to material in piles, bins and tanks and the latter to belts, chutes or conduits.

Certification
Certain makes and types of belt conveyor weighers and installations can be certified
(assized) for trade (custody transfer) purposes, as they are, for example, in the
supply of coal to power stations. Certification is installation specific and procedural
requirements may vary from one country to another. For commercial and Primary
Metal Accounting purposes, belt weighers must be certified in terms of this Code.
Where, after an assessment of the specific application, material and importance of
the process stream, the practicality and cost of achieving an installation of the
required standard and the risk to the company, it is decided that certification is not
warranted, an Exception Report must be motivated and agreed, by the Company’s
approval procedure, to permit uncertified operation. However, even in these cases,
the design, installation, operation and calibration should be in accordance with
suitable and clearly defined in-house procedures, so that a maximum error of ± 0,5 %
can be achieved and maintained.

3.4.3.1 Electro-Mechanical Weighers


The components of these weighers and the sources of error are described by
Colijn6, as well as the key factors for choice, design and correct installation
(Colijn7). The factors affecting accuracy are discussed further in Section 3.2

The basic components of an electromechanical belt scale are the following:

• The scale suspension (weighing) section on the conveyor which


transmits the load on the belt to the load cells sensor(s)
• The load sensor(s) which converts the load force to a form acceptable to
the mass totaliser
• The belt travel speed pickup which contacts the belt and transmits the
belt speed to the speed sensor
• The belt travel speed sensor which converts the belt speed to a form
suitable to the mass totaliser
• The mass totaliser which computes the mass travel over the conveyor
scales and indicates and records that value
The scale suspension must be rigid with torsional stability and designed with
minimal flat surfaces to reduce spillage build-up; it must also be capable of
withstanding high temporary over-loads. The suspension may have a single
weigh idler or multiple weigh idlers (up to 6 to 8) and it may be of various
designs such as pivoting, floating, counterweight etc (Colijn2). Modern belt
weighers are sometimes fitted with counterweights to counteract the weight of
the empty belt and thus increase sensitivity. In general, more weighing idlers

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improve accuracy. For Primary Accounting usually 4 to 6 weighing idlers are
required to achieve the necessary accuracy. However, the choice is specific
to the installation and two weigh idlers may be suitable in certain less onerous
applications. The load sensors may be single or multiple load cells and either
with direct bearing or with the load transmitted to them by a system of levers.
Information on the calibration of load cells may be found in OIML 60 and BS
8422.

The optimum choice is installation specific and scale suppliers have


guidelines for selecting the best option, as well as for the correct conveyor
layout and design, to achieve good tolerances in a specific application,
according to the requirements of various Standards (both for new installations
and for retrofits). The NIST requirements (Appendix C.1.3.) linked to OIML
Recommendation 50 are generally used, however, various countries have
their own requirements (for example in South Africa requirements are
specified in the Trade and Metrology Act 1973 Regulation 47).
The key requirements (Colijn7) for a conveyor belt weighing installation in
order to obtain the accuracy required for certification are:

• Conveyor should be close to horizontal and relatively short (less than 70


metres)
• Ideally the conveyor should have no curved (catenary) sections, but if
this is not possible the conveyor must not have a curved section
between the loading point and the scale and not closer than 6 metres or
5 idler spacings beyond the scale if convex, or at least 15 metres to the
curve tangent if concave
• The conveyor should be in contact with the idlers on the scale and the
three approach and lead idlers at all times
• Conveyor must be endless with any joints being smooth (spliced)
• Conveyor should be sized to assure at least 80% of volumetric loading
capacity, the belt loading centred and the belt as light and flexible as
possible for the intended service
• Maximum troughing angle for the idlers should be 35 degrees
(preferably 20)
• Conveyor stringers through the weigh region should be continuous and
of sufficient size to limit deflection and promote good alignment
• Conveyor take-up should be of the automatic counterweighted type
• Conveyor loading feeding system should supply as uniform and
constant a load as possible, within 50-90% of the scale range
• Conveyor weighers should be protected from wind, weather and
extreme or rapid temperature variations
• There should be no tripper on the conveyor
• The idlers in the weigh region must be carefully aligned to the specified
tolerances and the rolls within the specified eccentricity

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• The scale should be located between 6-15 metres from the loading point
• Side skirting or training idlers should not be closer than 6 metres to the
weigh section
The layout of the weighing system and conveyor should be such as to permit
calibration of the weigher with chains/ weights and the check weighing of the
material by weigh hopper or weighbridge for calibration purposes.

The accurate measurement of the belt travel speed is as important as the


mass on the conveyor and any error is directly proportional to the mass flow.
Various methods can be utilised. Their advantages and disadvantages are
summarised in the literature (Colijn8). For Metal Accounting, belt speed
measurement must be derived from a cylinder or wheel in contact with the
belt itself.

Calibration and Certification


Various calibration methods exist, such as dead (static) test weights,
calibration dynamically with an installed test weight, test chains of a certified
weight per metre and the material-run (bulk test) method. The latter is
preferred as it involves passing a known weight of the material, normally
measured by the weigher, over the actual weigher in the normal operating
mode and is the only acceptable method if the scale is to be certified. This
requires facilities such as reference weigh bins or weighbridges to test weigh
the material passing over the scale to a higher level of accuracy (± 0.1%
according to NIST Handbook 44) than that required for the belt scale being
calibrated. Calibration should cover a range of 20% to 100% of the belt
loading (NIST 44). Test chains are the next most suitable method

A new scale should be calibrated at the supplier before delivery, to establish


the tolerance and the initial intrinsic error (the laboratory tolerance for many
belt scales is often less than 0.1%). A new installation should then undergo
an Acceptance Test on site to establish the intrinsic error. For certifying
purposes, this should show a maximum error of ± 0.25 % (NIST 44 and OIML
50). Calibration according to recognised procedures gives the K-Factor
which is the factor (bias error) resulting from comparing the result of a bulk
test, to the theoretical calibration of the scale with test weights. This gives a
measure of the installation effects such as belt tension. For correctly
designed installations, this should be close to zero, which means that the
scale will tend to be much more stable. To maintain accuracy, zero balancing
should be performed frequently as well as a check with a static weight. The
frequency of material-run or chain calibration is dependent on operating
experience on the specific installation (periods of 3–6 months are common).
For critical applications, two belt weighers are often installed in series. This
provides a check on when any problems occur and the comparison can be
used to calculate the precision of the measurement (Merks1).

Certification has to be performed by an accredited company in terms of


specific country legislation, which is normally contained in the relevant Trade
and Metrology Acts, which, in turn, are usually based on OIML 50. If local

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standards do not exist for certification, the Best Practice is to adhere to OIML
50.

Most modern weighing installations are fitted with electronics for the
integrator, that facilitate the calibration and resetting of the speed zero and
span and the mass zero and span automatically, and accepting the
instrument readings as correct. However, there is no substitute for
fundamental checks of belt speed by timing a measured distance of travel
and of belt loadings by calibration with check weights. All these results, both
the as found and corrected, must be recorded and analysed to establish the
operating accuracy of the weigher.

3.4.3.2 Nuclear Belt Weighers


These use the principle of the absorption of nuclear (gamma) radiation to
measure belt loading and the relevant national nuclear authorities control their
use and maintenance. Suppliers provide guides to the selection of
electromechanical or nuclear weighers for a specific application.

They are simple to install and they are unaffected by belt effects, so the
conveyor design is not as important as it is for electro-mechanical weighers.
Nuclear belt weighers are also not susceptible to external forces such as
wind, they are less maintenance intensive and easier to calibrate. However,
they have the same operational limitations with respect to the measurement
of belt speed, plant housekeeping, moisture determination and regular
calibration. Most importantly, they are affected by variation in the size,
composition and shape of the material being measured and they are therefore
normally less accurate than electromechanical weighers, with maximum
errors of ± 1 to ± 2% being achievable, but higher error levels being common.
They can also be used, in certain applications, with nuclear neutron sources
to determine moisture content. Because of the fact that their measurements
are subject to errors from variations in the material being weighed, they
should not be used for metal accounting measurements.

3.4.4 Mass Flow in Conduits

3.4.4.1 Introduction
For convenience and practical reasons, mass flow in closed conduits is often
determined by measuring volume flow rate plus density or specific gravity in
order to calculate the dry mass. This type of measurement is very common in
the extractive industries for process flows and liquid and/or gaseous effluents.
The determination of the relative density or specific gravity is discussed in
3.6. The degree of uncertainty in the mass flow is made up of errors both in
the volume measurement, and in the density determination.

There are over one hundred types of flow meters commercially available,
operating on ten different principles. BS EN 7405 classifies flow meters into
12 different Groups (Strauss18). There is extensive literature available from
suppliers and many technical papers (Appendix B.1.) and standards
(Strauss19) on the selection of the correct flow meter for specific applications.
Strauss20 gives a comparison of the performance of different types of flow
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meters and Strauss21 shows the possible applicable areas for the different
types of flow meters for the twelve Groups. However, in the metallurgical
industry, many of the key process flows, in conduits, required for metal
accounting, are abrasive slurries containing a significant amount of solids.
This effectively limits the choice of a suitable meter for these applications to
an electromagnetic flow meter. In a few cases, with low flows and fine
particles, it may be possible to utilise a Coriolis mass flow meter, or for low
consistent solids contents, transit time ultrasonic flow meters may be suitable.
For free flowing solids, momentum type mass flow meters may be used.
Thus, this guide will concentrate on these four types. For relatively clean
solutions, many types of flow meter will operate satisfactorily and give good
accuracy. The measurement of gas flow, with or without particulates, for
metal accounting is normally required for off-gases and stacks, and it needs
specialist equipment but is not covered in detail in this Code.

3.4.4.2 Specifications and Performance


Often claims of accuracy for flow meters are ambiguous and misleading. The
three essentials for performance specifications are:

• Accuracy (total measurement uncertainty over the measuring range)


• Measuring range
• Traceability of the calibration back to a certified or approved flow
measurement.
The total uncertainty is made up of that associated with the reference (the
“true” value) plus that from the specific meter being tested. For flow meters
used for metal accounting purposes, these aspects are critical. Therefore, the
uncertainty of flow measurement must be specified and the specifications
must conform to ISO 11631. This standard defines the methods of specifying
the flow meter performance and the different classes of traceability from
Group A to F. For metal accounting, this must be Group A if possible, or at
least Group B.

3.4.4.3 Calibration and Certification


For metal accounting purposes the initial calibration and certification of the
meter must have been performed in accordance with ISO 4185 or ISO 8316
(or national equivalents) in a testing facility accredited in terms of ISO/IEC
Guide 25 or ISO 17025. This certification is carried out on water. The
uncertainty should be assessed utilising ISO/TR 7066-1 and 7066-2 and
ISO/TR 5168.

For critical metal accounting flows, such as thickener or flotation feed, where
the measurement is used for Primary Accounting, the instrument must be
calibrated regularly on the actual material in addition to the initial calibrations
conducted in the test facility.

Calibration can be performed in three ways:

• Volumetric method

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• Weight method
• Comparison with a standard meter
However, field calibration is often imprecise as frequently, inadequate
provision is made in the plant design and layout for calibrated weighing or
volumetric tanks and for a diversion system. In addition, the system has to be
accurately designed to ensure that volume or weight and the time of flow can
be measured to a sufficient degree of accuracy (which should be 5 times
better than that required for the meter). Although ISO 4185 and 8316 are
intended for accredited testing facilities, the principles are directly applicable
to in-plant calibration. It is also possible to remove the meters and test them
at the various approved facilities available. However, there is, at present, no
facility capable of testing the meters on slurries. This would also involve the
transport of a large quantity of the material to the facility. In-series installation
on site of a reference meter of proven stability and precision is a further
possibility.

3.4.4.4 Solutions
The measurement of the mass flow of solutions for accounting purposes is
mainly applicable in the industry to some process streams in the refining
sections of the process, and then usually only for intra-company accounting
or for the measurement of effluent streams, to determine losses or
conformance with permitted emissions. Differential pressure type meters will
operate satisfactorily (ISO 5167-1 gives the specifications for geometry,
operation and use), but at a lower level of accuracy than other types such as
magnetic flow meters. Thus they should not be used for Primary Metal
Accounting. The relevant standards, selection and calibration aspects are
covered in the section below on slurries.

3.4.4.5 Slurries
Electromagnetic flow meters

Slurries in the metallurgical industry are abrasive and normally have a range
of particle sizes, operating in the mixed-flow regime. Electromagnetic flow
meters are the most suitable for this application, providing the fluid is
conductive. They are available in a wide range of sizes and materials of
construction to suit the application. The measurement is unaffected by
pressure, temperature or viscosity. The measuring tube has no moving parts
and there are no restrictions to the pipe cross section.

However, they can only be used on conductive liquids and they are affected
by changes in the mineralogy, particle size, velocity and magnetic
constituents in the slurry. Meters of special design are available to handle
these magnetic materials and they give satisfactory results, providing the
magnetic content of the slurry is reasonably constant. Electromagnetic flow
meters are capable of giving an accuracy of ± 0.5% of reading or better on
water or clean solutions, providing they are installed correctly and calibrated
according to standard procedures. For slurries the accuracy is generally
lower.

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Flow meters should be manufactured in accordance with an international
standard. Standards (ISO 6817, ISO 9104:1991, ISO 13359, ASME MFC-
16M-1999) for the installation, calibration, and methods of evaluating their
performance must be adhered to. Manufacturers also provide recommended
parameters for installation. It is important that safety and health
considerations are taken into account in the installation to allow safe
operation, maintenance and calibration.

Coriolis Mass Meters


These meters measure mass flow directly by measuring the Coriolis force that
is developed when mass flows through an oscillating tube. They eliminate the
uncertainty of the density measurement, they are capable of an accuracy of
± 0.2% of reading and they require little space. However, they are relatively
expensive, unavailable in large sizes at present and, because of geometry
and erosion in the case of slurries, they can only be applied where the fluid
velocity can be kept under 2 m.s-1 and the products are relatively fine. A
possible application is for the measurement of flow of mineral concentrate.
Note should be taken of the fact that the accuracy of these meters is badly
affected by entrained air. Coriolis meters also give a measurement of the
density of the fluid. Standards (ISO 10790:1993/2003, ASME MFC-11M-
2003) give guidance on the selection, installation and use of Coriolis meters
and these standards should be followed. The general comments above on
certification and calibration are also relevant.

Ultrasonic Transit Type Flow Meters


This method (ISO TR 12765) utilises the fact that a fluid directly influences
the propagation velocity of sound waves within it. They can be fitted to the
exterior of pipes thus making retrofitting simple. If the fluid is homogeneous
they are unaffected by the physical properties. However, they require a
uniform flow profile and the accuracy is strongly dependent on the acoustic
transparency of the fluid and it ranges from ± 0.5 to ± 2% of full scale. Thus
applicability for Metal Accounting purposes is limited.

Calibration
If used for critical metal accounting flows, such as concentrate, thickener or
flotation feed, because static or conveyor belt weighing is not possible, the
flow meter must be calibrated regularly on the actual material as outlined in
3.4.4.3.

3.4.4.6 Solids
Impact mass flow meters can be utilised for free-flowing solids and they
operate by measuring the momentum of the solid stream impacting on a
measuring plate. They are described in Colijn9, who also discusses their
applicability and limitations. They are unaffected by the density of the
material and are pre-calibrated by the manufacturer for the user. Calibration
checks are with test weights and do not require material tests. They measure
wet mass flow and can give accuracies of ± 1%.

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3.4.4.7 Gases and Dusts
The mass flow of gases and dusts is required to measure the losses of
valuable materials in the dust, or the particulate content and the mass of
pollutant gases such as SO2 or NOX, from stacks or fugitive emissions into
the atmosphere, in order to measure conformity to environmental, health and
safety provisions.

The valuable component is normally very small (less than 1% of input) and
thus errors resulting from the measurement are seldom significant in the
overall metal balance calculation. However, because of the risk to a
company’s reputation from unauthorised emissions or from exceeding the
legal regulations and the emphasis on the triple bottom line, these
measurements are important.

Mass balancing for Environmental and Health needs is discussed further in


Section 7.7.1.

3.4.5 Mass Flow in Open Channels


For metal accounting, the measurement of flow in open channels would usually be
required for the measurement of effluent volumes to determine losses, which are
usually a small percentage of feed, or to check conformity with environmental
regulations and permits. Normally the solids content is small and the mass would be
derived from separating and weighing the solids from the samples taken for analysis.
An exception is concentrator tailings that are usually pumped in closed conduits.
This loss may be significant (5–20% of the feed) and the stream critical to Primary
Accounting. However, because of the difficulty in measuring the flow rate accurately,
the mass flows are often calculated by the two- or three-product formulae, from the
mill or float feed and concentrate mass flows and analyses. This practice must be
motivated by way of an Exception Report.

For the same reasons as given in 3.4.4.7, the measurement and accounting for
certain trace elements and potential pollutants has great significance for a company’s
reporting. This is discussed further in 7.7.2.

ISO/TR 8363 gives the guidelines for the selection of appropriate methods and lists
28 different methods for measuring flow in open channels that include velocity-area
methods, weirs and flumes. This standard also gives the expected degree of
uncertainty for the various methods varying from ± 10% for some to ± 1% for a thin-
plate, V-notch, sharp crest weir (ISO 1438-1) and it lists the various ISO standards
applying to all the different methods. Thin plate weirs must be used for accounting,
for process streams such as effluents, as they are the most accurate form of
measurement for this purpose.

3.4.6 Mass Flow for Bulk Commodities


Mass measurement for bulk commodities such as coal, bauxite, iron ore, or base
metal concentrates is normally carried out by static, in-motion or conveyor belt
weighing, to the degree of accuracy required in terms of the contracts of supply and
to meet the requirements for custody transfer. Thus, the weighers must be certified.

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These materials are often shipped direct in bulk from the supplier to the port, loaded
onto a bulk carrier and unloaded at the consumer’s port for onward supply to the
treatment facility.

Draught Surveys
In these cases, a method commonly specified and accepted for material being
transported by bulk carrier is that of the draught survey.

The draught survey is a mass measurement based on converting a difference


between the displacements of a vessel under different loading conditions into a wet
mass for a partial or full cargo. A suitably qualified marine surveyor, who operates in
terms of accepted formulae, performs the survey. A reasonable accuracy is
obtainable for full cargoes but partial cargoes or parcels are susceptible to a higher
degree of uncertainty. Accuracy is also affected by external factors such as water
density, currents, wind and waves and the skill of the surveyor.

There is not, at this stage, any ISO standard covering draught surveys but, in some
cases, the UN ECE Code for Coal Cargoes is used. There is also no degree of
traceability for the survey technique. This should be contrasted with a certified belt or
other type of weigher, the calibration of which can be traced back through a hierarchy
of testing to internationally accepted weight standards.

Marine surveyors quote an accuracy of ± 0.5% for full cargoes. Merks (1992) has
suggested, in an analysis of the precision of some draught survey data that the
coefficient of variation varies from 1% for full cargoes to 3% for partial cargoes. This
should be compared with that achievable from static scales or more advanced belt
scales as discussed elsewhere in this Code. On critical measurements, it is also
possible to improve the quality of the mass measurement by installing two belt
weighers in series and comparing the results continuously. However, the method of
mass determination for these custody transfers is usually specified in the sales
contract and in many cases, this is still the draught survey. Even where static or belt
conveyor weights are accepted, the draught survey is performed as a check and for
shipping purposes.

3.4.7 Mass in Storage Areas


Mass in storage areas can be a significant quantity and it can be material to metal
accounting. It is usually difficult to determine to a level of accuracy sufficient for
accounting purposes, and it can conceal mass measurement and accounting
discrepancies if it is measured only by difference and it is not cross checked by other
means such as reducing the stock to zero.

3.4.8 Mass in Stopes/ Ore Blocks


At this stage, this is not included in the Code, as the starting point for metal
accounting has been taken as the ore feed to the treatment plant. However, the
mass measurement and metal content at the treatment plant must be tracked back to
the shaft or open pit and reconciled with other mass measurements for the broken
ore, with surveyed measurements for the in-situ rock mined, (utilising the in-situ rock
density) and any stocks of broken ore underground or in the pit.

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3.4.9 Mass in Stockpiles
Measurement of mass in stockpiles is subject to a high degree of uncertainty. It is far
better to sample and weigh the input and output, which can usually be performed to a
higher level of accuracy, and calculate the contents of the stockpile by difference.
The recommended practice for stockpile assessment is to have a system of dual
parallel piles, which must be emptied at regular intervals.

It is possible to measure the volume of the stockpile to an accuracy of better than


± 5% using photogrammetry or computerised automated laser survey techniques,
which provide a 3-D image. The accuracy is dependent on the number of survey
points taken and these measurements have to be performed by qualified surveyors.
However, the measurement of the bulk density of the material in the stockpile, the
moisture content (where practical, in the case of higher value materials such as
concentrate, it is better for the stockpile to be under cover), and obtaining a
representative sample is much more difficult. The bulk density of many materials is
changed by compaction, ageing, swelling or oxidation and it is also affected by
stockpile practice such as trucks driving over the pile and the method of dumping.
Methods of measurement of bulk density are discussed in Section 3.7.

If the material is not homogeneous in size and content, sampling of a stockpile to the
accuracy desirable for metal accounting, is almost impossible. The uncertainty of the
metal content could be as poor as ± 15%; the only time when a stockpile value is
correct is when it is empty. In the case of bulk commodities, such as coal or iron ore,
where the material is reasonably consistent, and where the contents are large and
material to the operation, a survey may be useful as an independent check on other
tonnage measurements.

For other stockpiles, such as ore or intermediates, it is suggested that accurate


surveys should be performed only when measurement in and out is not possible, or
the value of the stockpile is material to the company’s results, or the content of the
stockpile has changed significantly over the accounting period for some reason,
and to fit in with reporting periods. The accuracy of the survey is dependent on the
number of survey points taken, which should be tailored to suit the expected
accuracy of the other variables and the importance of the value.

International Standards do not exist and the accuracy of the survey is dependent on
the skill of the surveyor.

3.4.10 Mass in Tanks and Bins


The measurement of mass in tanks or bins suffers from the same problems as those
found in stockpiles. Although the volume can be calculated reasonably accurately
from surveys, the tank or bin geometry, the level, the measurement of density and
sampling are all problematic. In the case of slurries there is also the possibility of
dead volumes, solids build-up or the concentration of the specific component (e.g.
gold) in some areas.

For the purposes of metal accounting, often it is the change in stock or inventory that
is significant. If the metal content is critical, such as in the PGM or gold industry,

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then the only solution is to empty the tank or bin for the periodic stock-take. Use of
parallel processing lines or storage facilities can be used to assist in this.

3.5 MASS IN PROCESS INVENTORY


The effort and resultant accuracy to determine these are dependent on the quantity
and value relative to the company’s income. Thus in the case of precious metals it is
essential on an annual basis, in the final refining operation, to use a method similar to
the bubble method to both check the material and empty the equipment in the
various stages. This assumes added importance if mass balance calculations show
significant abnormalities.

3.5.1 Transient
This is defined as process inventory (or lock-up) that is of short-term duration
because of some process disturbance and/or where the mass flow through is
continuous and live. It is normally contained in process vessels and equipment such
as mills, furnaces and reaction vessels. This can be estimated and calculated with
the same caveats as for tanks and bins above. It is possible that the accounting
metal can be present in more than one phase (e.g. solid and liquid, concentrate,
matte and slag) in which case estimates must be made for all phases. Normally,
estimates are made monthly, with periodic stock-takes to a more accurate level to
suit company reporting.

3.6 LONG TERM


Long-term process inventories are those that will remain for years, or the life of mine
or of that particular piece of equipment, and they include such items as:

• The dead load in silos


• The gold in mill liners
• The build-up in furnaces.
This inventory can be subdivided into:

• That which is absorbed or trapped in the process, such as gold into concrete
foundations, which can only be recovered when the plant is dismantled and
demolished (permanent inventory)
• That which is recovered at regular intervals such as when mills are relined or
furnaces re-bricked (semi-permanent inventory).
Measuring and assigning quantities to the former is very difficult and must be avoided.
(However, a “rule of thumb” figure used for early generation South African gold
plants of 0.3% of total gold input over the life of Plant has been confirmed by clean
up on closure). Quantities for the latter must be quantified and updated as the
inventory is periodically removed and this information carefully documented for future
use.

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3.7 DENSITY AND MOISTURE MEASUREMENT
The importance of density and moisture to mass measurement has been highlighted
in previous sections. In this context the Code refers to moisture that can be removed
from the sample by drying at temperatures up to 105 oC, as water can be present in
the material in different forms including the water of crystallisation.

In the Coal Industry, for example, the following are examples of the various types of
moisture that may be present in a sample:

• Free moisture
• Surface moisture
• Residual moisture
• Inherent moisture
• Equilibrium moisture
• Moisture holding capacity
• Total moisture
• Moisture in the analysis sample
• Hygroscopic moisture (lignite)
• Moisture of constitution
It is important to ensure that samples for moisture determination are taken in such a
manner, as specified by the Code, to ensure that the moisture in the sample is
representative of the material being weighed and that no evaporation can take place,
or water ingress occur, before the determination takes place. It is also very important
to ensure that any analysis is carried out on the sample that has been used for
moisture determination, or an appropriate correction made, in order that the
analytical result can be related directly to the dry tonnes value.

The measurement may be:

• Measurement of moisture in the material in road/rail trucks or other containers


• Measurement of the moisture content in material on a conveyor belt
• Measurement of moisture content of a material in bins/hoppers or stockpiles
• Bulk density of material in bins or stockpiles
• Specific gravity (SG)/relative density of slurry flowing in a conduit or in a tank
or other vessel
• Relative density of the solid and liquid components of slurry
The uncertainty in the density measurement has a direct effect on the resultant
calculated dry mass and it can be large, as for example in the case of low SG slurries.
At an SG of 1.25, a 2% error in the density measurement translates into a 10% mass
flow error, assuming that the carrying fluid has an SG of 1.00. In operating plants,
this fluid is often recirculated water, which may have a varying SG. If the SG is 1.05
then the error in the above example will increase to 12.5%. Thus there is no point in

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measuring the volume flow to ± 0.5% if critical attention is not paid to the density
measurement, including both the solids and solution.

3.7.1 Bulk and Laboratory Tests


The most precise and preferred method for measuring relative or bulk density, is by
bulk, laboratory or plant tests whereby an accurately known volume is weighed and
the bulk/solid/liquid/slurry density is then calculated. The volume of solids can be
determined by various methods including displacement of liquid. For determining
moisture, a known weight of material is dried under defined conditions and the loss in
weight due to moisture is calculated. This can be applied to bulk ore, stockpiles (test
pits) and conveyor belts. The degree of uncertainty is mainly dependent on correct
sampling and sample handling. Great care must be taken in the sampling of slurry
streams. For example, the precision of the measurement derived from small specific
gravity flasks is usually poor.

In the case of stockpiles, the water test can be used whereby pits are dug in the
stockpile, the material removed and accurately weighed. The pit is lined with an
impervious membrane and filled with a measured volume of water. The number and
location of the pits is decided by sampling theory.

In some cases historical information based on previous measurements and tests can
be applied, including analyses and mineralogy of the material, but it should be
regularly reviewed and re-measured.

3.7.2 Nuclear Gauges


These use neutrons or gamma rays. Neutron gauges can be used to measure the
moisture content of some materials in tanks or bins or on a conveyor belt. They
measure the hydrogen content of the material from which the water content can be
calculated. As they measure total hydrogen content they must be calibrated and
corrected for materials that contain hydrogen in forms other than water. If used in
conjunction with gamma belt weighers on a conveyor belt, which will give the total
wet mass of the material, the dry weight can be determined. They are limited to use
with relatively fine and homogeneous products. Accuracies of ± 1.0% are claimed for
wood chips at 50% moisture and ± 0.5% for concentrate (Colijn10).

Nuclear gamma gauges are also used for measurement of the bulk density in
stockpiles or heaps but can only penetrate to about 30 cm. The most common use is
for density measurement of slurry flow in conduits, used in conjunction with an
electromagnetic flow meter. The correct choice and accuracy is installation specific
and guidelines supplied by the vendors must be adhered to.

The initial calibration must be performed in the field at two points on the scale by
measuring the weights of known volumes of water and slurry passed through the
meter. Accuracy is affected by many of the similar aspects that affect flow meters. It
is essential that the relative densities of the solids and the carrier solution are
checked periodically and that the calibration be checked regularly, by correctly hand-
taken samples for SG. The meters themselves are capable of ± 1% accuracy, but
this is often not obtained in plant conditions, due to poor installation, inhomogeneity
and particle size changes.

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3.7.3 Microwave Gauges
These can be used in similar applications to those for which neutron gauges are
suitable. They operate on the principle that the intensity and speed of propagation of
microwaves is influenced by free water molecules. The change in intensity and
velocity of the waves is directly related to the moisture content in the material.

3.7.4 Penetrometers
These instruments have limited use to determine the bulk density of stockpiles of
material such as coal of a relatively fine uniform size, by measuring the force
required to penetrate a cone to a known depth. They require a skilled operator and
cannot be used on stockpiles with varying size material or containing rocks, such as
ROM ore.

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4 SAMPLING

4.1 INTRODUCTION
Within the mineral and metallurgical industries, process streams are very often in the
form of a flow of coarse broken ore or slag, or in the form of a flow of slurried finer
material. Metal accounting balances for such processes demand that these process
flows are sampled accurately with precisions that will cause the accuracy of the final
balance to fall within set target range(s). The ranges, into which the balance
uncertainties for the various target elements or chemical species of interest fall
(referred to in what follows as a measurand), are prescribed by management
considerations of the financial risk associated with the uncertainties. These
uncertainties must be acceptable to any stakeholders in the operations as well as to
outside bodies that are prescriptive of corporate governance standards.

The accuracy of the final result of a sampling of a process flow for a given
measurand depends on four factors:

• The ‘correctness’ of the sampling device


• The presentation of the process flow to be sampled to the sampling device
• The accuracy of the analytical method employed to arrive at the final analysis
assigned to a sample
• The heterogeneity of the material to be sampled and the design of the
sampling protocol, including the sample preparation protocol
There are two types of heterogeneity associated with a process flow:

Intrinsic heterogeneity (IH) which is determined entirely by the size distribution of the
solids and the variation of the concentration of the measurand from one particle to
the next, within the various size fractions of the solids
Distributional heterogeneity (DH) which depends on the variation of the total
measurand concentration from one moment to the next, as the process flow passes
the sampling point.
In most cases, with appropriate investment in equipment and the correct
arrangement of the process layout, it is possible to present the process flow to the
sampler and to take ‘mechanically correct’ sample increments from the process flow,
so that the sample formed by the collection of the increments is unbiased. This will
invariably not apply to sampling of run of mine ore because of the difficulties
presented by the range of, and variations in, the size and grade of individual particles,
moisture, and the problems associated with the design of a multi-stage sampling
system to generate an unbiased laboratory sample from the primary sample. The
accuracy of the sample (the variance between the true average analysis of the
process stream over the sampling period and the final analysis of the sample)
depends on the heterogeneity of the process flow, the accuracy of the analytical
method and the number and mass of the increments taken from the flow.

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4.2 SAMPLING ERRORS
As described by Gy (1982), Pitard (1993) and Holmes (2004), amongst others, the
total sampling error (TE) of a particular sampling stage may be divided into
contributions from a number of independent components as shown in the following
equation:

TEi = FEi + GEi + QE2i + QE3i + WEi + DEi + EEi + PEi [Eqn 4.1]

where FE = Fundamental Error; GE = Grouping and Segregation Error; QE2 = Long-


Range Quality Fluctuation Error; QE3 = Periodic Quality Fluctuation Error; WE =
Weighting Error; DE = Increment Delimitation Error; EE = Increment Extraction Error;
PE = Preparation Error.

In terms of the total error in metallurgical accounting, the error due to the mass
measurement including moisture determination, and the error occurring during the
analysis of the measurands, must be added to this equation.

In addition, as discussed by Holmes (2004), the components in the equation apply


principally to sampling from moving process streams and, therefore, not all of the
components apply to every sampling situation. For example, long-range and periodic
quality fluctuations and weighting errors do not apply to blast hole sampling. Holmes
also makes the point that delimitation error, extraction error and preparation error
require special attention, because they can easily introduce bias into the
measurement process. However, this can be minimised with careful attention to the
installation and operation of correctly designed sampling systems. The other
components are largely random errors that can never be completely eliminated, but
they can also be reduced to acceptable levels by careful design of the sampling
system.

Delimitation errors are caused by the incorrect geometrical definition of the sample
increment, (e.g. a parallel cutter opening in a rotary sampler) and they can be
eliminated if all parts of the stream’s cross-section are diverted by the sample cutter
for the same length of time. Increment extraction errors occur when a sample
increment is not fully extracted, (e.g. part of a process stream is missed by the
sample cutter), and these errors can be eliminated by ensuring that the increment is
completely extracted without any loss of sample.

Weighting errors are experienced when sampling a moving stream that has a high
variation in flow rate. It is not usually a major problem (assuming that both the
minimum and maximum flow rates are correctly sampled) and they can be overcome
by regulating the flow rate prior to sampling. As a general rule, the weighting error is
negligible for variations in flow rate up to 10%, and acceptable for variations in flow
rate up to 20%.

Careful sample preparation practice will ensure that the preparation error PE is
minimised.

The potential effects of long-range and periodic quality fluctuations can be


established by conducting variographic experiments as described by Gy (1979) and

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they are minimised by taking frequent increments based on a random stratified
sampling scheme.

Having minimised all of these errors, Equation 4.1 reduces to:

TE = FE + GE + QE2 [Eqn 4.2]

And the sampling variance is given by:

σ2S = σ2FE + σ2GE +σ2QE2 [Eqn 4.3]

These variances can be determined from a variographic experiment in which the


quality characteristics of at least 30 individual increments, taken from a lot, are
determined in duplicate.

The differences between increments at increasing intervals, called lags, are


calculated. A plot of the results is called a variogram.

The value of the variogram VE(t) corresponding to a lag of t increments is given by:

VE(t) = Σ (xi+t – xi)2 [Eqn 4.4]


2(n-t)

where: xi = the value of the quality characteristic for increment i for i = 1, 2, 3, , n


n-t = the number of pairs of increments at lag t apart

The resultant variogram is called the ‘experimental’ variogram and it includes the
variance of sample preparation and analysis as well as the sampling variance. To
give the ‘corrected’ variogram, which provides information on the sampling error only,
the sample preparation and analysis errors must be subtracted.

Variograms can usually be approximated to a straight line, especially over small


values of t. It can, therefore, be assumed that:

VC(t) = AC + Bt [Eqn 4.5]

where: AC = the random component of variance of the corrected variogram


B = the slope of the variogram

The sampling variance for systematic and random stratified sampling for mass basis
sampling is then given by the following equations:

Systematic Sampling
σS2 = AC + BmL [Eqn 4.6]
n 6n2
where: n = the number of increments

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mL = the total mass of the lot

Random Stratified Sampling

σS2 = AC + BmL [Eqn 4.7]


n 3n2
For time basis sampling, mL is replaced by tL, the total time for sampling the lot.

The first and second terms of these last two equations, correspond to the short-range
and long-range quality fluctuations respectively. For systematic sampling, therefore:

σQE12 = AC
n

σQE22 = BmL [Eqn 4.8]


6n2
The variogram intercept AC is made up of two components:

• The segregation and grouping variance σGE2


• The fundamental error variance σFE2 for the particular increment mass used
for the variographic experiment
The fundamental error variance results from the particle to particle variation in quality
of the material making up the increment and it can be determined as described in
4.3..

As described by Gy, the fundamental error variance is proportional to the cube of the
nominal top size of particles in the sample and inversely proportional to the increment
mass.

The variogram intercept AC can, therefore, be expressed as:

AC = σGE2 + AFd3 [Eqn 4.9]


ml
where: AF = a constant
d = the nominal top size of the particles in millimetres
ml = the increment mass
A worked example of the calculation of a corrected variogram and the parameters
derived from it is given in Appendix B of the Australian Standard AS 2884.1–1997.

The relative variance due to intrinsic heterogeneity is equivalent to the fundamental


sampling error (FE) and the following sections focus on the intrinsic heterogeneity of
the solids, the manner in which the heterogeneity can be quantified and/or measured,
and the impact that this heterogeneity has on every stage of sampling and sample
preparation.

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4.3 STATISTICAL BASIS OF SAMPLING THEORY
The theory of sampling of particulate solids is based on a simple concept of how the
numbers of particles of different size and composition vary from one nominally
identical sub-sample of a material to the next. A conceptual ‘model’ of a
heterogeneous particulate material must be developed to understand how the
statistical concepts come together to provide results useful to sampling practice.

It must be imagined that the material is separated into various size fractions by
sieving or some other suitable method, and, that for each size fraction, the particles
are sorted into composition classes, as illustrated in the diagram below, and the
particles within each size and composition class are assumed to be identical. The
amount of detail concerning the particles can always be improved by increasing the
number of size and composition classes.

Composition > 1 2 3 4 . . . Nc
Size v 1
2
3
4
.
.
1 2 3 4 5 6 7 8 9 10
.
Class

Ns

Figure 4.1 Size and composition classes


th th
The particles in the i size and j composition class are taken to have a volume:

⎛ d i3 + d i3+1 ⎞
Vi = f ⎜ ⎟ [Eqn 4.10]
⎝ 2 ⎠
d d
where i and i +1 are the sieve apertures defining the i th size fraction and f is a
shape factor than can be taken to be 0.5 for blocky particles. The particle density is
ρ ij mij = ρijVi
denoted by which gives them a typical mass of . The concentration
a ij
of the measurand in the particles is denoted as .

With the definition of these values for the various size and composition fractions, it is
nij
then possible to describe a sample of material if the numbers of particles, , of
each type are known or specified. The measurand concentration in the sample as a
whole is:

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Ns Nc

∑∑a
i =1 j =1
ij m ij n ij
as = Ns Nc

∑∑m
i =1 j =1
ij n ij
[Eqn 4.11]

Where Ns is the total number of size classes and Nc is the total number of
composition classes.
and the sample mass is:

Ns Nc
M s = ∑ ∑ mij nij
i =1 j =1
[Eqn 4.12]
In order to understand the statistics of sampling of a lot of material, it may be
imagined that a substantial mass of the material is collected and each particle in the
lot is given a number starting at 1 and going up to some very large figure N. To
‘sample’ the material, a set of S numbers is drawn entirely at random, from the
numbers 1 to N, and the particles whose numbers are drawn are the ones taken as
the ‘sample’.

By selecting the particles in this way, there is no bias in favour of particles of any one
type. In fact, this ‘ideal’ method of sampling can be considered as a standard against
which any other method of particle selection for sampling can be compared. This
method is the most equitable possible method of selecting particles for a sample,
since the numbers of any one type of particle taken into the sample do not depend on
the numbers of particles of any other type taken into the sample, and it is often
referred to as the ‘equiprobable’ sampling method in discussions about sampling.

4.3.1 Intrinsic heterogeneity of a particulate material


To understand how the numbers of particles in a sample taken from a process
stream vary when a sample cutter is moved through the stream, (for example, at a
conveyor transfer point), it must be recognised that the number of particles taken into
the sample in consecutive motions of the cutter will vary, even when the mass flow
rate of the process stream is constant,

It follows from this description of the sampling process that the number of particles of
any one type that arrive in a sample follow a Poisson probability density. A number
following a Poisson distribution is characterised simply by its expected or mean value.
The expected value need not be a whole number, but the number of particles must of
course be integers.

The important aspect of the Poisson density is that the variance of the distribution is
equal to the expected value.

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This concept of the number statistics of the particles is all that is required to
understand how the concentration of the measurand varies from one nominally
identical sub-sample to the next. In the formula for the measurand concentration of a
sample, the number of particles of any one type in the sample follows a Poisson
distribution with an expected number of particles n ij ; the numbers vary
independently. Using simple propagation of variance rules, it is possible to show
that:

1 Ns Nc
Var {a S } = ∑ ∑ ( aij − a L ) m ij2 nij
2

M s2 i =1 j =1
[Eqn 4.13]
where the nominal measurand concentration in the sampled material (the ‘lot’) is:

Ns Nc

∑∑a
i =1 j =1
ij mij nij
aL = Ns Nc

∑∑m
i =1 j =1
ij nij
[Eqn 4.14]

Dividing through by aL in Equation 4.13 gives:

2
⎧a ⎫ 1 Ns Nc
⎛ aij − aL ⎞ 2
Var ⎨ S ⎬ = 2 ∑∑ ⎜ ⎟ mij nij [Eqn 4.15]
⎩ aL ⎭ M s i =1 j =1 ⎝ a L ⎠
This formula in terms of the particle numbers is not very convenient to use. It is
preferable to restate the formula in terms of variables that are more familiar. For the
nominal analysis of the material, the mass fraction in the I th size fraction is denoted
as Xi , and the mass fraction of material in the j th
composition class within the I th

size fraction as Yij . It is then a simple matter to convert Equation 4.15 to the form:

2
⎧aS ⎫ 1 Ns
⎛ aij − aL ⎞ Nc
Var ⎨ ⎬ = ∑XV i i ∑Yij ρij ⎜ ⎟
⎩ L ⎭IH
a MS i=1 j=1 ⎝ L ⎠a [Eqn 4.16]

This formula relates the relative variance (the square root of the left hand side is the
relative standard deviation, expressed as a fraction rather than a percentage) of the
measurand concentration between nominally identical samples of mass M s to the
size distribution and the composition distributions within each size fraction. At a
given state of comminution, the size and composition distributions completely
characterise the material particulate heterogeneity with respect to a particular
measurand.

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It is convenient to define a quantity, Ks , which may be called the sampling constant
for a material, taking:

⎧a ⎫ K
Var ⎨ S ⎬ = s
⎩ aL ⎭IH M S
2
Ns Nc
⎛ aij − aL ⎞
Ks = ∑ X iVi ∑Yij ρij ⎜
where [Eqn 4.17]

i =1 j =1 ⎝ aL ⎠
The relative variance due to intrinsic heterogeneity is also called the ‘fundamental
sampling error’ (or variance) by Gy (1979).

The sampling constant captures all the necessary information about the intrinsic
heterogeneity of the material to be sampled. Since the variance is a relative variance,
it is dimensionless and the sampling constant has units of mass. If the particle
volume is calculated in cm3, and the particle density has units of g cm-3, the sampling
constant will have units of g. To determine the sample mass that must be retained to
ensure that the relative standard deviation (RSD) between nominally identical
samples does not exceed a fraction r, then:

Ks
Ms = [Eqn 4.18]
r2
If r = 0.02 (2% relative), then:

Ks
Ms = = 2500 K s
0.0004
The sampling constant ‘sets the scale’ of sampling for a material. It is a quantitative
measure of the material intrinsic heterogeneity with respect to a particular measurand.
It is for that reason that the relative variance is given the subscript IH.

It should be noted that a material can be very heterogeneous (large sampling


constant) with respect to one measurand and nearly homogeneous with respect to
some other measurand. For example, a low-grade gold ore of the appropriate
mineralogy will have a low sampling constant with respect to silica and a relatively
large sampling constant with respect to gold.

4.3.1.1 Practical use of the sampling constant


Knowledge of the sampling constant for a material permits the calculation of
the expected variance between nominally identical sub-samples of a given
mass. This means that if some mass of material is put through a rotary
sample divider and nominally identical sub-samples of mass M s are formed,
the variance in the true analyses of the sub-samples with respect to a
measurand cannot be less than the value calculated from the sampling
constant. In practice, if the sub-samples were all prepared for analysis with
great care, the variance between the analyses from each sub-sample would
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be larger than the value calculated from the sampling constant, because the
analytical results would also involve a component of variance due to the
uncertainties in the analytical procedure.

Knowledge of the sampling constant is also critical to the design of sampling


systems. For example, if a sampling system is considered in which primary
increments are taken from a process stream over the duration of a shift, each
primary increment is then sub-sampled within the sampling system
immediately after it is taken, the increments taken by the secondary sampler
are collected and at the end of the shift they will have a mass Ms .

In the case in which there is no distributional heterogeneity in the process


stream (the concentration of the measurand does not change during the
shift), the relative variance between the true value of the average measurand
concentration in the process stream over the shift and the true measurand
concentration in the sample cannot be less than K s M s . In real terms, the
variance will be greater because there will be some distributional
heterogeneity. The variance component due to distributional heterogeneity
can be denoted as var [ a s a L ]DH and the total relative variance between the
true value of the average measurand concentration in the process stream
over the shift and the true measurand concentration in the sample will be the
sum:

⎧a ⎫ ⎧a ⎫ ⎧a ⎫
var ⎨ s ⎬ = var ⎨ s ⎬ + var ⎨ s ⎬
⎩ a L ⎭ total ⎩ a L ⎭ DH ⎩ a L ⎭ IH [Eqn 4.19]

4.3.1.2 Variance increase due to mass division of a sample

The shift sample of mass Ms is then taken to a laboratory and reduced in


mass by careful rotary division, after drying, retaining a mass M s1 . This step
of mass division introduces an additional component of uncertainty between
the process stream measurand concentration and the true analysis of the
sub-sample of mass M s1 . The increase in the relative variance is given by:

⎧a ⎫ ⎡ 1 1 ⎤
∆ var ⎨ s ⎬ = K s ⎢ − ⎥
⎩ a L ⎭ IH ⎣ M s1 M s ⎦ [Eqn 4.20]
This means that the new variance is:

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⎧a ⎫ K ⎡ 1 1⎤
var ⎨ s ⎬ = s + Ks ⎢ − ⎥
⎩aL ⎭IH1 Ms ⎣ Ms1 Ms ⎦
K
= s
Ms1 [Eqn 4.21]
If the sample mass division is not carried out by rotary division, the variance
between the process stream measurand concentration and the true analysis
of the sub-sample will be larger. The sample may have been segregated
before the mass division, and, as a result, the smaller sub-sample may end
up being biased. Essentially, the sample, due to segregation, may have
acquired some distributional heterogeneity (DH), and the sub-sample after the
division will carry an additional component of variance due to this DH. If the
rotary division involves taking 50 to 100 increments (50 to 100 revolutions of
the divider) during the division process, the variance due to DH will have been
reduced to a negligible magnitude.

4.3.1.3 Change in the sampling constant with material top size

If the sub-sample is now crushed or pulverised to a new top size D 2 from its
original top size D1 , the sampling constant for the material will be reduced. In
order to understand how the value will change, the expression for the
sampling constant must be examined in more detail. The intrinsic
heterogeneity term is separated out thus:

2
Nc
⎛ aij − aL ⎞
IH i = ∑ Yij ρ ij ⎜ ⎟
j =1 ⎝ aL ⎠ [Eqn 4.22]
This term is equivalent to a variance of the composition distribution over the
composition classes. In fact, if the density of the particles does not change
significantly from one composition class to the next (the phase carrying the
measurand does not differ in density from the remainder of the particle or is
present in low concentration) and the mass of material in each composition
class is constant, then:

Yρ Nc

∑ ( aij − aL )
2
IH i = i 2 i [Eqn 4.23]
aL j =1

and IHi the intrinsic heterogeneity of the I th


size fraction is directly
proportional to the variance of the composition distribution.

In general terms, when an ore or similar material is further comminuted, there


is a tendency for mineral phases to liberate and the concentration distribution
becomes wider. In extreme cases, when all particles in a size fraction consist

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of one or another pure mineral phase, the heterogeneity of the size fraction
cannot increase further.

The sampling constant is now written as:

NS
Ks = ∑ X iVi IHi
i =1 [Eqn 4.24]
It should be noted that the intrinsic heterogeneity (IH) of each size fraction is
multiplied by the volume of the particles in the size fraction. For many
materials, this means that the value of the sampling constant is controlled by
the IH of the coarsest particles in the material; while the fines may show a
substantially wider composition distribution, their influence on the value of the
sampling constant is suppressed by the particle volume factor.

If the shape of the size distribution remains more or less similar as the
material is comminuted (the cumulative size distribution is simply shifted
sideways on a log size plot), the sampling constant will in most cases (there
are important exceptions) be proportional to the cube of the top size of the
material. Reducing the top size by a factor of 2 reduces the value of the
sampling constant by a factor of 8, if the phases carrying the measurand are
not significantly liberated by the comminution. If the liberation does increase
with reduction in top size, then the sampling constant is reduced by a factor
less than 8.

When dealing with complex materials, where the measurand(s) are carried in
a number of mineralogical phases, it is very difficult to predict the real extent
of reduction in the sampling constant with reduction in top size. This is
especially true when the starting material is coarse and there is little liberation
of the phases carrying the measurand. If the material is crushed past some
critical size, which will depend on the nature of the material, the intrinsic
heterogeneity of the coarser size fractions may show a substantial increase,
possibly by as much as an order of magnitude. In such a case, the sampling
constant reduction with size would be seriously reduced.

There is potentially, therefore, a substantial risk associated with making


assumptions and extrapolations of the value of the sampling constant over
the particle size scale as proposed by the use of the Sampling Safety Line
(Gy 1979).

4.3.1.4 The value of the sampling constant for the analytical


aliquot
When materials are pulverised prior to weighing out an analytical aliquot, the
material is usually visibly very fine. This often leads to the assumption that
the material is so fine that the intrinsic heterogeneity variance component
associated with the mass reduction from the analytical sample of mass M as
to the analytical aliquot mass M aa is negligible. In many cases, this
assumption is untrue. Low-grade materials in particular can be shown to

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have significant intrinsic heterogeneity components associated with this step.
If the material cannot be successfully further reduced in particle size to
reduce the effect, it is necessary to fuse the material to destroy its
heterogeneity, to pulverise it again and then to extract the aliquot. If fusion is
not an option, and the variance of the analysis is to be reduced, the aliquot
mass must be increased.

Analysis of materials by XRF using pressed pellets must be approached with


particular care when low atomic number elements are the measurand. While
the mass of the aliquot used to make the pellet may be substantial, the
analysis depth of the x-rays from the element in the pellet material can be
very low (10s of microns: a Cr x-ray in chromite loses 90% of its intensity over
60 microns). The effective aliquot mass is then controlled by the analysis
spot size and the x-ray analysis depth. The effective aliquot mass may be
reduced by a factor of 1000, increasing the intrinsic heterogeneity standard
deviation due to aliquot mass by a factor of about 30.

4.3.1.5 Determination of the value of the sampling constant for a


material
Use of the basic formula:

2
Ns
⎛ aij − aL ⎞
Nc
Ks = ∑ X iVi ∑Yij ρij ⎜ ⎟ [Eqn 4.17]
i =1 j =1 ⎝ a L ⎠
for the calculation of the sampling constant presupposes that the composition
distribution with respect to the measurand for all the size fractions that have
an impact on the sampling constant value can be determined. In many cases
carrying out such an analysis is simply not a realistic goal; some other means
must be found for estimation of the value of Ks .

There are three basic methods that can be used:

• Individual particle analysis, also known as the ‘50 (or more) piece
analysis’ method
• Use of scanning electron microscope data from particle sections
• Multiple sample analysis
These methods all have their limitations, which are discussed below.

Individual particle analysis

If a material has a top size that makes it feasible to analyse individual


particles for a range of measurands, the measurand(s) is present in
reasonable concentration, and the material shows significant liberation of the
phases carrying the measurand(s), this method can be very effective.

A specially collected composite sample that is deemed to be similar in


heterogeneity to the average material to be sampled is first divided to provide
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a sample for size by size analysis; this sample is screened on at least a √2-
series of sieves and each size fraction is prepared for analysis with respect to
the measurands of interest. From a suitable sample or sub-sample of the
remainder of the material, the two top size fractions are screened out.

These sieve fractions should be chosen so that they each carry about 10% by
mass of the size distribution and the actual mass fractions that they represent
should be calculated and recorded. These fractions do not have to coincide
with the fractions defined in the first sample, but it is convenient if they do.
Then, each fragment is numbered and 50 fragments from each size fraction
are randomly selected (by choosing the 100 numbers at random).

Each fragment must be carefully prepared and analysed to produce 100


results for each measurand of interest and the standard deviation associated
with the analytical methods must be known. For the coarsest material, a
histogram of the results for each measurand is then plotted.

To apply the 50-piece method to the estimation of the sampling constant for a
chosen measurand, the histogram should show a spread (standard deviation)
that is significantly larger than the standard deviation associated with the
analysis. Furthermore, the spread of the analyses of the full set of size
fractions should not be substantially larger than the spread for the particles in
the top size fraction. If there is evidence in the finer fractions of unusual
liberation of phases carrying the measurand(s), one must proceed with more
caution (this issue is illustrated below).

The sampling constant can be written as:

2
Ns Nc
⎛ a ij − a L ⎞
K s = ∑ X i ∑ Y ij V i ρ ij ⎜⎜ ⎟⎟
i =1 j =1 ⎝ aL ⎠
2
Ns Nc
⎛ a ij − a L ⎞
ie , K s = ∑ X i ∑ Y ij m ij ⎜⎜ ⎟⎟
i =1 j =1 ⎝ aL ⎠
2
2 50
⎛ a ij − a L ⎞
∴ K s = ∑ X i ∑ Y ij m ij ⎜⎜ ⎟⎟
i =1 j =1 ⎝ aL ⎠
[Eqn 4.25]
Assuming that the 50 particles in each of the two top size fractions are a
sufficiently good representation of the material, the mass fraction of the jth
particle in the size fraction is:

mij
Yij = 50

∑m
j =1
ij
[Eqn 4.26]
so
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2
⎛ aij − aL ⎞
50

2 ∑ m ⎜⎜ 2
ij
⎟⎟
Ks = ∑ X i
j =1 ⎝ L ⎠a
50 [Eqn 4.27]
i =1
∑mik k =1

The values of X1 and X2 are now the mass fractions determined by


screening out the fractions from the sample (the aim is to have about 10% in
each size fraction).

Note that the analysis aL in the above formula is the average measurand
concentration determined from the size-by-size analysis of all the size
fractions and the a ij are the analyses of the individual particles.

The use of this formula is illustrated in Appendix F.

An example of a material where this method must be applied with caution is


provided by the UG2 ore of South Africa. Figure 4.2 below shows the grade
of the particles in a run of mine sample crushed to a nominal top size of 3
mm, on a size-by-size basis. The UG2 ore is a chromite cumulative texture in
which the sulphides and PGMs are found in the interstices of the texture
dominated by euhedral chromite grains.

The larger material has a grade that is essentially equal to the head grade of
the ore. Chromite grains dominate the size fractions near 350 microns and
these fractions are relatively low in PGMs (the PGM grade goes down to 0.5
g/t). The heterogeneity with respect to PGMs of the fractions above 350
microns is low, but for sizes below 100 microns, the heterogeneity increases
radically. Given the particle volume weighting, the overall heterogeneity of
the ore with respect to PGMs will have contributions from all but the finest
fractions. The heterogeneity with respect to chromite will be dominated by
the larger particles because their grade differs significantly from the head
grade. This ore provides an example of a material that must be carefully
analysed to discover its full heterogeneity with respect to all measurands of
interest.

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30 60

25 50

20 40

Cr 2O 3 [%]
Pt [g/t]

15 30
Cr 2 O 3 head
grade
10 20

5 10
Pt head
grade
0 0
1 10 100 1000 10000 100000

Particle Size (microns)

Figure 4.2: The grade of particles in a run of mine sample of UG2 ore crushed to a nominal
top size of 3 mm, on a size-by-size basis

Use of scanning electron microscope data

When the particles in the material are too small for individual analysis, it is
possible to take advantage of the automated electron microscope
instruments, QEM*SEM and the Mineral Liberation Analyser (MLA) that have
been purpose built to analyse sectioned particle mounts rapidly and
effectively. These instruments are specialised to scan sectioned and polished
mounts of particles of an ore; they have the facility to identify mineral phases
and to analyse by XRF the phases with respect to a given element. They
also have the facility to search the mounts for mineral grains of rare phases
such as gold, electrum and PGMs.

If a chosen size fraction of particles is mounted in resin, cut, polished and


prepared for an electron microscope, the instrument will provide a set of
analyses of hundreds or thousands of individual particle sections. The
instrument will provide the area fraction of each mineral for each particle
section. The areal fraction of the particle section does not unequivocally
provide the volume fraction of the mineral in the particle. The difference
between the two is called stereological error.

In some cases stereological error is negligible and in other cases it can be


significant. Procedures for correcting this error are available but seldom
applied in practice. Such procedures are called stereological correction. This
means that if, instead of using stereological correction, the distribution of the
areal fractions is used as a surrogate for the volume fractions of the target
mineral phase, the standard deviation of the distribution is always over-
estimated. However, the mean of the distribution is unbiased, which means
that assays estimated from area sections give an unbiased estimate of the
assays of the particles.

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If the two top size fractions of, for example, a flotation concentrate are
mounted and analysed, the sampling constant for the material can be
estimated, under the same caveats as for the ‘50 piece analysis, from this
electron microscope analysis. It is important to know the average measurand
concentration, aL for the sample, and it is necessary to convert from volume
to mass fraction units of concentration. Thus, the calculations for the method
are rather more involved than the procedure for large particles. However, this
method permits the analysis of particles down to some 10s of microns in size
and so can reveal heterogeneity problems with the analytical aliquot.

Multiple sample analysis

When the above methods cannot be used, it is necessary to resort to the


multiple sample analysis method. This method is very simple, but it is
necessary to be aware of the impact of analytical precision of the values used
in the calculations relating to the method. This method can be used to track
the material heterogeneity as a function of the material top size.

The concept of the method is directly related to the form of Equation 4.17,
which indicates that the variance of measurand concentration between
nominally identical sub-samples of mass M s is inversely proportional to the
sample mass.

To establish the sampling constant at a given top size of the material of


interest, a set (six or more) of nominally identical samples of a series of
nominal sample masses is prepared by rotary sample division. The samples
masses are denoted as Ms1 , M s 2 , …, Msn. Each of the six or more samples
of a given nominal mass is analysed for the measurands of interest and the
variance of each of the measurand concentrations over the set is calculated
in the usual manner. The process is repeated for the progressively smaller
nominal masses, Ms1 , Ms2 , …, Msn to provide variance estimates ŝ12 , ŝ22 , …,
sˆn2 . Then a plot of the variance versus the reciprocal of the sample mass is
made and a regression line fitted to the points that follow a linear trend. The
slope of the line is the value of the sampling constant at the particular top
size.

This method must, however, be used with common sense. When the sample
mass is large, the measurand variance over the nominally identical samples
will indicate nothing but the analytical variance. The variance over the
samples will not increase until the mass is low enough to expose the material
heterogeneity. The heterogeneity with respect to different measurands may
well appear on different scales.

4.4 ACCURACY OF THE SAMPLING SYSTEM


A sampling system that is mechanically correct cannot be biased in the long run.
The most effective manner of ensuring that sampling systems are free of bias is to
design them to be mechanically correct under all circumstances (material types and

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range of mass flow). If a sampling system cannot be designed, installed, operated
and maintained in a manner that is unequivocally mechanically correct, provision
must be made to allow accurate bias testing. If the nature of the flow being sampled
changes, a sampler that is not mechanically correct must be bias tested on the new
material type.

A correct sampling system can show a bias over a short period of time if the sampler
takes increments at fixed time intervals, and this interval is a multiple of the period of
a periodic variation in the mass flow or quality of the process stream. To eliminate
this effect, the sampler must be operated in a random stratified sampling mode,
preferably based on time intervals.

Stopped belt sampling using a correctly designed former, which is the recognised
reference sampling method for conveyer systems, can obviously be used. But there
is usually a significant cost associated with a stopped belt exercise and this
procedure is usually reserved for establishing the accuracy of alternative sampling
methods.

The sampling from stockpiles and bins for purposes of Metal Accounting must be
avoided because it is almost impossible to obtain a representative sample. The
recommended method is to evaluate the material as it is added to or removed from
the stockpile or bin.

The sampling of trucks, wagons, skips and drums must only be undertaken using
correctly designed auger samplers and in accordance with a Standard such as JIS M
8100.

Solutions, but not slurries, in pipes must be sampled after passing through an
efficient in-line mixer, and in drums they must be thoroughly stirred before sampling.
If there are suspended solids in the drums, the contents must be filtered and the
solution and solids sampled and analysed separately by accepted procedures.

Final metals must be sampled according to the appropriate standard in order to


obtain an unbiased sample with respect to the trace elements.

Effluents and discharges through stacks normally only have a minor effect on Metal
Accounting, although this is not the case if accountability of sulphur in a smelter, for
example, is important. Accurate stack sampling requires specialised equipment and
expertise and for this reason, it is often outsourced. Effluents can be accurately
sampled using cross-stream or flexible hose samplers.

The requirements for an accurate cross-stream sampler are given in a number of


texts and they include the following list given by Holmes (2004):

• The sample cutter must be non-restrictive and self-cleaning


• The geometry of the cutter opening must be such that the cutting time at each
point in the stream is equal. For linear-path cutters, the cutter edges (called
lips) must be parallel and for cutters travelling in an arc or a circle, they must
be radial. Flap or diverter type cutters are always incorrect in this regard,
because they divert one side of the stream for a longer period than the other
(Pitard)
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• No materials other than the sample must be introduced into the cutter e.g.
dust or slurry must be prevented from accumulating in the cutter when it is in
the parked position
• The cutter must intersect the stream in a plane normal to, or along an arc
normal to, the mean trajectory of the stream
• The cutter must travel through the stream at a uniform speed – an adequately
powered electric drive is a pre-requisite for this
• The cutter aperture (gap) must be not less than three times the nominal top
size of the material, with a minimum size of 10 mm. For wet solids a
minimum of 50 mm is recommended to avoid bridging
• The cutter must have sufficient capacity to accommodate the increment
mass at the maximum flow rate of the stream. Bucket samplers, in particular,
must have sufficient capacity to accommodate the increment mass at
maximum flow rate of the stream without any reflux or overflow of material
from the cutter aperture
• For slurries, loss of sample material due to dribbles must be avoided
• The maximum cutter speed must not exceed 0.6 m.s-1
• Cutters that collect only part of the stream on a continuous or periodic basis
e.g. “shark fin” cutters, pressure pipe samplers, T-pieces or “bleeds” from the
side of a pipe must be avoided
• For sticky materials, steep chute angles of >60o and stainless steel or
polythene chute linings are recommended to reduce adhesion, and the cutter
gap may also need to be enlarged to prevent bridging
• The plane of the cutter lips must not be vertical or near vertical, because
particles that strike the inside edge of the cutter lips are deflected away from
the cutter by gravity
• If a belt scraper is required to remove material adhering to the belt, the
scraped material must fall within the area traversed by the cutter
Another very useful source of information on factors to be considered in the design of
accurate samplers is the paper by Pitard presented at the Second World Conference
on Sampling and Blending, held in Brisbane in May 2005.

4.4.1 Reference Sampling Method


The accepted Reference Sampling Method for material on conveyors is the so-called
Stopped Belt sampling method. Here the material of interest is moved on a
conveyor belt, which is stopped periodically. A former that is as wide as the belt, with
a separation of the plates of not less than three times the nominal top size of the
material with a minimum size of 30 mm, is placed on the belt and all of the material
between the plates is removed. In the situation where the position of the former is
fixed, it is the convention that any material caught under the plate on the upside of
the conveyor is included in the sample and that on the downside rejected. An effort
should be made to ensure that the mechanical sampler being tested takes its
increment from material as close to that taken by the stopped belt former as possible.
The absence of bias from the mechanical sampler is established by conducting the

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experiments specified in a number of Standards such as ISO 13292:1997, ISO
3085:1998, AS4433 and JISM8100. The data analysis method must consider both
bias of scale and absolute bias.

4.4.2 Slurry Sampling


Obviously, the stopped belt sampling method cannot be used as a reference method
for slurry being conveyed in a pipe or launder. In this case it has been stated by Gy
(1979) that, provided the cross-stream sampler has been installed to satisfy all of the
points given in Section 4.4, the sample may be considered to be accurate. It would
also be prudent to add the points given by Bartlett (2001) concerning the design of
the launder, the slurry velocity, a cutter gap of 20 mm, a cutter speed of 0.3 m.s-1 and
the streamlined design of the cutter body. As pointed out by Hunt (2002), however,
the fact that a sampler obeys all of the rules for a correct design does not
automatically produce an unbiased sample. Great emphasis must be placed on the
ongoing correct operation of the sampler, sample presentation and the auditing of the
system.

4.4.3 Stock-pile or Bin Sampling


Unless the material in a stockpile or bin is completely homogeneous, it is impossible
to sample accurately and, therefore, attempts to include such samples in a metal
accounting process will invariably lead to inaccuracies. The only measurement of a
stockpile or bin that can be performed accurately is that of volume. But the
conversion of this measurement to a dry mass is confounded by the fact that it is
almost impossible to obtain accurate bulk density and moisture values.

It is recommended that the contents of stockpiles and bins only be evaluated by the
accurate sampling of material as it is added to or removed from the stockpile or bin.

If this is impossible and there is no viable alternative to attempting to sample a


stockpile, then the situation must be covered by an Exception Report.

4.4.4 Truck, Wagon, Skip and Drum Sampling


It is possible to establish the accuracy of auger sampling of trucks or wagons if the
material can be transported by a conveyor and subjected to stopped belt sampling
(Section 4.4.1) or re-slurried and sampled by a correctly designed cross-stream
mechanical sampler (Section 4.4.2). For an auger to have a reasonable chance of
being accurate, the particle size of the material being sampled must be reasonably
fine and there must be no free water associated with the material being sampled. In
addition, the auger must penetrate to the bottom of the “container” and all of the
material sampled must be retained within the auger. A spear sampler, i.e. a tube
sampler without an inner Archimedean screw, is not recommended even if it is
mechanically driven. This is because after a certain distance, the frictional force due
to the material going up the inside of the spear becomes greater than the force
required to move aside the material on the outside of the tube. Consequently, only
the upper layer of the material will be sampled.

The precision of an auger sampler can also be established by carrying out a suitable
number (>30) of inter-leaved sampling experiments on the material being sampled.

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A paired t-test can then be applied to the data sets to confirm that there is no
significant difference between the pairs of results.

4.4.5 Solution Sampling


The accuracy of solution sampling can be established by experiments that compare
the concentration of analytes in the sample with the concentrations in the reject
solution.

This is usually achieved by conducting experiments where a solution is pumped past


the same sampling point at least 10 times and the analytical data from the
successive samples is examined statistically to ensure that it is free from drift.

Because solutions pumped through pipes can be thoroughly mixed using in-line
mixers, the normal requirement, of repeated sampling of all of the stream part of the
time, can be relaxed and a portion of the stream can be removed under controlled
conditions. There are a number of commercially available sampling systems that can
do this. However, there are examples, for instance in a precious metals refinery,
where the density of a process liquor can be so high that segregation of the liquor
occurs. In these cases it is impossible to take a dip sample and the rule of sampling
a process stream while it is in motion must be applied.

There are areas in Hydrometallurgical Plants where solutions must be sampled when
they are hot and/or under high pressure. In these circumstances, specialised
equipment is usually necessary and care should be taken to ensure the safety of the
plant operators. In addition, care must be taken to avoid the evaporation of water.
The effect of crystallisation when the solution cools to ambient temperature must also
be taken into account.

4.4.6 Final Metals and alloys


Because of the normally high purity of final metals, >99%, they are essentially
homogeneous with respect to the major constituent and, therefore, the sampling of
them to account for the major metal is not problematic. It is usual to establish the
concentration of the major metal by summing the concentrations of the impurities and
subtracting this value from 100%. Sampling for the evaluation of trace impurities,
however, should be carried out according to an appropriate standard such as
ASTM1587.

The sampling of ferro- and non-ferrous alloys is well covered in a number of


international standards (Appendix C.2.3).

4.4.7 Scraps and residues


Frequently the sampling of scraps and residues has particular difficulties. This is
because they can consist of a mixture of metallics and plastics, e.g. computer scrap,
or other materials. The design of a sampling protocol for scraps and residues must,
therefore, be done with a high degree of common sense and with due regard to the
requirements for obtaining an accurate sample. For example:

• Computer scrap may be chopped into fine pieces prior to sampling

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• Residues containing metallics and powder could be sieved to separate the
two and each material sampled separately

4.5 PRECISION OF THE SAMPLING SYSTEM


The precision of a sampling and sample preparation system is determined
unequivocally by inter-leaved sampling methods, the procedure for which can be
found in a variety of Standards (e.g. ISO 12743 and ISO 12744:1997). In an inter-
leaved sampling test, the primary sample cutter is operated at twice the usual rate
and the alternate increments are directed to separate containers. If the sampling
system consists of more than one stage, the material from successive primary
increments must remain separate as it moves through the sampling system and is
collected in the separate containers.

The two sample containers are collected at the end of the sampling period and they
are processed separately to arrive at a set of analytical results. By collecting a
substantial number of samples in this way, the average absolute difference between
the sample pairs, or the mean squared difference between the sample pairs, can be
used to estimate the total variance of sampling, plus sample preparation, plus
analysis. If it is an objective to break this variance down into its components,
additional work must be undertaken to establish the analytical variance (which should
be known from records of duplicate determinations in the laboratories) and the
sample preparation variance. The Standards are very clear as to how to undertake
inter-leaved sampling work.

However, if inter-leaved sampling is to be used periodically to establish the sampling


variance, especially when changes in the process have been implemented, the
system must be designed to allow sampling in this mode.

The variance of sampling, with respect to a target analyte, is generally composed of


two basic components when sampling a particulate material. The first, usually
referred to as the 'fundamental error', is related to the range of analyte contents of
the particle. It is possible to calculate a 'sampling constant', K s for a material in a
given state of comminution and with respect to a particular measurand, (Section 4.3).

If the mass retained at the end of a sampling period (e.g. a shift) is Ms , the sampling
variance due to the fundamental error is:

Ks
σ 2 = a2 [Eqn 4.28]
Ms
where a is the assay of the sample. Note that K s is usually calculated in units of
grams.

The second component of the sampling variance is due to the time variation of the
grade of the process stream during the sampling period. This component of variance
is proportional to the variance of the measurand concentration about the mean for
the sampling period and it is inversely proportional to an increasing function of the
number of increments taken from the process stream during the sampling period.

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In a multi-stage sampling system, it is vital that an adequate number of increments is
extracted from each primary increment, and from all the successive stages of the
system. This is particularly important in multi-stage slurry sampling systems. The
number of increments required depends entirely on the tendency of the material to
segregate with respect to measurand concentration or particle size, as it is handled
within the sampling system. Ideally, 30 increments should be taken at each stage,
but in practice, this is often difficult to achieve. However, especially in multi-stage
slurry sampling, the extraction of numerous increments is important to reduce the
possibility of bias in the sampling. It is in such a circumstance that Hunt's comment
that a sampling system consisting entirely of correct samplers may still end up
showing a bias is likely to occur. The bias incurred under these circumstances is
always a consequence of allowing the material to be sampled to segregate. Thus,
correct presentation of the material to be sampled to the sampler will essentially
eliminate the bias.

In a multi-stage sampling system, there is an increase in the sampling variance at


each successive stage of sampling. If the sample is reduced in mass from Ms to
Mss , the increase in variance is given by the following equation:

⎡ 1 1 ⎤
∆σ 2 = a2 K s ⎢ - ⎥ [Eqn 4.29]
⎣ Mss Ms ⎦
where Ks is the sampling constant for the material at its particular state of
comminution and a is the sample assay.

If the sample is reduced in particle size by crushing or pulverising, the sampling


constant will change in value. The change is determined by two competing factors.
Firstly, the sampling constant is broadly proportional to the volume of a particle
having a size equal to the 95% passing size, with the exceptions outlined in 4.3.
Secondly, the sampling constant increases with the extent of the liberation of the
phases carrying the measurand of interest. It must be emphasised that this latter
variation is entirely dependent on the nature of the phases carrying the measurand of
interest. A material can have a small sampling constant with respect to one
measurand and a very large component with respect to a second measurand. For
materials in which the phase carrying the measurand of interest is very high grade
and the overall grade of the sample is low, the sampling constant may not behave
according to the broad rules stated above. A coarse-grained low-grade gold ore may
have an essentially constant sampling constant that does not depend on the particle
size at all. A PGM material where most of the grade is due to 'metallics' will have a
similarly perverse behaviour in terms of its sampling constant. It is therefore
extremely risky to make broad statements regarding the nature of the fundamental
error for an ore, with respect to any measurand.

The sampling safety line plot, originally proposed by Gy, is based on the assumption
that the sampling constant is proportional to particle top size cubed. If this is not true,
the sampling safety line is, therefore, correspondingly misleading.

Every stage of sample preparation in which the ore is reduced in size, and
subsequently reduced in mass, causes a change in the sampling constant, and it

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incurs an increase in the total sampling and preparation variance according to the
formula above. This increase in variance continues right down to the point of
extracting the analytical aliquot from the prepared sample.

From the point of view of the variance of sampling, preparation and analysis, the
preparation stages must be treated in exactly the same way as the sampling stages.

When the material being sampled changes in its mineralogical make-up, or the
intensity of the process grade variations with respect to any measurand of interest
changes, the precision of sampling may need to be re-estimated. New tests of the
sampling precision, using inter-leaved sampling, may be the most effective way of
determining the change in precision. Given that the sampling systems have been
designed to permit inter-leaved sampling, which is highly recommended for metal
accounting samples, this is a simple procedure which can be carried out periodically
and documented on an on-going basis. Such a procedure is a sound component of a
quality assurance program.

It is recommended that the precision of samplers be measured on a regular basis, at


least annually. This allows the contribution of the samplers to the total variance to
be calculated, thereby indicating where effort should be focused in the valuation
system.

4.6 MULTI-STAGE SAMPLING SYSTEMS


It is quite probable, due to the constraints on the requirements of the sampling device
e.g. cutter gap, cutter speed and number of increments, that the mass of sample,
especially if taken at primary or secondary sampling stages, will be too large to
submit to a laboratory for analysis. This is most likely to be true for coarser materials
and/or process streams with a large tonnage throughput. In these cases, it is usual
to design a sampling system with multiple stages. It is important that any reduction
of sample mass is done with the objective of minimising additional sampling variance.

Three methods can be used to establish the Sampling Constant and hence the
sampling protocol to achieve a desired level of sampling variance and they are
discussed in Section 4.1.

In addition, to enable the recommended number of increments (>30) to be taken at


each sampling stage, intermediate storage bins with controlled feed to the next
sampling/reduction stage are normally required. Secondary and any subsequent
samplers must be running continuously or be triggered at a random time ahead of
any material to be sampled.

The bias of a sampling system can be determined only by comparison of the samples
from the installed sampling system with some reference method of sampling
(stopped belt for material flows on conveyors and some other method for other
situations).

Bias is not a statistical quantity and is, therefore, much more difficult to quantify than
sampling precision. A test to estimate bias must be designed to detect a certain level
of bias. As the magnitude of the bias to be detected becomes smaller, in relation to
the sampling precision (or standard deviation), the number of pairs of 'test' and

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'reference' samples needed to show up the bias in a statistically significant manner
becomes steadily larger. To find a bias that is one quarter of the standard deviation
is very difficult. Standards deal very effectively with the estimation of bias and the
general rules for doing the tests are all similar. The statistical analysis of the test for
bias must include a test for bias of scale as well as for absolute bias. The method by
which this can be done is documented in an article by Lyman (1993).

The best defence against bias in sampling systems is the mechanically correct
sampling of the process stream and the extraction of adequate numbers of
increments at each stage of sampling.

The extraction of the analytical aliquot from the mass of prepared sample must not
be ignored. This is almost universally done by use of a spatula, which is not a
mechanically correct method of sampling and it is prone to bias. Where the material
for analysis has refractory and easily ground phases and density differences between
mineralogical phases, there is a perfect opportunity for phase segregation at the very
point where the phases are best liberated. To reduce bias and variance to their
minima, miniature rotary sample dividers should be used to extract the analytical
aliquot from a mass of sample that has been prepared to a target mass without any
manual 'dipping' of sample increments. To accomplish this task, a 'variable split'
rotary sample divider is recommended.

In the Coal Industry, for example, the particle size of a plant product can be an
important measurement parameter. Particle size reduction, therefore, cannot be
carried out during a multi-stage sampling system on the portion of the sample to be
used for particle size measurement. Systems have been designed, however, where
a separate portion is taken specifically for particle size analysis.

4.7 SAMPLE STORAGE PRIOR TO DELIVERY TO A LABORATORY


Prior to their delivery to a laboratory for analysis, it is important that samples are
stored in suitable sealed containers in areas where any change to their physical or
chemical parameters is minimised. This is especially important with respect to their
moisture content.

4.8 SAMPLE LABELLING


All samples must be labelled in such a way that their unique identity is unambiguous.
There are several computer-based sample-numbering protocols available to ensure
this unique identity. The use of a bar coding system is preferable; however, to
maintain readability, small bar coding systems should be avoided

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5 SAMPLE PREPARATION AND ANALYSIS

5.1 INTRODUCTION
All operations in sample preparation and analysis must be carried out in order to
provide accurate data with a known and acceptable precision within a time frame
that is suitable for Metal Accounting purposes.

Cross-contamination of samples during sample preparation must always be guarded


against. Samples with known differences in concentration such as feeds, tails,
concentrates, mattes and slags must be prepared in separately enclosed areas using
dedicated equipment. In cases such as underground and geological samples, where
large variations of grade are unavoidable and unknown, it must be established that
there is minimal hold-up of material within the sample reduction equipment. Frequent
cleaning of this equipment may be necessary.

5.2 SAMPLE PREPARATION

5.2.1 Moisture Determination


The moisture determination must be carried out as soon as possible after the sample
has been taken and the sample must have been stored in a sealed, air-tight, non-
corroding container. The whole sample received in the Laboratory must be dried to
constant mass for the moisture determination. When removing the sample from the
canister in which it arrives at the laboratory, specific attention should be given to
removing moisture in the container that has 'sweated' out of the sample. A tared
piece of paper towel can be used for this task. This issue is clearly more important
for samples of relatively small mass.

In some operations where a large sample is delivered to the laboratory (>10 kg) this
must be sub-sampled through a correctly designed sample division system, in an
enclosed space (particularly in conditions of low ambient humidity), to provide
material for further treatment within the laboratory.

The drying temperature, which must not exceed 105°C, must be such that the
physical and chemical properties of the sample are unaffected. In the Coal Industry,
for example, it is usual practice to air-dry samples at ambient temperatures.

5.2.2 Sample Reduction


Sample reduction must only be carried out in equipment that does not contaminate
the sample. Because “zero contamination” is probably not achievable, experiments
must be conducted to establish the level of any contamination by running suitable
blank samples through the system at periodic intervals. In the cases of known
potential contaminants, such as cobalt from a tungsten carbide mill and chromium
from a ferrochrome mill, alternative systems should be chosen if the contaminant is a
required measurand.

Dust losses must be avoided because there have been numerous occasions where it
has been demonstrated that the fine material in a sample has a very different

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concentration range than the bulk material, for certain measurands. Examples of this
are ROM samples in the Gold Mining industry where, due to density differences,
fines likely to be lost as dust essentially have a zero gold content, and in Platinum
smelters, fines in converter matte samples have very low PGM concentrations. In
both cases, the loss of fines during the sample preparation process will, therefore,
significantly upgrade the sample.

Suitably sized jaw and roll crushers, pulverisers and “puck and ring” mills are
acceptable for sample particle size reduction.

Sample reduction ahead of sample division must always be done to a particle size
that is known to maintain the sample preparation variance at the desired level for the
sample concerned, as determined by an appropriate test and analysis of sample
variance.

5.2.3 Sample Mixing


Provided that Sample Division is carried out using correctly designed mechanical
spinning riffle systems, samples do not require further mixing after a reduction stage.
If the sample is to be mixed, sealed mechanical systems such as Y-blenders or
other suitable mixers are preferred as they prevent dust losses during mixing. Care
must be taken to ensure that the mixing containers are not filled to more than 50% of
their volumetric capacity.

Paper or sheet rolling, which is sometimes used in sample preparation facilities, must
be avoided, because of the potential for dust loss, increased segregation and
inadvertent sample loss if the mixing is carried out too vigorously.

The mixing tray procedure specified in JIS M 8100 and by Merks (1985) is
acceptable, where sealed mechanical systems are not available. Because this is a
manual system, there is an upper limit to the sample mass that can be handled in
practice.

5.2.4 Sample Division


The degree of sample division must always be done with the aim of achieving a
desired level of sample preparation variance.

Properly designed mechanical sample division systems, such as rotary rifflers, are
preferred provided that the requirements of good sampling practice such as speed of
rotation < 0,6ms-1, radial cutter gaps and a minimum of 30 increments are observed.
In addition these systems should provide completely proportional samples and QC
procedures must be in place to confirm this.

The Incremental Division Procedure specified in JIS M 8100 and Merks (1985) is
acceptable.

Stationary rifflers must be avoided, because, even when the riffler is equipped with a
feed bin to ensure the even distribution of material to both sides of the divider, the
probability of unsatisfactory operation is too high.

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5.2.5 Sample Storage after Sample Preparation
Samples, including acid liquids, must be stored in sealed glass containers, after
sample preparation, to minimise any possible physical or chemical changes. Alkaline
liquid samples must be stored in sealed plastic containers. If samples are to be
stored for long periods, i.e. for longer than 3 months, they must be stored under
nitrogen. For periods longer than 6 months, consideration should be given to storage
in hermetically sealed plastic containers under nitrogen.

After prolonged storage, solid samples must be mixed in a sealed system prior to
extracting an analytical portion.

There must be an appropriate administration system in place to monitor the removal


of samples from storage for the purposes of further analysis or disposal.

5.3 ANALYSIS

5.3.1 Laboratory Accreditation


Analytical procedures used to analyse samples for Metal Accounting must be
accredited to the ISO 17025 standard. This has become the de facto worldwide
standard for laboratory accreditation, with local accreditation boards established in
most countries with significant mining/metallurgical operations. Accreditation is seen
as a requirement for material such as concentrates and mattes that are part of a
commercial transaction between a buyer and seller and for other materials that are
part of a metal accounting system.

It is likely that most of the procedures in the following sections will be implemented as
part of an accreditation exercise.

5.3.2 Twin Stream (independent parallel) Analysis


Samples for Metal Accounting should be analysed in a twin stream analysis scheme
in which a set of nominally identical aliquots of the sample are analysed by different
analysts using different instruments at different times. There should be no more than
6, but at least 2 nominally identical samples in each set. A maximum of 6 samples is
recommended for each set because fewer samples are inefficient and it has been
found that if the number becomes too large there is a tendency to avoid strict
application of any QC procedure.

5.3.3 Reference Materials


In addition to the samples, each set of materials analysed should include at least one
Reference Material (RM), which is similar in matrix and concentration to the samples.
Preferably this should be a Certified Reference Material (CRM), if it is an Internal
Working Reference Material (IWRM) then the accepted values should have been
derived by a multi-laboratory round robin exercise using a CRM as a QC sample.
Periodically a Reference Material should be included in routine analysis, preferably
as a blind sample; it is common practise for blind samples to constitute 5–10% of a
laboratory’s throughput.

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5.3.4 Instrumental Calibration (ICP, AA, UV/VIS, XRF [solutions])
At least seven standard solutions, including a blank, should be prepared to cover
evenly the calibration range, which itself must be designed so that the concentrations
of the sample solutions are close to the centre of the range. The standards should
preferably be matrix-matched to the sample solutions which should be measured in a
random order, both before and after the sample solutions. The best practice of
instrumental calibration is covered in the VAM document LGC/VAM/2003/032.

5.3.5 Instrumental Calibrations (XRF [Pressed Powder and Fused


Bead])
At least 15 standards are required to cover the expected concentration range of the
samples and, in the case of the Pressed Powder technique, they should be closely
matrix-matched to the samples to be analysed. This will probably require that the
standards are replaced on at least an annual basis. The analytical values assigned
to the standards must be accurately established using other accredited methods.
This can be done in-house or by using the facilities of another laboratory that has
demonstrated its ongoing ability to analyse the types of sample concerned. The
concentrations of all non-metal accounting elements with a concentration > 2% must
have accurate values assigned to them to allow for the estimation of inter-element
effects. The sum of all known elements in the standards must be > 95%. The best
practice for calibrating an XRF instrument should be followed. Particular attention
should be given to ensuring that all pressed pellet standards have the correct particle
size distribution.

5.3.6 Instrumental Calibrations (Other)


Calibration of other analytical instruments should always be to the best practice
possible. This is in relation to the number of standards required to establish the
response of the instrument, full coverage of the analytical range, matrix matching to
the samples and measurement of the precision of the instrument during the analysis
of a batch of samples.

5.3.7 On-Line Analysers


A specialised area of instrumental analysis is On-Line Analysers, but they are not
often used for Metal Accounting purposes; however, but where they are used, their
calibration should be carried out to satisfy the requirements of Section 5.3.6.

5.3.8 Fire assay


Fire Assay is used extensively in the Gold and PGM mining industries and special
care must be taken to ensure the reproducibility of analytical conditions such as
fusion and cupellation temperatures and times. QC samples must be analysed with
each set of samples with its replicates distributed amongst the sample positions.

Because of the known losses during the lead collection fire assay of the PGMs,
which are reasonably reproducible if the operating conditions are kept constant, a fire
assay correction factor is often used to correct for these losses. These corrected
values must not be used for Primary Metal Accounting, which must be based on a
technique such as nickel sulphide collection, but they may be used for Secondary

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Accounting and Plant Control purposes. The same stipulation applies to gold assays
where a silver correction has been applied.

5.3.9 Mineralogical Analysis


In some operations there is a requirement to analyse samples for their mineral rather
than their elemental content. Preferably this analysis should be carried out using
computer controlled electron microscopes, but if it is done manually by point counting,
then for major (> 50%) phases/minerals at least 600 points must be counted and for
minor (± 5%) phases/minerals, the point count must be increased to 6 000. The
number of points must be sufficient to provide a statistically meaningful result, and
will depend on the variability of the material and the required precision.

5.3.10 QC Procedures
QC procedures must be established, and strictly adhered to, in relation to the
allowable differences between the accepted and actual values of the Reference
Materials and the differences between replicates in the twin stream (independent
parallel) sets. The use of Shewhart and CUSUM control graphs are recommended
for the monitoring and rapid identification of possible analytical problems. Action to
be taken in these situations must be formalised in the QC procedures.

5.3.11 QA Procedures
Regular multi-laboratory interchanges of samples (Round Robin exercises or
Proficiency Testing) must be conducted with laboratories whose ability to conduct
such analysis has been proven by means such as laboratory accreditation to ISO
17025. The exercise should preferably include laboratories that are independent of
the organisation concerned.

The statistical analysis of accumulated analytical results for reference materials and
for duplicate determinations is a very valuable tool for the on-going improvement of
analytical procedures and it is vital to the maintenance of targets for accuracy and
precision within the analytical systems. These analyses also provide an index of the
efficiency of the laboratories; an increase in the fraction of the samples that require
repetition because they have fallen outside the tolerance for agreement between
duplicates not only indicates that the precision of the analysis is decreasing, but it
also increases the load on the laboratory, limiting its throughput of fresh samples.

It is extremely important that all assay results are collected into a database. The
assay duplicates that failed to meet the tolerance must be included in the database.
If they are not included, the database becomes 'censored' and is therefore very
difficult to use in statistical analysis, since distributions of assay results are then
truncated.

5.3.12 Umpire Laboratory


The availability of an Umpire Laboratory is an integral requirement of a laboratory
carrying out analysis for Metal Accounting. The Umpire Laboratory must obviously
be accredited to ISO 17025 for all analytical services that it provides. In areas where
particular analytical skills are needed, such as PGM analysis, the Umpire Laboratory
will be required to have on-going experience of the analysis and this will probably

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result in the Metal Accounting laboratory having to submit samples regularly rather
than on an as-required basis.

The assay censoring issue also arises in the use of umpire laboratories. External
laboratories may be asked to provide a database that indicates their ability to provide
precise results. The results in this database must not be censored, since this would
make it impossible to understand the risks associated with use of that laboratory.

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6 STOCK-TAKES
Physical stock-takes and the determination of the Plant Stocks and total Process
Inventory are an integral part of metal accounting. The calculation of the dry mass
and content of process inventory held in stockpiles, bins, tanks or other process
vessels is subject to a high degree of uncertainty, mainly due to the difficulty in
obtaining a representative bulk density and sample as discussed in Section 3.5. It
can also be difficult to make estimates of the volume of material that complies with
the standard of accuracy needed for metallurgical accounting.The effort put into the
estimation of an item of plant stock should be dictated by the value of the material in
that item, relative to the value of the entire stock, as well as by the accuracy of the
balance being carried out. A great deal of reliance is placed by external financial
auditors on “setting the clock to zero”; i.e. a full stock-take at regular intervals.

The frequency with which stock-takes are carried out is a management decision and
it should relate to the value of the plant throughput and the in-process inventories
relative to the expected profit at year-end and the cost of executing the stock-takes,
but it must be carried out on at least an annual basis. Stock-takes can be performed
more frequently, for plant control, to a lesser degree of accuracy than that required
for financial reporting. The latter stock-takes must be performed in conjunction with
the company’s auditors.

The cost of executing the stock-takes increases with the demand for the accuracy of
the result. The final decision regarding stock-take frequency and accuracy will be
determined by the level of financial risk associated with a particular strategy. The
costs incurred should be offset against the benefit achieved by the more timely
availability of accurate information of production performance and of stock shortages
or excesses. The overall confidence level in the result of the stock-take must be
established from the uncertainties in the component measurements and reported
with the results.

Having developed a stock-take policy, the procedure must be documented to ensure


a clear definition of roles and responsibilities leading to the rapid and effective
execution of the stock-take and the reporting of results. Procedures for handling
differences between book and measured stocks must be fully documented. Any
adjustments must be made only after the appropriate authorisation as defined in the
Code and these Guidelines.

It is readily demonstrated that in-process stocks and draw-down or build-up of stock-


piles are likely to represent the largest uncertainties in a Metal Balance. The most
successful strategy for elimination of these uncertainties is to use a policy of building
parallel stockpiles, one of which can be exhausted at the end of the accounting
period. If stocks are never exhausted, measurement uncertainties will accumulate to
a point where the balances will be essentially meaningless.

Therefore, the policy of eliminating stockpiles on a regular basis must be built into the
general processing strategy.

In cases in which the in-process inventory has a value that is large compared to the
value of the net input for the accounting period, the accounting strategy must involve

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an operating policy which permits the exhaustion of the in-process inventory
immediately prior to the stock-take, such as the use of the Bubble Method.

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7 METAL BALANCING

7.1 INTRODUCTION
The metals/commodities, alloys or concentrates produced by a metallurgical
processing operation are the source of income which both sustains the operation
financially and justifies the initial capital investment.

The income generated is the result of a commercial transaction, which is based on a


mass measurement and one or more analyses, which indicate the mass or proportion
of saleable materials and any penalty elements. As might be expected, products
which do not achieve a target grade and/or contain penalty elements attract a lower
price, as detailed in a contract of sale.

A mineral or metallurgical processing operation, which “purchases” its feedstock, has


similar quality and mass measurement issues relating to a transfer of custody for
both feeds and products.

Those operations which mine their own deposits as feed stock commonly have
royalty obligations relating to the depletion of the resource and, in some cases, may
attract environmental penalties if levels of, for example, acid generating material or
heavy metals in water, exceed agreed limits.

The metal balance is critical for corporate governance, for monitoring, checking and
improving performance and for identifying and quantifying losses and emissions. A
satisfactory metal balance provides a convincing demonstration that:

"What comes into the operation, less any internal accumulation, plus any draw down
from internal stock, is sufficiently similar, i.e. within acceptable limits in mass and
analysed components, to what goes out as product(s) and reject." (Check in-Check
out)

This is the fundamental purpose of the metal balancing and reconciliation process.

The calculation process will include calculations which verify that the data is as
correct as expected and it will help to identify data which results from intermittent
problems (systematic errors) as well as to identify biases which accumulate within
the process flowsheet. The calculation process should provide the best possible
estimates of product metal recovery, minor element and/or elemental distributions,
ore source grades and tonnages and the accumulation of mass and metal values
within the circuit. It should also identify significant biases in the data over time. In
principle, smoothed data can be used, provided it is used on a consistent and
transparent basis.

Using the Check in-Check out System, all streams into and out of the process or
plant, for which the balance is being performed, are measured, sampled and
analysed. In terms of this Code, this is the standard procedure to be adopted for
Metal Accounting in all operations and all deviations from this approach must be
justified in an Exception Report and approved by company Management.

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Older plants, particularly those in which the metal accounting system was not
designed as a part of the initial plant specification, can experience difficulties in
applying this system. Typical problems relate to the lack of suitable installed facilities
for mass and flow measurement of all streams, resulting in incomplete accounting
data. Some operations, particularly those handling commodities such as coal or iron
ore, do not normally measure the mass flow of every stream, nor is every stream
sampled and analysed. In addition, there are certain types of operations or process
flows where accurate measurement is difficult and/or expensive.

Applying the Check in-Check out system will normally generate an imbalance, due to
measurement, sampling and analytical errors, or unknown losses. This imbalance is
treated as an unaccounted gain or loss.

The balance equation is:

Output = Input ± Change in Stock and Inventory ± Unaccounted [Eqn 7.1]


The Unaccounted is made up of:

Unaccounted = Unknown Losses ± Bias, Random and other Errors [Eqn 7.2]
For each of the accounting streams the precision of the dry mass, sampling and
analytical measurements is calculated and the precision of the overall balance is then
derived. If the imbalance or unaccounted quantity is greater than the limits defined
by this precision, or if the limits of the precision so calculated are excessive, then this
should be regarded as material and the result of an unsatisfactory measurement or
unknown loss.

The manner in which this unaccounted gain or loss is managed and investigated
must be based on procedures laid down in terms of the Code.

Beyond a transparent demonstration that "what goes in is statistically similar to what


goes out" the metal balance allows key performance parameters or indicators (KPIs)
to be calculated.

7.2 THE METAL ACCOUNTING PROCESS


Metal Accounting provides the interface between the metal recovery operations and
the financial and commercial centres of the company. It involves the recording, to
accounting standards, of information relating to the flow and transfer of metals,
while the term “to accounting standards” includes criteria such as accuracy, integrity,
security and auditability which must be met. In turn, auditability requires that all
source data must be able to be traced and all changes to the data must be
authorised and recorded, together with reasons for the change, and filed so as to
provide an audit trail. There are usually legal requirements for the period over which
metal accounting documentation should be retained, typically for a minimum of fifteen
years, although, ideally, it should be retained as a permanent record.

Metal Accounting is a routine activity based on an accounting period (typically one


month), which is usually determined by company reporting requirements, but it could
also be determined by specific reporting requirements for the operation concerned.

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Primary Accounting has been defined as the balance across an entire plant and it
is the major focus of this Code. Often, because of process time lags and process
inventory, meaningful calculations can only be made over a longer period e.g. a
quarter. Provided the accounting period selected is relatively large, compared with
the process residence time, a mass balance can be carried out using all available
data. If this mass balance indicates a large unaccounted balance, there may be
problems in the mass measurement or sampling and analysis techniques. The
source of these problems may be isolated by conducting mass balances over smaller
sections of the total plant circuit, defined as Secondary Accounting, which is used
to identify where inventory build-up is occurring, time lags are involved or where any
measurement problems exist, and/or by the various techniques discussed in Section
7.4 and in Appendix E. These techniques are utilised to reconcile the balance in
order to assess bias and other errors, or unknown losses, as well as to identify where
effort should be concentrated to improve mass measurement, sampling and analysis.

The Metal Accounting Process can be considered as a flow of measurement activity


and Custody Transfers, through the various stages of processing from ore resource
to customer. Thus, the metal balancing process will often cover several different
plants. Some typical examples of the processes and the measurement basis
commonly used for these processes are shown in Table 7.1 below.

Table 7.1: Typical Stages of Metallurgical Processing

Area Representation/Process Measurement Basis


Mine Mine Reserves or Drill Core/Geostat Model
Resource Model
Mining Process Number of
Trucks/Hoppers
Truck/Hopper Factor
Block Model Assays
Survey Measurements
Bulk Density and Moisture
Custody transfer to Concentrator Feed Occasional Surveys
concentrator Stockpile
Comminution and
Separation

To Rejects (Tailings) Flow Rates, Density,


Mass/Flow Measurement,
Samples for Moisture and
Analysis
To Products Flow Rates, Density,
(Concentrates) Mass/Flow Measurement,
Samples for Analysis and
Moisture

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Area Representation/Process Measurement Basis
Custody Transfer to Concentrate Load Certified Masses,
Transport out/Shipment Transfer to Transport
Samples for Moisture and
Analysis, Sizing, TML, etc
Custody Transfer to Concentrate Receipt Certified Masses,
Smelter Samples for Moisture,
Analysis, Sizing, etc
Residues Masses,
Samples for Analysis
Dusts and gases Flows, Samples for
Reject Solutions Analysis
Slags Masses, Samples for
Analysis

Custody transfers of material from one operation to another, (e.g. from a mine to a
concentrator, from a concentrator to a smelter, etc.) follow the generally accepted
practice of utilising the receiver’s mass, sample and analysis. Where these transfers
occur within the same company, the Home and Away System (double sampling and
analysis), whereby both the receiver and the dispatching operation independently
weigh, sample, and analyse the material being transferred, ensures that gross
accounting errors do not occur. The dispatching operation will record both the
dispatched mass and the metal contents and those determined by the receiver. The
receiver’s quantities will apply and any discrepancy is recorded as an unaccounted
loss or gain. Where serious discrepancies between the quantities reported by the
two operations occur, they must be investigated immediately and corrective action
taken.

Custody transfers of material between independent companies, e.g. toll smelting,


refining or metal purchase, require the terms of the transfer be set out contractually.
A typical approach is that the receiver and the sender will separately analyse portions
of the receiver’s sample, although the Home and Away System, described above, is
recommended. The results of the separate analyses are exchanged and compared
by the two organisations, at a pre-determined time and date. Differences between
the two results for each analysed metal are compared against splitting limits, which
are set out in the governing contract and they are based on the estimated precision
of the weighing, sampling and assay processes involved, as well as the level of risk
involved in the metal transfer. Results which fall within the splitting limits are usually
averaged, while those that fall outside these limits are usually re-analysed, settled by
mutual agreement between the parties to the contract, or sent to a third, Umpire
Laboratory, chosen by the parties. In the event of an umpire laboratory being used,
final settlement of disputed analyses is reached by comparing the umpire analysis
with those of the contract parties, based on procedures laid down in the contract.

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7.3 METAL BALANCING
In the past, Metal Accounting has been subject to many technical limitations in terms
of mass measurement, sampling, assaying and, in particular, computational power.

The last few decades have seen substantial improvement in all areas of
measurement and computational power has ceased to be a constraint. However, the
traditional methods described below are still in common use.

A distinct terminology has developed to indicate which calculation method is likely to


have been used. These terms and their associated calculation methods are defined
below.

Evaluation involves activities, some technological and some statistical, concerned


with the technical quality of the accepted data and it normally involves the
comparison of two independent measurements of the same quantity.

Recovery and accountability are separate but related parameters, the


determination of which is necessary for the efficient monitoring of the performance of
metallurgical processes and for reliable forecasting and planning.

Various formulae can be used in metal accounting exercises to calculate recovery,


depending on the specific application, although certain formulae are preferred and
specified for this Code. However, the most important issue is that the chosen
formulae should be used consistently and not changed arbitrarily to suit specific
needs at the time of reporting, as these formulae use different combinations of the
same data to give different and confusing figures for what is believed to be the same
value. It is also necessary to define the boundaries over which recovery or
accountability is measured, and over which all inputs and outputs are measured, and
this must be included in the recovery or accountability statement to avoid any
confusion.

Recovery, calculated on the basis of all process inputs, is defined as Actual, as


shown below:

Actual Recovery (%) = (sum of all useful or desired outputs) x 100


(sum of all inputs) [Eqn 7.3]
The above expression forms the basis of the recovery calculation for the Check in-
Check out approach required in terms of the Code.

An alternative approach is to use Built-up Recovery (sometimes called


Retrospective Recovery), and it is calculated based on all process outputs, as set out
below:

Built-up Recovery (%) = (sum of all useful or desired outputs) x 100


(sum of all outputs) [Eqn 7.4]
Another alternative definition used in some metal processing industries is
Theoretical Recovery, which is defined by the expression:

Theoretical Recovery (%) = (metal input – metal in losses) x 100


metal input [Eqn 7.5]

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Any reference to recovery not qualified by a statement of the type and boundary of
that recovery can be ambiguous and, therefore, meaningless. Use of any recovery
calculation method other than the Actual Recovery defined above must be motivated
via an Exception Report and approved by company management in terms of the
Code.

Accountability is defined by the following formula:

1 Accountability (%) = (sum of all outputs + stock and inventory change) x 100
(sum of all inputs)
[Eqn 7.6]
This, too, must be defined in terms of boundaries and it provides a check as to
whether over time, inputs, outputs and stock changes reconcile. It must be
accompanied by a clear indication of its confidence limits, as calculated from the
constituent measurements.

An alternative form of the above expression for accountability which is also used is:

2 Accountability (%) = (sum of all outputs + Closing stock) x 100


(sum of all inputs + Opening stock)
[Eqn 7.7]
Expression 1 provides no credit for dormant process stocks whereas Expression 2
provides 100% accountability for such dormant stocks. If these dormant stocks are
large relative to the throughput in the accounting period under consideration,
Expression 2 enhances the accountability figure, bringing it closer to 100% and it
provides an incentive to hold and manipulate large plant stocks or plant inventory.
As the purpose of a metal accounting system is to measure the accountability over a
specified accounting period, use of Expression 1 is required in terms of the Code.

Any material received by a plant from a previous processing operation, but which has
not yet entered a process stream, or any material produced by that plant to dispatch
standard quality, but which has not yet been dispatched, is generally defined as
plant stock. Any material which has entered the process stream, but which has not
yet been produced as a product for treatment in the next process, is generally
defined as process inventory.

The day-to-day data collected from a metallurgical plant is rarely consistent and it will
usually contain redundant information. In general, any two methods of calculation
will yield different results and, therefore, many factors influence the selection of a
suitable metal accounting strategy. These include the degree to which it is practical
(and economically justified) to weigh and sample accurately the feed to, and the
products from, a processing operation to achieve Check in-Check out, and the
availability of redundant data. An important additional factor is the degree to which
the metallurgical accounting system supports process performance evaluation and
optimisation.

There are some general guidelines. Mining operations and deposit models are
usually relatively sparse in terms of available redundant data. By way of contrast,
and recognising the difficulty in accurate mass measurement and sampling of ROM
ore, a modern mineral processing operation usually enjoys a wealth of redundant

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data, especially downstream of the main size reduction process. Reducing the
particle size and transferring the ore past a single point, greatly simplifies mass
measurement and sampling. Similar comments are often true for hydrometallurgical
plants.

When the material reaches the pyrometallurgical plant, the situation may well reverse
with data becoming scarce and being limited by risk of access to hot metal and by
toxic off-gases.

Table 7.2 below indicates some strategies commonly used for various types of
operations in the metallurgical industry. However, each situation is unique and
should be carefully assessed. While the dominant purpose of metal accounting is to
manage Custody Transfer, it is recommended that the same process be used to
monitor process efficiency and intermediate process inventory.

It is essential to ensure that the Custody Transfer measures are within the expected
limits. For concentrators, if limited data is available, the Two-Product Formula
(Section 7.5.1.1) or the Three-Product Formula (Section 7.5.1.2), as appropriate,
can be used to provide some independent indication of the validity of the selected
measurements. If the measurement accuracies are known and there is sufficient
redundant data, the mass balancing reconciliation measures outlined in 7.4 can
provide a robust means of checking on the measurements used for the balance. If
two measurement methods agree to within the desired statistical criteria, the Custody
Transfer measurements can be accepted as being "correct", within the limitations of
the measuring system. If the measurement methods do not agree to within the
specified criteria, the mass balance can often provide detailed guidance to identify
the source of the problem.

Table 7.2: Strategies for Metal Balancing

Type of Operation Examples


Type 1: Smelter, Metal Refinery
High grade / high value feed. Recommended strategy is Check in-
Medium Flow rates. Check out.
High Value Product.
Significant plant inventory.
Weigh and sample all inputs: Check In.
Weigh and sample all outputs: Check Out.
Type 2: Gold Operation
Low value feed – medium to high flow rates, Recommended strategy is to reconstitute
often of coarse feed. tailings at measured feed rate and
High value product. production.
Low mass, high value plant inventory.
Weigh and sample product.
Type 3: Base Metal Concentrator
Low value feed – medium to high flow rates Recommended strategy is to mass
– sampled after primary grind. balance feed analyses, concentrate

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Type of Operation Examples
Low value product – sampled as concentrate analyses and tailings analyses at
shipments. measured feed rate and production rates.
Low plant inventory.
Conveyor weigh-scale or weigh feeder for
feed mass into plant.
Accurate sampling of fine tailings.
Type 4: Coal Operation, Iron Ore
High tonnage of feed and products. A commodity sales contract will detail
Minor rejects. Low plant inventory. prices and penalties as well as
acceptable measurement techniques for
Sometimes direct shipment to customer.
both producer and buyer.
Detailed product specifications.
Recommended strategy is to weigh and
International standards for sampling and sample feed and product streams.
characterisation.
Custody transfer mass will often be a
draught survey or a train load out weight.
Type 5: Precious Metals Refineries
High value, low tonnage of feed. Recommended strategy is Check in-
High value products. Check out
Minor reject streams. Significant plant
inventory.
Weigh and sample all inputs: Check In
Weigh and sample all outputs: Check Out
Type 6: Aggregates
Low value, high tonnage feed. A commodity sales contract will detail
Minor rejects, usually based on particle size prices, usually based on tonnage and
or density. size specification.
Minimal plant inventory. Recommended strategy is to weigh
feed and product streams.
Type 7: Heap Leach
Low grade, high tonnage feed. Weigh, sample and analyse feed and
Residues remain in situ in some cases. product.
Very high, difficult to measure, process Perform accurate solution balance.
inventory. Periodic checks of heap solution
Non steady state, two phase slow reaction inventories and heap residue metal
kinetics. contents.

Type 8: Industrial Minerals


Medium to low value, high tonnage feed. May be treated as a commodity.
Low process inventory. May be produced as different grades.
Require use of Mineralogical analysis. Weigh feed and product streams.
Products may be in bulk, bags, or other
containers.

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7.4 RECONCILIATION OF METAL BALANCES
The challenge for a metallurgical accountant is to evaluate and establish the
precision of all the input variables used and of the resultant balance, to identify and
reduce errors and to improve the accuracy and confidence in the balance whilst
ensuring that data is both self-consistent and as accurate a representation of plant
performance as possible. Techniques to achieve this, such as:

• The use of Secondary Accounting


• The calculation of stream values from different components and sources
• The use of tie substances, which pass unchanged through the process
• The use of CUSUMS to identify problems
are discussed below and in the sections which follow.

All plant measurements contain some usable information and effective corporate
governance is greatly enhanced by better knowledge of which measurements are the
most valid.

Knowing the precision of each measurement, the general mathematical solution to


the fundamental problem:

“Is what comes out equal to what goes in?”

becomes a more detailed question:

"How much should each measurement be adjusted (relative to its measured


precision) to generate a mathematically exact balance?"

A mathematically exact balance means a balance where all of the balance


flowsheet constraints are satisfied and total and component masses are consistent
across the complete balance with no unaccounted losses or gains.

To make statistical statements about the balance and the results that are found, it is
necessary to adopt a specific approach to the solution of the mass balance problem.
A simple approach to the problem in which both mass flow and assays are involved
in a balance around a plant or around units within the plant is given in the paper by
Lyman (Appendix E3). In this paper, the data adjustment problem is formulated as a
mass flow adjustment problem, where the mass flow is the product of a measured
flow rate and a measured assay. The assay adjustments can be back-calculated
from the adjusted flows, but this detail is omitted for brevity.

The changes which are applied to each measured value to achieve this balance are
usually called Adjustments. When adjustments to an analysis or a mass flow are
divided by the estimated standard deviation of the corresponding measurement, they
can be described as 'weighted' adjustments. If all the measurements which are
employed in the metallurgical balance are relatively accurate, the expected value of
any one adjustment is very close to zero. The distribution of the adjustments will also
tend to be normal, but all adjustments calculated from the balance will be statistically
dependent or correlated. One might also think that the weighted adjustments should
have unit variance because they have been divided by a standard deviation, but this
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is not correct because the balance equations introduce constraints between the
values of the adjustments.

Any balance problem will have a certain number of degrees of freedom that depend
on the interconnection of the process streams and on what has been measured
(mass flows and number of species involved in the balance and whether or not total
mass flows are balanced as well as the species flows). The total sum of squares for
the adjustment problem is approximately distributed as a chi-squared random
variable with the number of degrees of freedom that the particular adjustment
problem possesses. As such, the expected value of the total sum of squares is
approximately equal to the number of degrees of freedom.

The true expected value of the sum of the weighted adjustments may vary from zero
because, for example, the simultaneous adjustment of mass flows and assays in flow
sheet is a non-linear problem. However, in many cases this expectation can be
taken to be zero.

To test whether or not the weighted adjustments being applied to the data are too big,
advantage may be taken of the fact that the weighted sum of squares of adjustments
is approximately chi-squared. Then, a goodness of fit test can be applied to the
weighted sum of squares value. If it exceeds the chi-squared value at, say, 95%
confidence for the appropriate number of degrees of freedom, there is an unresolved
problem. Either the estimates of the data precision are incorrect or some
combination of measurements has a precision lower than stated. One or more
values used in the balance may be biased. The cause for the excessive weighted
sum of squares should be investigated. Under such circumstances, an Exception
Report must be generated.

It can be difficult to pin down which of the measurements causes the increase in the
chi-squared value. The best approach is to conduct the balance successively with
more and more analyses included in the balance, or with different combinations of
analyses. This strategy may show up the problem quite quickly. The important
statistical results with a case study are provided in Appendix E.3. An alternative
approach to balancing data is provided in Appendix E.1

The examples provided do not consider internal stockpiles (or bin inventories for
example). However, they can be included in the balance by creating an input stream
for draw-down from a stockpile and an output for build-up of a stockpile. It is critical
that the accuracy with which these inputs and outputs can be estimated is
determined.

In many cases, the accuracy on the draw-down or build-up will be low and
adjustments to these mass flows will represent the majority of the overall adjustments
applied to the data. The overall confidence limits attached to the period balance will
be correspondingly wide with a concomitant increase in the risk associated with the
balance. A high risk level may necessitate an improvement in the way these stocks
are handled.

Each change to the raw data must be recorded and justified, and then authorized by
the responsible senior management appointee. An audit trail must be available to
trace the path from the initial balance with its associated recovery and accountability,

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to the equivalent values in the adjusted balance for the accounting period and this
information must be available for audit purposes. The adjusted balance must clearly
indicate the magnitude of any adjustment.

7.4.1 Detecting Random Error (or Illegitimate/Spurious Errors)


If a measurement has been adjusted by more than twice its estimated standard
deviation, then it is worthy of further examination. If a subsequent balance, which
omits this measurement (or increases the estimate of its standard deviation), shows
a significant overall improvement, the measurement is likely to be in error. However,
some investigation is usually required to ascertain whether the error is random or
spurious – or even a larger than usual bias.

7.4.2 Bias
The problem of bias is important and may not become apparent until many balances
have been carried out. The objective is to identify and to eliminate bias, not to adjust
data, and thus conceal the bias. For a given balance structure, it is possible to
calculate the variance of the arithmetic sum of the weighted adjustments for each
analysis type (this calculation is not detailed in E.3, but it can be derived from the
results there; it will be applicable to that type of balance only). With this estimate of
the variance for the analysis type, it is possible to test the significance of the sum of
the adjustments.

Appendix E.3 also provides the covariance matrix of the adjustments and the
diagonal elements of that matrix provide the variance of the adjustments. These two
can be used to test the magnitude of individual adjustments. Note that the
adjustments should be tested against their variance, not the variance of the original
measurement.

The comments about detection of a bias (1.7.2) which is small relative to the
accuracy of measurement for a single accounting period are still valid. The relevant
Cusums can be of adjustments (or of weighted adjustments) for each measurement.

A graph, which shows measured and adjusted data plotted together against
successive accounting periods, will often show a bias very clearly. That is, instead of
crossing on a reasonably frequent basis, one line will lie above or below the other for
many accounting periods.

7.4.3 Estimating Flow Rate Accuracy


The general approach described in Appendix E.3 provides estimates of variance for
each flow rate in the balance which are intrinsic to many reconciliation methods.
However, for other methods some random variation can be added to each
measurement or adjusted value and the solution re-calculated many times. This is
called a Monte Carlo approach. The variation of flow rates, or parameters such as
accountability and recovery, provides an estimate of the variance of each. In
qualitative terms, a small variation in a well-defined flow rate will produce a much
larger variation in the sum of squared adjustments than a similar variation in a poorly
defined flow rate. If a flow does not produce any variation in the sum of weighted
squared adjustments, it is very poorly defined.

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7.5 METAL BALANCING APPLICATIONS

7.5.1 Concentrators with minimal accumulation


Metal accounting in concentrators is based on one of the recovery expressions
referred to in Section 7.3. The specific expression used, actual recovery (required
in terms of this Code) or built-up recovery, will depend on the information available
to the plant management and, in particular, on where the primary feed sample is
taken. Ideally, where sufficient information is available, both expressions are used
and compared to identify accounting discrepancies, but only one will be used for
accounting reports. As there is no significant accumulation of process inventory in
this type of concentrator, accountability is measured by comparing all outputs with all
process inputs over the accounting period.

As values of recovery, concentration ratio and enrichment ratio (c/f) can be


determined from analytical results alone, the two-product formula is often used to
provide information for plant control, although this will be retrospective, depending on
the time taken to receive and process assay results. Direct control can be achieved
by the use of on-stream analysis systems through which values of c, f, and t can be
continuously measured and computed to provide up-to-date values of metallurgical
performance.

There are many methods used to account for a plant’s production and most
concentrators produce a metallurgical balance showing the performance of each
shift. These balances are accumulated over a longer period (eg: daily, weekly,
monthly, annually) to show the performance over the period in question. The actual
recovery over the accounting period is declared and any discrepancy between that
and the accountability is regarded as an unaccounted loss or gain. Physical
losses do occur on any plant and every effort should be made to keep these as low
as possible at all times. Care must be taken to ensure that the balance is not
compromised by recycle streams and the return of plant spillage to the circuit
especially if these are of higher or lower grade than the main stream.

7.5.1.1 The Two-Product Formula


Typically, in concentrators, it is possible to obtain reliable measurements of
the feed (once the ROM ore has been reduced in size) and concentrate
masses, but it is usually more difficult to measure the mass of the tailings
stream. In order to assess concentrator plant performance on a shift or on a
daily basis, and to control the operation using the evaluated results, it is
necessary to account for the products in terms of material and contained
component masses. Thus, if the masses of the feed, concentrate and tailings
are F, C and T, respectively, and their corresponding assays are f, c, and t,
and it is assumed that there are no closure errors in the mass balance (i.e.
F – C – T = 0), the two-product formula below can be used. (If the tailings
mass is also accurately known, any closure error can be reported as an
unaccounted loss or gain of material).

Therefore: F=C+T
And: Ff = Cc + Tt
Or: Ff = Cc + (F – C)t

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This gives: F/C = (c - t)/(f - t) [Eqn 7.8]
where F/C is the concentration ratio.

Therefore, C/F = (f – t)/(c – t) and


plant recovery = (Cc/Ff) x 100% = 100c(f – t)/f(c – t) [Eqn 7.9]
Equation 7.9 is known as the Two-Product Formula

7.5.1.2 The Three-Product Formula


In some concentrators, typically lead-zinc concentrators, for example, more
than one concentrate is produced in addition to the tailings. Using the
example of a lead-zinc concentrator, if the weights of the feed, lead
concentrate and zinc concentrate and tailings are F, P, Z, and T respectively
and their corresponding analyses f, p, z and t, then

F=P+Z+T

i.e. material input = material output

If one of these weights is known, the other three can be calculated, provided
that two component balances are available, i.e.

Ff1 = Pp1 + Zz1 + Tt1

Ff2 = Pp2 + Zz2 + Tt2 [Eqn 7.10]


where f1, p1, z1 and t1 represent the analysis of component 1 and f2, p2, z2 and
t2 represent the analysis of component 2. Hence, application of the three-
product formula requires two component analyses on each product.

From these calculations, the concentration ratio and metal recoveries can be
calculated in a similar manner to the two-product formula above.

The three-product formula has its limitations. The equations assume steady-
state conditions and the fundamental assumption that input is equal to output.
This is true over long periods but it may not be true over shift periods. The
three-product formula is subject to appreciable errors when the components
are poorly separated and it is preferable to obtain accurate mass flow
measurements of products rather than to infer them in this way. The formulas
of three or more products are more sensitive to small errors both in data and
calculation, especially when one of the products is of relatively small weight
and low concentration, and this can lead to serious balancing errors (Taggart
1945).

Plants using this approach typically prepare three-product formulae


metallurgical balances on a daily basis. These daily balances are
accumulated over the accounting period, in order to obtain the weighted
average analyses of the streams for the period. It is obvious that the values
of concentrate and tailings weights calculated by this method are totally
dependent on the analytical values. Because of inaccuracies in obtaining
representative samples from continuous flow streams, and due to errors in

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analysis, the calculated values of concentrate and tailings weights can vary,
depending on the components used to determine the balance.

7.5.2 Concentrators with Intermediate Accumulation


Over a typical accounting period (e.g. a month) where a change in inventory in a
concentrator occurs, it can be quantified by assessing the amount of concentrate
retained in the plant in thickeners, tanks, filters, etc. and in stockpiles in the
concentrate handling and dispatch area.

Although sampling and analysing the stockpiles and other areas of accumulation can
assess the metal content of the inventory, it may be more accurate to rely on the
weighted concentrate analysis produced from daily or shift plant balances.

Where accumulation in plant inventory occurs, the determination of the concentrator


recovery has to take this into account. The two-product formula to be used is then:

Recovery (%) = [(Cc + change in inventory) x 100] / Ff [Eqn 7.11]

7.5.3 Coal Treatment Plants


In the coal industry the practice of metal/commodity accounting, on a full Check in-
Check out basis, is not rigorously practised, in the sense of tracking a valuable
component in the plant feed/ore to a final product containing an enhanced
concentration of that valuable component.

A metal/commodity balance could be performed on the basis of an ash balance.


However, this would require extensive sampling of all waste streams, which is not
generally the practice in coal preparation plants. Reconciliations could be completed
to cross check declared yields at fixed size ranges against a ROM washability,
although this would be of limited use, as it does not simulate the actual separation
process.

Materials balances are generally completed on an air-dried basis, which tracks ROM
coal as it leaves the pithead, to the point of delivery to the final customer as a final
product. Balances to account for the reject materials can be completed but this is
done to varying levels of detail, depending on the value it is considered to add to the
accounting process.

Whilst the formal application of metal/commodity material balancing has limited


application in coal, there are nonetheless stringent requirements regarding the mass
measurement and sampling of coal (Refer to Appendix C.2.2) as contained in various
international standards. Emphasis is placed on achieving the desired consistency of
the quality of the coal and the implementation of quality control systems such as
those defined in the relevant ISO standards.

7.5.4 Pyrometallurgical Plants


Pyrometallurgical Plants include roasting, calcining and smelting processes.
Smelters introduce phase changes into the processing chain, in that feed materials
are melted and chemical reactions, usually involving oxidation and reduction, take
place to separate the valuable components from the gangue and impurities, thereby

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upgrading them. The products normally proceed as feed material to the next stage of
refining. The usual process stages are:

• Feed material preparation (such as crushing and drying), roasting or


calcining, often followed by smelting with various fluxes and/ or reductants in
a furnace
• Withdrawal of a molten matte, alloy or metal from the furnace and upgrading
and/or purification of this to product for dispatch by various means such as
converting
• Removal of molten slag for treatment to recover valuable constituents and/or
disposal and gas and dust recovery. In some cases, such as with ilmenite
smelting, the slag is a product for sale.

Feed
The feed material depends on the purpose of the pyrometallurgical plant. This may
be a reducing or an oxidising roast, smelting of sulphidic metal containing materials
to remove gangue materials and iron, melting to reduce oxides (ilmenite smelting),
the oxidation of unwanted species in the metal phase (steel making), or melting to
separate the metal phase from the oxide phase. The gas phases may be air/oxygen
or reducing such as carbon monoxide depending on the purpose of the smelter.

Feed is often mineral concentrate or ore and reducing agent (anthracite/coal) and/or
fluxes from an adjacent plant or from another supplier and it may be from the same
company or it may be for toll treatment. However, many other materials can also be
treated in a furnace owing to the nature of the process. These include recycle
streams from elsewhere in the process and scrap. All these materials may contain
moisture and it is important that appropriate samples are taken to establish the dry
weight.

In-house concentrate may be pumped from thickeners or transported in suitable


containers or tankers as a filter cake or as slurry. This must be weighed in these
containers or, if pumped slurry, measured by electromagnetic flow meter and density
gauge and sampled with suitable equipment. It can also be measured by conveyor
belt weighing or bin weighing after drying, before being fed to the furnaces. Ore or
other feed materials must be weighed on delivery by road/rail and/or by belt weigher
or weigh bins when processed.

Pneumatic conveying is sometimes used for transport of the dry material to the
furnaces. In this case the material is usually weighed in batches in weigh bins at the
feed end or in bins on top of the furnace. The weight and analysis of the feed
material should be compared with that from the supplying concentrator or mine. That
weight may have been calculated from the two-product formula and/or measured on
static scales such as weigh bins or weigh tanks. This usually means measuring or
estimating the stock held in thickeners or stockpiles, which, as highlighted previously,
is difficult and inaccurate. However, the comparison can highlight problem areas and
arrangements can be made to reduce or eliminate the stock periodically to provide an
absolute stock value.

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Which of these values for the inputs should be used on an ongoing basis for the
metal accounting calculations should be decided based on an assessment of the
accuracy of the equipment and the methodology used to measure the mass and take
the samples at the various points.

Toll treatment materials are processed under contracts, which specify the mass
measurement and sampling methodology for custody transfer and which often
include weighing and sampling in dedicated facilities , after crushing or slurrying, in
order to obtain representative samples. Calculated contents are compared with those
of the supplier and they are subject to agreed maximum tolerances (splitting limits
and umpire analyses). Payment terms, toll refining charges and recoveries are
based on the agreed calculated weight and content. Normally, the toll treatment
company will guarantee a specific recovery within a certain time frame and it will
deliver to the supplier the agreed quantity of product or market it as part of its own
production. Thus any gain or loss resulting from the actual recovery achieved can
reflect on the recovery of in-house materials.

Products
Products are usually furnace or converter matte, metals, metal alloys, and metallic
anodes and they constitute one or more metal phases), an oxide phase and, in some
cases, a gas phase. These are normally sold or sent to a refinery for further
processing. This further treatment may be in-house or on a toll refining basis. In all
cases the product, which may be crushed or granulated, or in the form of ingots or
lumps, must be weighed by the supplier and the consumer on static scales, weigh
bins or on conveyor weigh scales, and sampled/analysed by both parties. The
calculated contents must then be compared and those for metal accounting use must
be agreed according to contractual terms or in-house procedures. This weight is
usually the most accurate mass measurement in a smelter. However, the material
often contains some moisture and this can introduce a significant source of error
depending on the mode of storage, loading/unloading, transport and sampling and
can change during these operations.

Slag
Furnace Slag is usually a discard from smelting operations, although often it is further
processed to recover contained or entrained metals before being discarded.
Normally, losses of valuable constituents are a relatively small percentage of the feed.
Sampling and weighing of furnace slag depends on the manner in which the slag is
handled after it is tapped from the furnace. Samples can be taken during the tapping
operation from the molten material for plant control, but these are not recommended
for metal accounting use. If the slag is granulated or crushed before further
treatment and disposal, sampling and weighing must take place during the conveying
or trucking to treatment/disposal. In some cases, such as in the smelting of ilmenite,
slag can be a product for sale and it should be weighed and sampled as for other
smelter products.

Converter Slag usually contains significant levels of valuable metals. In some


operations it is discarded with the furnace slag, in which case it must be sampled and
weighed in a similar manner to that used for the furnace slag, to ensure satisfactory
metal accounting. Normally, converter slag is subjected to further processing in slag
cleaning furnaces before discarding or it is recycled to the smelting furnaces for
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recovery of the contained metals. Transfer usually takes place as hot liquid metal in
a ladle transferred by a crane. This transfer can be weighed by load cells fitted to the
gantry cranes and sampled to meet internal plant or Secondary Accounting
requirements.

Dusts / Gases
Dusts are recovered from the dust removal equipment treating the off-gases from the
furnaces, converters or other process steps and the dust extraction equipment on the
transfer points. This dust is normally returned to the process but it is not usually
weighed and it is treated as an internal recycle. Some dust is lost to the atmosphere.
This normally contains only a small proportion of the valuable constituents in the
smelter feed and measurement of the mass and sampling on a periodic basis may be
satisfactory, in these cases, to provide an estimate of the losses.

Off-gases may be also recovered to utilise their waste heat or to recover pollutants or
economic constituents.

Sulphur Fixation
In the case of sulphide smelting, a proportion of the sulphur is recovered as sulphuric
acid, or as sulphur fixed in some suitable compound or, in some cases, it passes
directly to the atmosphere as sulphur oxides without any treatment. Sulphur is
usually analysed in the off-gases and the final sulphur product is weighed and sold if
it is sulphuric acid or some other tradeable product.

Smelters operate under permits that limit the mass emission of sulphur to the
atmosphere and they are subject to environmental regulations that specify
permissible ground level concentrations of various pollutants such as sulphur dioxide.
Thus a balance must be performed to calculate recovery and losses of sulphur.

Metal Accounting
Recovery and accountability for smelters and pyrometallurgical plants are
calculated utilising the same formulae as shown in Section 7.3. For Check in-Check
out all input and output streams around the plant must be measured and sampled
leading to the calculation of material balance closure errors for various species.
These balance closure errors reflect the material that is unaccounted. However,
dust and gas losses are normally subject to a high level of uncertainty and slag
quantities are often not accurately measured, thus Check in-Check out cannot be
carried out for species affected by such losses and lack of measurement. Slags are
not homogeneous, they may have metal or alloy inclusions, and may contain varying
amounts of moisture, especially in the case of water-granulated slags. However, the
metal content in gases, dusts and slags is usually only a small proportion of the feed
and, as such, the effect of omissions on the balance should not be significant. The
amount of effort put into improving the accuracy of measurement of dust and slag
losses is dependent on their magnitude and value, risk potential and the
requirements for environmental reporting. However, it is recommended that furnace
slag be weighed before disposal or recycling rather than using truck factors, which
are notoriously inaccurate, as this will provide more accurate information for closure
of the balance.

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Smelters represent a challenge in terms of metal accounting because of the difficulty
in measuring in-process inventories, intermediates and recycles, which are often
significant; these include material from ladles and refractory repairs and metal/alloy
build up in furnaces. Furthermore, the materials in streams around furnaces and
converters are coarse, highly heterogeneous, variable in grade and they may be
molten. They are therefore among the most difficult materials to sample.
Nevertheless, the accounting system must either treat these materials as in-process
stock or recycle them out and back into the process on a Check in-Check out basis.

Suitable tie components such as iron or silica, which report solely to one stream, or
whose distribution is known, which are abundant and which can be readily analysed
to a high precision, can also be used to calculate multiple balances, to provide
redundant data and to facilitate the solving of anomalies, especially where Check in-
Check out is not performed. In some cases indirect measurements such as
temperature can assist in providing additional data.

The mass balancing of reducing agents such as coke or anthracite is important in


many pyrometallurgical operations as they are a major cost component and critical to
process performance. Thus a carbon balance is important.

Stocks are particularly difficult to measure accurately and they should therefore be
kept to a minimum and, ideally, they should periodically be run down to zero since
month-to-month recoveries can give a distorted picture of the metal balance.

One practical way of calculating recovery over a period is to obtain a balance closure
for a minimum of three major elements; this will provide redundant data and thus
enable problem areas to be identified.

Internal, Secondary Accounting between process stages is complicated by the


recycling of materials which are normally returned to the furnaces (sometimes in
molten form) and which are often not weighed and sampled. Dust from the dust
recovery equipment is also recycled to the furnaces and it is also often not weighed.
Thus the individual balances over the various process steps, required for plant
performance, are more complex than for the smelter as a whole. However, the
balance around individual process steps can assist in strengthening the reliability of
the Primary balance. There is also the possibility of combining one or more process
steps where that combination will clarify the accounting because the inputs and
outputs can be well quantified.

Care must be taken to ensure that the system design for the mass measurement and
sampling, allows for recycle streams and for the intermittent return of spillage.

In addition to the above issues, the inherent variability of individual furnace


processes in relation to the accuracy achievable through appropriate sampling and
analysis can either produce a bias in the overall balance or it can reduce the overall
accuracy of the balance.

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7.5.5 Hydrometallurgical Plants
Hydrometallurgical plants are often the last stages in the processing chain to produce
saleable products. As such, they are usually relatively complicated with multiple
stages, many circuits for purification and upgrading and several recycle streams. In
addition, Metal Accounting is often required for more components than in the earlier
stages of processing, including for multiple products, residues, impurities, reagents
and effluents. Processing will normally involve dissolution or other preparation of the
feed material, separation and purification of the valuable constituents and the
production of the final products as metals, salts or solutions and thus measurement is
required in solid, liquid and, sometimes, gaseous phases. The liquid phases may
include metals in organic materials as well as aqueous solutions.

Feed
Hydrometallurgical plants typically treat a solid feed material, such as ore, flotation
concentrate, matte or other intermediate materials, including metal alloys, scrap
metal, metallic concentrates and a variety of recycled materials in solid or liquid form,
all of which may contain some moisture. The materials may be products from an
earlier stage of processing from the same company or they may be purchased for toll
treatment from outside companies. The comments in Section 7.5.4 on Smelters are
equally applicable for measuring, handling and treating these materials.

Products
The feed materials are processed to give product metals, salts, oxides or other metal
containing materials, as well as process effluent streams, and, often, intermediate
products for treatment at some other facility.

The solid products can normally be weighed and sampled to a high degree of
precision by using static weighing methods during the final packaging into drums,
bags or bales and again during dispatch, giving check weights. Terms of sale will
usually specify the acceptable precision and that mass measurement instruments
must be certified for custody transfer. Solutions must likewise be weighed in the
drums or tankers on certified equipment. In some cases, products may be solid
residues sold for further processing. These may also contain moisture or solution
and they may be in the form of slurry or filter cake.

Measurement of process effluent streams is critical to establish losses of valuable


components (including reagents) and impurity content in order to conform to
environmental permits and good corporate governance as discussed further in
Section 7.7.

Metal Accounting
As process streams can be made up of either, or both, solids and liquids with both
containing significant quantities of metals, the metal accounting system for such
plants must make adequate provision for the sampling and mass measurement of all
components of each feed and output stream and it must allow for the measurement
and assessment of continuous recycle streams and of process spillage which may
occur on a periodic basis.

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Check in-Check out is essential for the feed and product streams including liquid and
gaseous effluents. The precise measurement of the latter is difficult, but usually the
mass content of these streams is relatively small. Mass balancing of the individual
process steps and circuits is important to monitor process performance and can
provide checks on the Primary Accounting.

Depending on the specific operation, the feed material is usually stockpiled ahead of
the process to ensure continuous operation. Estimation of the metal content of the
stockpile, however, can be a significant factor in overall process metal accounting.
Similarly, hydrometallurgical plants usually have a significant process inventory, in
the form of metals in solutions and in solids, including the inventory in solvent
extraction and electrowinning circuits. Estimation of this inventory is complicated by
the changing metal contents of the solid and liquid phases as they progress through
the plant and it has to incorporate tank level measurements, slurry pulp densities and
solution and solids analyses at each stage of the process. The presence of a large
stockpile of feed (or any other semi-processed intermediate) material complicates
this estimation.

In plants treating high value metals, the process inventory estimate should be verified
at prescribed intervals by physical stock-takes, using the procedures such as the
‘bubble’ method, to reduce the probability of major stock write-offs caused by
undetected errors in the routine accounting system.

Determining metal recoveries in these plants has to be based on the company’s


requirements and guidelines but it must be calculated on a consistent basis. For
example, a plant recovering several metals from one or more feed materials may
decide to base all recovery figures on the primary product metal only, as this could
be the basis on which all financial reporting is carried out. The procedures should
also clearly define how the recovery is calculated, to allow for changes in process
inventory and to define how metals contained in intermediate products for treatment
by third parties should be handled. For example, the procedures should clearly state
whether the metal in these intermediate materials should be treated as product metal,
or whether the recovery calculation should allow for future losses of metal from these
streams as they undergo further processing.

Hydrometallurgical plants are subject to losses of valuable materials in effluents and


they also normally generate various solid residues, which will contain some metal
values in both solid and solution. Effluents are treated to minimise the losses, to
recover as much of the valuable constituents as possible and to remove deleterious
impurities before disposal. Similarly, solid residues may be retreated before being
discarded, sold or recycled to earlier stages of processing. Besides the valuable
constituents, it is necessary to measure, account for and report on various impurities
and pollutants to ensure conformity with environmental regulations.

7.5.6 Heap Leaching


The heterogeneous (two-phase), non-steady state nature of Dump and Heap
Leaching, together with a protracted leach cycle (several months) and the
consequent large process inventory all complicate metal balancing. In addition, the
fact that the process inventory includes unleached, partially leached and fully leached
ore, as well as solution with varying metal contents, and that a significant proportion

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of the metal is not recoverable, raises issues that are not encountered in other
processes. (In-situ leaching has the same problems to a much greater degree, but it
is not covered in this Code, as it is regarded as a part of the mining process).

Although the principles which follow can be applied in theory to both dump and heap
leaching, in practice they would be impossible or not cost effective to achieve for
many dump leaches where the metal content of the dump is not known with any
degree of accuracy, and which cannot be adequately sampled, where the material is
of low grade or value and high mass and thus Check in-Check out cannot be
achieved or is not economically justified. Therefore, the recommendations in the
following sections will refer to heap leaching only.

In large heap leaching operations, there are often many piles being operated in
parallel but at different stages of the leaching cycle. The large inventory also means
that the effect of input or other changes is subject to long delays and it is not readily
apparent.

Process inventory in heap leach piles or pads has the following components:

• Metal in solid form in the material (undissolved but not recoverable)


• Metal in solid form in the material (undissolved but recoverable)
• Metal in solution which has been leached as the solution percolates through
the heaps
• Metal which has been dissolved into solution but re-precipitates in the leach
bed, due to local conditions such as pH changes. This will slowly re-dissolve
as conditions are corrected
Process inventory is normally reported as the second and third items above, as the
total amount of the metal in the heaps is not relevant if it is not recoverable.

The main concerns are the inventory build-up of metal in the leach solution and the
determination and prediction of the recoverable metal in the feed material. The type
of heap construction, as discussed further below, affects the determination and
significance of these inventories.

7.5.6.1 Types of Heap Leach


Single lift heaps
The material for leaching is mechanically placed on gently sloping terrain in
modules (which may be separated by berms) from which the drained solution
can be measured and sampled separately from the others. This type of heap
will tend to have fewer problems with inventory build-up. The individual
modules can be monitored separately and the total area under irrigation
remains fairly constant, and this leads to a more stable solution volume
inventory in the heaps, with the content then changing as feed grade
changes. These heaps can be washed (eluted), after completion of leaching,
to remove most of the metals in the solution. It is usual to sample them by
auger or drill to determine the completeness of leaching of the recoverable
metal and the value of the residue.

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On/off “dynamic heaps” can also be used where the residue, after completion
of leaching is removed, in which case sampling is easier and more accurate.

Multiple Lift Heaps


These are similar to the above, except that material is placed on top of the
first heaps after a period of leaching has taken place. This process may be
repeated several times. Thus solution inventory will always increase as the
leach solution saturates the new material and permeates into the earlier
deposits. In addition, the fact that the leach heaps are usually higher may
affect permeability, thus further increasing inventory and affecting recovery.

Valley-fill Multiple Lift Systems


These heaps are placed in valleys and the determination of inventory is
problematic, as the monitoring and control of the solution is difficult due to the
shape of the terrain and the fact that pregnant liquor may be retained in the
heap.

7.5.6.2 Mass Measurement Sampling and Analysis of Process


Streams
Feed
Feed material can be Run of Mine Ore from opencast operations and/or
dumps of low-grade ore that have been stockpiled. (In the latter case the
treatment is sometimes of a secondary nature for material that was not
initially economic to treat). This material is usually crushed before being
placed on the heaps but it may be agglomerated if it is too fine to permit an
adequate flow of solution through the heap. Determination of the mass of
material, and sampling to determine the metal content of the material being
placed on the heaps, are both very important. They must be carried out
according to prescribed procedures which must comply with the requirements
of this Code and Guidelines.

The most suitable place to perform these measurements is on the crusher


product conveyor, before any water and additional reagents (e.g. acid, lime
cement) are added, where adequate weighing and sampling equipment, as
defined in this Code, can be installed. In the case of run of mine ore, blast
hole sampling measurements should also be available and these figures
should be reconciled with the crushed ore samples and the block ore grades.
In both cases, the material must be tracked to the leach heap to provide the
amount of material and metal or recoverable metal placed on the individual
cells or modules of the heaps and pads. This is also important in order to
generate information which can be used to predict performance for later
operation.

Samples of feed, crushed to the size deposited on the heaps, should also be
taken for leach tests on weekly or monthly composites, to predict the
recoverable metal and reaction kinetics for the material being deposited and
for comparison with the original feasibility test work.

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Solution Balance Monitoring and Management
The pregnant solution containing the dissolved metals is often stored in
dams before being withdrawn for further processing. The barren solution
after processing is usually returned to make up the leach solution used to
irrigate the heaps.

The solution metal balance for each heap or module is the first indication of
the heap performance. Irrigation solution and drained pregnant solution from
each heap must be accurately measured by suitable flow meters, which can
be calibrated according to recognised techniques and sampled for analysis,
according to this Code. Reconciliation of these flows is important in order to
provide a calculation of the solution inventory in the leach piles, the metal
extraction from all the heaps or modules under irrigation, and total plant
production. Performing this reconciliation requires estimates to be made of
the amount of rainfall, evaporation and the solution content of each
abandoned heap. Rainfall and evaporation should be based on actual site
measurements over the accounting period. The solution content of operating,
abandoned and resting heaps should be periodically established by test work,
although standard figures based on experience are often used. It should be
noted that the metal content in the solution in the heaps is normally the
largest component of the total solution inventory and it can be equivalent to
several months production, thereby emphasising the importance of this figure
to the metal balance.

Metal Accounting
An accurate solution metal balance must be obtained, so that the total metal
recovered from the material abandoned can be calculated. The importance of
an accurate measurement of the metal placed on the heap was highlighted
above. However, the accounting is complicated further by the fact that not all
the metal is recoverable, and this non-recoverable metal can form a
significant percentage of the total, leading to a very large process inventory.
It is common practice, therefore, to use the recoverable metal placed on the
heap, rather than total metal, for process control and for mass balance and
performance calculations. If recoverable metal is also being used for
accounting, then this must be approved by means of an Exception Report.

This recoverable metal should be determined, for the specific material being
placed, by suitable laboratory tests such as rolling bottle or shake tests, or
pilot scale column tests, on representative samples. These values are then
adjusted by factors, based on experience in older heaps, to reflect the
predicted ideal performance of an operating heap. The procedures and
methodology for performing these tests and calculations should be rigorously
designed, documented and monitored. Thus, the balance will reconcile the
output metal in solution with the inputted recoverable metal to give the
recoverable metal still in the heap in both solid and solution forms.

To achieve a Check in-Check out balance, when a particular pile/heap has


reached the end of its life after leaching and washing has been completed, a
closing balance must be performed and the heap sampled to check the
amount of total and recoverable metal remaining. This sampling should be
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performed by mechanical drill/auger or preferably by sonic drilling on a
regular grid designed in accordance with sampling theory to give the requisite
number of samples for a meaningful result if the material is to be left in place.
If it is to be moved, such as in the case of an on-off heap, it must be sampled
by approved methods as it is being removed. If it has been decided not to
perform Check in-Check out, such as when the metal leached has been
calculated solely from the solution content subtracted from that fed to the
heap or pad, then this must be approved in an Exception Report.

The metal that was not recovered must be removed from the plant inventory
when a heap is abandoned. If variations in feed grade are small, then, as
many heaps are operated at one time, the process inventory will tend to
stabilise as heaps are established and abandoned. Sampling of heaps is
subject to a high level of inaccuracy and due cognisance of this must be
taken in the use of the information generated for stock evaluation and in
predicting future performance.

The metal balancing from the output leach solution through the purifying and
refining steps to metal product is similar to that for hydrometallurgical
processes shown in Section 7.5.5. General practice is to calculate the
recovery as the metal finally produced, after the purifying/ refining process, as
a percentage of the metal placed on the heaps.

Process modelling based on laboratory, pilot plant and actual performance is


important in order to improve the predicted recovery from a specific operation
and, for metal balancing purposes, to enable better predictions of the
recoverable metals and process inventory. Modelling can be empirical or
deterministic and various modelling tools can be used. Empirical modelling is
based initially on test work and it should be updated regularly, based on the
actual performance of an operation.

7.5.7 Bench Scale, Pilot and Demonstration Plants

7.5.7.1 Introduction
The throughput scale of pilot plant testing covers a large range from Bench
Scale Plants through Pilot Plants to Demonstration Plants.

Pilot plant work is undertaken for a number of different objectives such as:

• Determining process economics


• Performing process development
• Demonstrating technical feasibility
• Providing technical services
• Supporting market development
Pilot plants must be designed to meet the relevant objective. This type of
testing is often desirable and it is required, both by in-house procedures and
by external financiers, as part of the Risk Management process for a new
metallurgical project or process, or for new stages of a process. Thus testing

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is critical to the decision whether to proceed or not. Some or all of the scales
of testing may be appropriate. Normally, testing would proceed from bench to
pilot plant and then possibly to demonstration plant, with each stage of
proving the process reducing the technical risk and demonstrating the
feasibility on a larger scale.

The degree and scale of testing required is dependent upon:

• the novelty and degree of understanding of the process or process


stage
• knowledge of the metal content and impurities and behaviour of the
material to be treated in the specific process
• the scale of the commercial operation
• the degree of risk, both financial and commercial, as well the risk to
reputation.
The above considerations determine the scale-up factor to the commercial
plant that is acceptable. This may vary from a factor of 10 for a new
technology to 1000 for a typical well-known South African gold ore, for
example.

7.5.7.2 Feed Materials


Feed materials for pilot plants may be bulk ore samples that have been
collected from a site by a drilling and sampling programme, or they may be
partially processed materials from various sources that have been collected
and brought to the test facility; however, they may also be a portion of a
stream taken on an on-going basis from an operating plant, in which case, the
pilot plant is located at that plant. In all cases, sampling procedures must
ensure that:

• the pilot plant feed material is representative of the ore body or the
material to be tested
• the sampling protocol must ensure that there is continuous traceability
of the bulk sample from source to pilot plant
• the mass is measured and monitored according to the recognised
procedures as required by this Code.

7.5.7.3 Design
Metal Accounting for pilot plants must embody all the principles covered in
other sections of this Code. However, in addition, the following factors must
also be considered when designing the plant and the system for deriving the
metal balance:

• The design of the pilot plant must take into account all safety, health and
environmental factors as well as company and regulatory requirements.
Hazops analysis should be carried out

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• The normal design process must be followed, such as process design
criteria, PFDs, P & IDs, and equipment specifications, with adequate
provision for mass measurement and sampling to the requirements of
this Code
• The pilot plant can be used to establish extraction or recovery of the
primary products as well the deportment of impurities, effluent quality
and the consumption of reagents
• The plant can also be used to assist in proving materials of construction,
and establishing process control philosophy and key measurement
parameters
• Pilot plants are often operated under variable flow rates and conditions,
in order to establish the optimum conditions for the full scale plant
• Bench scale tests may be batch, but a pilot or demonstration plant
should operate continuously and appropriate streams be recycled
• Pilot plant circuits and designs are often based on scale up from
laboratory or bench scale tests and circuits may be subject to change,
thus flexibility must be allowed for
• The information obtained will be scaled up by some orders of magnitude
to design the full-scale plant, thus errors will have an effect on both
capital and operating costs, as well as on performance
• In many cases, the performance of the full-scale plant will be less
efficient than the pilot plant because of inefficiencies in the larger scale
equipment, and factors need to be applied for assessing the viability of
the full-scale process. These factors can only be based on previous
experience and company policy
• The generation of sufficient product for evaluation by potential
customers may be required
• Pilot plants can be used to facilitate the training of supervisors and
operators.

7.5.7.4 Operation
The design and operation of the plant must allow for suitable equipment and
procedures, in line with the Code, for mass measurement, sampling and
analysis that will ensure that meaningful results to a known accuracy can be
obtained for the metal balances and to facilitate the decision process.
Operating and sampling manuals are required.

As a fundamental principle, all input and output streams must be accounted


for, i.e. Check in-Check out and:

• accountability must be better than 100 % ± 5 % at 95% confidence


levels for the product metals and 100 % ± 10 % for impurities, for the
results to be utilised for economic and process decisions
• as quantities are much smaller than a full-scale plant, static weighing on
certified weighers only must be used to establish feed and product

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weights. Conveyor belt weighers or other approved mass flow
measurement devices may be used for control of flow to the process but
these must be reconciled back to the batch weights of feed determined
by static weighing
• samples are a larger proportion of the process flows than in a full-scale
plant and the mass and metal content of the samples must be included
in the metal balance as part of the Check in-Check out
• similarly spillage must be collected, weighed, analysed, and accounted
for in the balance at the appropriate stage. It should not be returned to
the circuit, as it causes process disturbances. Spillage should be kept
to a minimum
• effluents must be collected, accurately weighed and sampled
• appropriate metal balancing methods must be used to estimate plant
performance
• the entire sampling frequency and plan must be statistically designed to
yield meaningful results, allowing for the fact that planned variations in
operating conditions will occur and that different circuits may be tested,
that a wider range of analyses, to a much better precision, is required
than on a full-scale plant and that stage by stage performance
measurement is often necessary (i.e. both Primary and Secondary
Accounting)
• pilot plant operation must be carefully supervised on a continuous basis.
Each shift should be under the control of a graduate and it is essential
that the operators are trained and have sufficient experience in order to
ensure that the sampling, weighing and data collection are performed to
the necessary standard
• the piloting campaign must be of sufficient duration (several weeks) to
generate adequate data and care must be taken that steady state
conditions exist for the period of the metal balance

7.5.7.5 Reporting Results


The report on the pilot plant results and metal balance, especially in the case
of proving process economics or project feasibility, must include the following:

• Information on the source and provenance of the feed material


• Information on the scale and throughput rate of the plant
• Information on the methodology used to obtain all data and analyses
and the precision of the results
• A complete metal balance with a full Check in-Check out system
• An accountability for the constituents in the feed of greater than the
agreed minimum percentage as defined in Section 7.5.4
• An assessment of the accuracy of the overall balance

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• A comparison of the repeatability of the various campaigns. A
recommendation as to the factor to be applied to the key parameters of
the results to allow for the inefficiencies of the large scale commercial
plant.

7.6 MINE TO PRODUCT BALANCING AND RECONCILIATION


A common terminology used, especially in the case of precious metals, for assessing
operating performance, is the ‘call’ system, in terms of which the amount of metal
that is produced as final metal, and in the residues or tailings, is compared to the
quantity delivered to the plant in the plant feed. This gives the plant call factor,
which is usually expressed as a percentage, and it is a measure of the
accountability.

In the same way, the measured mass of metal in the ore delivered to the shaft from
the mining operations is compared with the estimated metal content in the ore mined,
as determined by sampling and surveying, to give the shaft (or mine section) call
factor, also expressed as a percentage. The combined plant and shaft call factors
give the mine call factor for the operation. Typically, these call factors are
calculated monthly and they form a useful means of monitoring discrepancies
between the expected and actual mine output.

However, the reconciliation of Metal Accounting back to stopes or ore blocks is


outside the scope of this Code at present.

7.7 MASS BALANCING FOR ENVIRONMENT AND HEALTH MONITORING


The increasing level of public awareness, responsible corporate governance and
emphasis on the triple bottom line has meant an additional focus on this area.

Measurements are required to quantify stack or other emissions to the atmosphere


and the resultant exposure of affected persons, as well as liquid and solid effluents
(including storm water run-off) disposed of in treatment ponds and dams or
discharged into rivers or the sea. The ability to monitor and report on the efficiency
of energy utilisation is also required and the Kyoto Protocol has introduced the
possibility of Carbon Credits for reduced greenhouse gas emissions. Some
companies have adopted an objective of achieving a zero effluent status. The
effective use of scarce water resources and, in some cases adhering to the use of
permitted quantities, is another factor which makes an overall water balance
desirable. All of these aspects may have a monetary value, in terms of penalties or
credits and there may be risks to reputation, as well as legal risks to the company.

For metal balance purposes measurement of streams from operating plants only is
relevant. However, measurement and quantification of any dissolution of heavy
metals and other contaminants from surface dump material, such as, acid mine
(rock) drainage and percolation of critical compounds into aquifers or watercourses,
or gases emitted and dust blown from slag and tailings dumps, is also necessary for
corporate governance. An overall understanding of the balance of these components
is desirable to provide information in order to take corrective action and make
improvements as required in ISO 14001.

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7.7.1 Gases and Dusts
Measurement is often required to provide a mass balance for impurities such as
sulphur, greenhouse gases, nitrous oxides, trace elements and impurities such as
arsenic, selenium and mercury, in order to establish the quantity emitted to the
atmosphere and conformity in terms of the permits and regulations. Measurements
are also required to determine ground level concentrations and the exposure of
employees in the plants, or persons in adjacent areas, to gases or dusts containing
toxic or harmful constituents.

Mass measurement and sampling are normally relatively complex, requiring


specialist equipment and often on-line sampling and analysis. The volumetric flow of
gases and the solids content in the stack or ducting has to be measured and suitable
samples withdrawn (isokinetically), separating solids from the gases for analysis of
both, taking due cognisance of the flow profile in the conduit and the temperature.
Similarly, ground level and personal samplers are required to determine atmospheric
contaminants and employee exposure, separating and collecting solids and gases to
determine mass flow and composition. Methods of measurement, sampling, and
analysis are laid down and specified by organisations such as the EPA, NIOSH,
WHO and other national bodies, as well as in national Air Quality Acts and other
legislation. Companies should adhere to the appropriate regulations and guidelines.
In many cases, companies have adopted international standards for worldwide
application, even where local standards do not exist or are more lenient. Further
assessment of these measurements is outside the scope of this Code at present.

7.7.2 Liquid Effluents


These are normally pumped as slurries in the case of tailings or other residues, or as
solutions, or flow in open drains or channels. Measurement may also be required to
determine the run-off of pollutants (for example dissolved salts such as sulphates,
fluorides or chlorides and metals such as nickel, hexavalent chromium, mercury or
cadmium) from storage facilities or stockpiles through ongoing monitoring, and the
possible contamination of the underground aquifer by the sampling and analysis of
boreholes.

Measurements tend to be more difficult than main process streams and the level of
pollutants and methods of measurement are defined by international agencies as
mentioned above and in relevant national Water Quality Acts and Regulations.
Companies should adhere to these guidelines and/or approved worldwide standards.
Further discussion of the methodology is outside the present scope of the Guidelines.

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8 REPORTING
The Metal Accounting system must generate suitable reports over various time
frames and accounting periods.

The primary purpose of these reports is to:

• provide a metal balance of the desired constituents over the reporting period
(this would normally be monthly, with quarterly or six monthly reports for the
audited company financial reports)
• provide this information promptly to Plant Management and to the Financial
Accountants
• highlight inconsistencies and problem areas in the reported data
• report the level of error in all the reported outputs and their comparison with
target levels
As a secondary objective, the reports should be capable of being used to:

• assist in providing information for diagnosing problems in plant operation,


performance and control on an ongoing basis, for shorter time periods than
those required for financial accounting (weekly or daily)
• assist in predicting plant recovery and outputs for future planning and project
evaluation
• provide information on inaccuracies and inconsistencies in the input data

In order to meet these objectives the reports must:

• be prepared by personnel who are adequately trained and who understand


the source and meaning of the inputs
• make use of data which has been subject to the minimum number of manual
entries /re-entries. Ideally each piece of data should only be entered once or
collected directly from SCADA, LIMS or similar systems
• have used reasonable, determined allowances for error for each of the inputs
that have been generated, by recognised error determination procedures,
where the accuracy and precision of the data have been determined by a
recognised method
• have used an approved procedure to reconcile the mass balance, to identify
inputs subject to illegitimate (spurious) errors, to determine bias, and to
facilitate remedial action if warranted
• provide clear traceability back to the sources of all inputs
• be “cast in stone” and incapable of being adjusted or altered without the
written authorisation of the responsible person. Any authorised alteration
must be logged so that it can be seen by all
• be available to all who should have access, with suitable safeguards to
prevent unauthorised access

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• be as simple as possible and such that it can be adapted to suit changing
circumstances and process flow sheets
• be reviewed and signed off by a metal accounting committee, or other
suitable authority, for subsequent approval by the Audit Committee of the
Board
• comply with International Auditing Standards as set out in IAS 2
• clearly indicate the performance of key indicators such as accountability and
recovery with targeted levels
• give historical comparisons over a suitable longer-term time-frame to enable
long-term trends to be identified.
An important point of custody transfer is the interface between the Mine operations
and the Plant operations. The estimate of the metal delivered by the Mine must be
reconciled with that which the Plant estimates it received. Normally, the receiving
values are accepted but, periodically, adjustments to the plant estimates will be
required when large discrepancies prevail. Therefore, the primary input to the plant
may have to be adjusted, irrespective of its own measurements.

The integrity of home-grown spreadsheets used for metal accounting, which can be
subject to modification by the metal accounting personnel to suit specific reporting
needs, can be a serious concern. The use of such spreadsheets for metal
accounting purposes must be avoided. Various commercial metal accounting
software packages are available and these should be used in preference. Where
home-grown spreadsheets are used, clear rules for setting up such spreadsheets
must be set down, stating that the spreadsheet must be contained in a single file,
with no multiple linked files allowed, and with no incorporation of macros or any other
sub-form of programming. This is to ensure that the system used is uncomplicated
and that it can be serviced and maintained in the absence of the original designer.
The rules must also state that the system must receive original input, which is to be
independently verified, and that it must not receive input via links to any other file or
system, other than data logging systems; this is to ensure that the accounting system
remains uncorrupted by spurious formulae, which may be introduced from other
sources. The rules must further stipulate that no accounting data may be altered
unless the alteration is fully explained and motivated in a written report, which must
also be approved at an appropriate level of authority, defined by the operation
concerned, and retained for record purposes.

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9 SELECTION AND USE OF A COMPETENT PERSON
The Competent Person must have sufficient relevant experience and expertise to
provide sound advice for the definition of realistic objectives in the setting up a metal
accounting system and for the identification of problems in an established system.

The Competent Person must be formally appointed by the management of the


company or operation concerned to undertake the auditing and setting up of metal
accounting reporting systems and must accept full responsibility for the system and
must not treat the procedure merely as a ‘rubber-stamp’ exercise. The letter of
appointment must clearly define the duties and responsibilities of the Competent
Person including:

• Responsibility for final approval of the design of the Metal Accounting system
• Responsibility for auditing the system once it has been installed, to assess
compliance with the design specifications
• Responsibility for periodic reviews and audits of the system, at pre-
determined intervals, to ensure continued compliance and, as required, to
investigate problems which may occur
• Submission of reports to management in regard to the compliance of the
system and monitoring of the action plans produced periodically to remedy
faults
• Independence from the operation concerned.
The Competent Person should not be required for routine metal accounting, or for the
transfer of materials between organisations, but the Competent Person’s services
should be used to ensure that a complete metal accounting system, or a particular
aspect of it, is working as well as can be expected. Often, in metal accounting, one
is in the hands of a few select people and problems occur, which could be material.
It is recommended that an appropriately experienced person is involved to assist in
solving these problems when they do occur. If the solution results in a change in the
metal accounting system, it is essential the change be reviewed and approved by the
Competent Person.

A Competent Person, for the purposes of this Code, must be a member of the
relevant local, professional registration authority or any other statutory local or
international body that is recognised by the relevant Code administrators. If a
complaint is made in respect of the professional work of a Competent Person, the
complaint will be referred to the recognised professional body with which the
Competent Person is registered.

A Competent Person should have a minimum of five years experience relevant to the
type of metal or mineral under consideration and to the type of operation involved.
The key word ‘relevant’ means that it is not always necessary for a person to have
five years experience in each and every type of metal, mineral or metallurgical
operation, in order to act as a Competent Person. For example, a person with twenty
years experience in metal accounting in a variety of base metals extraction and
recovery operations may not require five years specific experience in a precious
metals operation in order to act as a Competent Person. Experience in the other

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operations would count towards the required experience in relation to precious
metals.

In addition to experience in the type of metal or mineral and the operations involved,
a Competent Person assessing metal accounting must have sufficient knowledge of
sampling and analysis techniques, relevant to the metal or mineral under
consideration, in order to be aware of problems that could affect the reliability of the
data. Some appreciation of the mining operation and mineralization applicable to that
deposit type would also be important.

As a general guide, people being called upon to sign as Competent Persons must be
clearly satisfied in their own minds that they can face their peers and demonstrate
competence in the commodity, type of operation and situation under consideration.

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10 DESIGN OF METAL ACCOUNTING SYSTEMS
Metal accounting data is generated primarily for management information purposes
and not for financial reporting requirements. However, the outputs of the metal
accounting system do feed into the company’s financial reports and, as such, the
system must be transparent and associated with a clearly defined audit trail. The
design of the accounting system should form part of the design scope for new plants
and it should include careful identification of the mass measurement and sampling
points required to enable a reliable metal balance to be determined. It should also
include careful attention to the detail of the installation, calibration, maintenance and
routine operation of the relevant equipment. The design of the metal accounting
system, however, must not be left as an afterthought, to be incorporated at a late
stage in the final plant design specification. Changes to the design, to accommodate
metal accounting equipment at this point, are costly and could lead to compromises
in the installation of the equipment, which, in turn, could have a negative effect on
their operability and long-term reliability.

Incorporation of the metal accounting system in the plant design specification


requires the involvement of the plant operating personnel during the design of the
system. This involvement, together with thorough education and training of the
operating personnel in the theory and practice of the accounting system, are
essential for the successful implementation and operation of the system and for the
acceptance, by the operating staff, of the system’s principles and procedures.

The specification of the metal accounting system should comply with this Code and it
should include a clear set of objectives, including:

• A system for data acquisition and management


• Reporting intervals, dates and timing
• Samples, sampling frequency, sample preparation procedures and analyses
required, as well as cross-reference to the required analytical procedures and
target accuracies
• Mass measurement points, types of measuring devices and the required
accuracy
• Reporting rules and procedures for all outputs from the accounting system
• Levels of authority for approval of the data and, where necessary, for
handling and approving changes to the data
• Accounting battery limits
• Stock-take procedures and frequencies
The major objectives of a metal accounting system are to ensure that:

• the production of the metal balance is timely in terms of required operational


decisions, in addition to its basic requirement to contribute to financial
reporting
• the financial risk associated with the metal accounting system can be
quantified and managed

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• the entire system is transparent, with a clear audit trail and well-documented
standard procedures, in line with international or local standards, to cover
mass measurement, sampling, sample preparation, and analysis
• the system incorporates the necessary and appropriate checking and
statistical analysis procedures to enable biases in mass measurement,
sampling and analysis to be quantified
• the system is audited by a team of suitably qualified persons (both internal
and external to the company) at a pre-determined frequency
• clear levels of authority and clear procedures are set down for handling the
metal accounting data and making any adjustments to the data
• battery limits of all operations covered by the system are clearly identified and
that clear accounting procedures are laid down and the appropriate sampling
and mass measurement facilities required clearly specified
The design of a metal accounting system should cater primarily for the needs of the
accounting process. Data collection and handling must be thought through during
the design stage and reporting requirements should form part of the system
specification. Where the metal accounting data is required for other purposes, such
as forecasting or project evaluation, for example, access to and use of the data
should be controlled and limited to designated persons. The system output, however,
should be user friendly and should be able to be easily incorporated into other
company management systems, such as financial reports.

The key stages in data management are to:

• agree the performance indicators required for the Metal Accounting System
• decide what data needs to be collected to measure performance against each
indicator
• look at the possible sources of data related to each indicator
• decide who has responsibility for collecting what data
• establish a clear timetable for data collection, so that everyone knows what
they should do and when they should do it
• standardise data collection so that everyone gathers and reports data in the
same way
• agree the appropriate metal balancing procedures, protocols and algorithms
• train and support the data collectors so that they are competent and confident
• check or verify the data that is collected
• set up appropriate and timely communication or reporting systems
• determine the accuracy limits of the data
• analyse the data to support self-assessment and continuous improvement
• evaluate performance using the data

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Battery limits should be specified to meet the needs of the metal accounting system
and they should focus on the inputs to and the outputs from the specified process
system. Measurements of internal transfers and recycle loops, within the battery
limits, are usually required to meet specific company management or control
purposes and they are secondary to the metal accounting goals. As such, they
should be accommodated within the metal accounting system as far as possible, but
the system itself should not be compromised to provide for these secondary outputs.
Design of the mass measurement and sampling systems should comply with the
needs of the metal accounting system, as defined by the battery limits. The level of
accuracy and sophistication incorporated into the design should also reflect the value
of the material being measured or sampled, as well as the risk to the operation in
terms of both financial loss and damage to the company’s reputation caused by
erroneous accounting.

Measurement points, whether of mass or metal content by sampling and analysis,


should provide sufficient, redundant data to allow the metal accounting balance to be
crosschecked, optimised and reconciled. The rules and procedures required for this
optimising and reconciliation process must be clearly defined as part of the metal
accounting system.

Several commercial metal accounting software packages for the compilation of metal
accounting data, using a central database, are available. These packages are
usually designed to be user-friendly, requiring minimal training of metal accounting
personnel, and they are considered preferable to the use of spreadsheets developed
in-house, as these can easily be corrupted and they are seldom adequately
documented. However, manual entry of data to operator log sheets and
transposition to spreadsheets is common practice on some plants. Spreadsheets do
not allow for controlled data entry; it is easy to inadvertently type over data, lose track
of records, duplicate and improperly enter data in a spreadsheet. Further to this, the
justification of formulae in spreadsheets often lacks clarity, and the justification is not
always recorded with the spreadsheet and it can get lost, especially if the developer
of the spreadsheet moves on, thereby making spreadsheets vulnerable to error and
unjustified computations. For these reasons, spreadsheets must be avoided as a
method of data entry.

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11 METAL ACCOUNTING AUDITING RULES

11.1 INTRODUCTION
A company must have metal accounting rules and a procedure for auditing these.
These rules are primarily technical to provide management information and to
promote good corporate governance but they must also provide the quantities and
the reconciliation necessary for the financial reports. A set of “Check Lists” is given in
Appendix D, which can form the basis of inspections and audits.

11.2 AUDIT TEAM AND ITS RESPONSIBILITIES


A team to audit the metal accounting system must be established and it must include
a financial auditor. Periodically, the team must include a Competent Person who
could be a member of the Company Head Office Internal Audit team, but preferably
should be an outsider with no connection to the company.

The team’s objective is to obtain a fair and soundly based analysis of an existing
metal balancing and reconciliation operation and to report its findings as appropriate.
A minimum of an annual stock-take is preferred, both to confirm the base line figures
and to lend credibility to the metal accounts.

The team will:

• witness stock-takes
• verify the mass flow measurements and analytical results
• assess compliance of mass flow, sampling, sample preparation and analytical
procedures.
In addition, an assessment of the accuracy, precision and reconciliation of metal
accounting figures is required. To this end, an audit trail, with clear supporting
documentation, is essential. Reporting should be done to suit the company’s
reporting period, in compliance with international practice and stock exchange
requirements, as applicable. The inclusion of an annual stock-take as part of the
report is recommended.

The use of a Competent Person to sign off the metal accounts is seen as an issue
relating to sound corporate governance, while other critical issues are transparency,
credibility and full disclosure.

The audit must identify and advise on areas that are inadequate and the
recommended actions required to achieve satisfactory performance.

It is essential that the Competent Person conducting the audit should have an
adequate support structure. It should not be necessary for the Competent Person to
sign off the metal accounts every year, but there must be an independent audit of the
metal accounting procedures by a Competent Person at least every three years.

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11.3 METAL ACCOUNTING REVIEW
On at least an annual basis, the metal accounting system methodology must be
reviewed by a team of suitably experienced staff, to ensure that it is still fulfilling its
requirements. The review should draw information from a number of sources,
including:

• Results from internal audits


• External assessments
• Internal quality control studies
• Any ongoing biases indicated in any of the measurements.
Should this review lead to recommendations for changes to the existing system,
these must be approved by a Competent Person, prior to incorporation in the system.

11.4 PHYSICAL AUDITS


A series of physical audits must be implemented to ensure that all aspects of the
metal accounting chain are operating as specified. It is preferable that pre-designed
hard-copy checklists for each operation are followed to ensure that the audits are
consistent and that they are retained as a record.

The recommendations given in the Australian Standard AS 4433.6 should be


followed and they can be easily adapted to apply to mass measurement devices as
well.

For laboratories, the recommendations given in the CITAC/EUROCHEM Guide CG1


must be carried out at least bi-annually.

Obviously, the auditing of problem areas must be scheduled at a frequency to enable


the problem to be positively identified and eliminated in as short a time period as
possible.

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GLOSSARY
Acceptance Test – A test carried out on a new conveyor weigher installation in order
to determine whether the error is within the specified tolerance.

Accountability – The comparison of the total output of a plant, or section of a plant,


to its total input, normally expressed as a percentage.

Accounting Period – The period in which a company would normally report its
financial results to the market. For example in the USA this is quarterly, while in
many other financial markets the requirement is bi-annually. In metal accounting,
however, the accounting period is usually one month, but metal accounting reports
also have to be prepared to cover the company’s financial accounting period.

Accounting Standards – The financial accounting standards required by the


relevant regulatory authorities including Stock Exchanges.

Accreditation – Procedure by which an authoritative body gives formal recognition


that a body or person is competent to carry out specific tasks.

Accuracy – A measurement is accurate if it, or the average of a number of


measurements, is close to the true value. In metallurgical operations this true value
is unknown. In addition, there is often misunderstanding between the terms accuracy
and precision, which is the measure of the spread of a number of measurements
around their mean value. For these reasons, it has been decided to adopt the
following definition for accuracy, which incorporates the concept of precision, and is
based on that given in ISO 5725-1:1994.

A measurement that is accurate is one that is free of bias and has a dispersion
(standard deviation) that is lower than a defined dispersion or indeed a probability
density of a particular nature. The level of dispersion or the nature of the probability
density is defined with the purpose of separating measurements that are entirely fit
for a particular purpose or use and those that are not.

Acid Mine (Rock) Drainage – The low pH effluent which seeps from waste rock, ore
dumps or stockpiles of materials which have an insufficient capacity to neutralise the
acidic products, containing the dissolution products of minerals.

Actual Recovery – The sum of all useful or desired outputs from a process, divided
by the sum of all inputs to that process, expressed as a percentage.

Adjustments – The changes which are applied to each measurand to achieve a


mathematically exact balance, that is a balance where all of the balance flow sheet
constraints are satisfied and total and component masses are consistent across the
complete balance.

Analysis Depth – Is the maximum depth in a sample, such as a pressed pellet, from
which the fluorescent X-rays of an element can leave the sample.

Analyte – The component of a material whose concentration is determined by


chemical analysis.

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Audit Trails – In metal accounting, an audit trail is a sequence of paperwork/data
entries that validates or invalidates metal accounting entries. Many metal accounting
entries are based on those made to computers, and the term could also be used for
an electronic or paper log used to track computer activity.

Auditability – A user-oriented quality requirement specifying the degree to which an


application shall keep sufficient records to support a financial or technical audit.

Auger Sampler – A tubular device containing an Archimedean screw which when


driven through material in a container retains a representative portion of that material.

Auger Sampling – An increment is collected from, usually, a relatively fine and dry
particulate material using a correctly designed auger sampler.

Back-up Systems – Systems for copying or saving metal accounting data to a


different location so that one can restore the back-up copy if data is lost or damaged.

Barren Solution (Tails Solution) – The discard solution from a metal recovery
process.

Battery Limits – The boundaries of a metal accounting system, across which all
inputs to and outputs from that system are measured and balanced.

Belt Scale/Weigher – A mass measurement device that continuously integrates and


records as a cumulative mass, the load on a belt while it passes the suspended scale
or measuring section of the belt.

Belt travel speed – The average speed of a conveyor belt, which is used in
conjunction with the weigher, to calculate the tonnage of material conveyed over a
period of time.

Belt-speed sensor – A device that generates a signal as a result of the belt speed.

Bench Scale Plant – Equipment used to perform tests in a laboratory on a relatively


small scale, on a stage in a process or the entire process in order to establish the
parameters and performance of the process.

Berm – An elongated earthen structure which acts as a barrier to contain or redirect


the flow of water or solution.

Best Practical Means – The most precise method of performing a measurement


taking into account the risk, degree of importance, cost and practicality for the stream
and variable being measured.

Best Practices – The most precise method of performing a measurement with the
information and equipment available at that time.

Bias – Bias is the difference between the mean result of one or more measurements
and the true value of the quantity being measured. It also can be seen as an
ongoing difference between two, or more, measuring systems. (e.g. sender’s and
receiver’s weights, the analysis of the same sample by two laboratories etc.)

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Bin Scale – A bin that is fitted with load sensors or other mass detecting devices,
which has been calibrated so that the weight of the contents can be established and
weighed on a continuous or batch basis.

Bubble Method – A method whereby the flow of material through a process plant is
interrupted to allow for equipment to be emptied in series to facilitate stock-takes
(normally applied to high value materials in the latter stages of processing).

Built-up Recovery – The sum of all useful or desired outputs from a process,
divided by the sum of all outputs from that process, expressed as a percentage.

Bulk Density – The density of a granular material normally stored in a bin, other
container or stockpile, defined as the mass of the material divided by the volume
occupied by the material (including the space between the particles).

By-products – A metal/commodity made during the manufacture of another. They


are incidental to the production of the common products and often contribute a
relatively small value to the process revenue.

Calibration Test (flow meters) – A set of operations which establish, under


specified conditions, the relationship between values of quantities indicated by a flow
meter and the corresponding values indicated by a standard of reference.

Calibration Test (weighers) – A test, using known weights and forces to load a
scale, in order to determine the performance and operating tolerance compared to
standard values.

Carbon Credits – The process of trading (buying or selling), between countries,


operations or companies, an achieved reduction in the emission of green house
gases (GHG) such as carbon dioxide, through the mechanisms established for that
purpose as a result of the Kyoto Protocol.

Certification (Test) – A calibration of a scale or flow meter in terms of accepted


standards defined by the relevant government authority to permit its use for trade
purposes and custody transfer.

Certified Reference Material (CRM) – Reference material, accompanied by a


certificate, one or more of whose property values are certified by a procedure, which
establishes its traceability to an accurate realisation of the units in which the property
values are expressed, and for which each certified value is accompanied by an
uncertainty at a stated level of confidence.

Certified Weight – A weight, which has been certified by the relevant national body,
or an agent authorised by that body, to have a mass within a defined tolerance, to be
used for certifying weighing instruments.

Check in-Check out System – The system whereby all streams into and out of the
Process or Plant, for which the balance is being performed, are measured, sampled
and analysed.

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Closure Errors – The difference between the inputs and outputs for a complete
metal balance (that is Check In-Check Out) over a plant or process, including
inventory and stock changes, over a prescribed period, and zero.

Coefficient of Variation – The quotient of the standard deviation and the mean
value of a measurement, expressed as a percentage.

Combined Standard Uncertainty – The result of the combination of standard


uncertainty components.

Common Product – Metals or commodities produced in large quantities, which


make a material contribution to process revenue.

Competent Person – A person with suitable qualifications and experience to


undertake a review of the design and the performance of the Metal Accounting
system and Balance.

Concentrate – Term used for the product from a mineral processing operation such
as gravity separation or flotation in which the valuable constituents have been
upgraded and a large proportion of the gangue material discarded in the tailings.

Concentration Ratio – The ratio of the tonnes of ore in the feed to the tonnes
produced as concentrate.

Consistency Errors – A set of samples, providing an estimate of the value of a


parameter, is said to be consistent if, as the number of samples increases, the
limiting value of the estimate is the true value of the parameter in question.

Constraint – In a mathematical expression or model, a constraint (restriction) occurs


for every parameter in that model or expression, which has to be estimated from
observed data. (See also Degrees of Freedom).

Coriolis Mass Flow Meter – A device, consisting of a flow sensor and a transmitter,
which primarily measures the mass flow by means of the interaction between a
flowing fluid and the oscillation of a tube or tubes; it may also provide measurements
of the density and the process temperature of the fluid.

Corporate Governance – Corporate governance is concerned with holding the


balance between economic and social goals and between individual and communal
goals. The corporate governance framework is there to encourage the efficient use
of resources and equally to require accountability for the stewardship of those
resources. The aim is to align as nearly as possible the interests of individuals,
corporations and society.

Coupled In-Motion Weighing – The weighing in-motion of a train of coupled


wagons to obtain a weight indication or print out of the individual wagons.

Coverage Factor – A number that, when multiplied by the combined standard


uncertainty, produces an interval (the expanded uncertainty) about the
measurement result that may be expected to encompass a large, specified fraction
(e.g. 95%) of the distribution of values that could be reasonably attributed to the
measurand.
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Cross-Stream Sampler – A mechanical sampling device that is used to collect an
increment from a falling stream of material either from a conveyor of particulate
material or from a slurry stream.

Custody Transfer – The transfer of risk and/or ownership of a material from one
party to another. This includes ore from a mine to a processing plant, intermediate
products such as concentrate and matte from one plant to another, both in-house
and inter-company and waste products for sale or safe disposal, as well as final
products.

CUSUM Graphs – CUSUM (Cumulative Sum) graphs are constructed by plotting the
cumulative difference between the measurand and its accepted value.
Measurements are “In control” if the plotted line meanders around the zero difference
line. Plotted lines that deviate from the zero difference line are an indication of bias.

Data – In a metal balancing context is almost always a numerical measurement.


(See also Smoothing)

Degrees of Freedom – The number of degrees of freedom of a statistic is defined as


the number of independent observations in the sample (i.e. the sample size) minus
the number of population parameters, which must be estimated from those sample
observations.

Demonstration Plant – A small-scale plant (but orders of magnitude larger than a


pilot plant) designed to test and prove a process and equipment, through a series of
stages on a continuous basis, on specific feed materials.

Differential Pressure – The difference between the static pressures measured at


the wall pressure tappings, one of which is on the upstream side and the other on the
downstream side (or in the throat for a Venturi tube) of a primary device inserted in a
straight pipe through which flow occurs, when any difference in height between the
upstream and downstream tappings has been taken into account.

Division – The process of decreasing sample mass (without modification of the


particle size of the constituent pieces) whereby one or more representative parts of
the sample are retained. (AS 4433.2 – 1997)

Draught Survey – A mass measurement technique that is based on converting a


difference between a vessel’s displacement under different loads into a mass on the
basis of its draught tables while taking into account the density and temperature of
the water and ballast, and changes in ballast and supplies.

Dump Leaching – Normally refers to a process whereby metals are extracted by


"heaping" uncrushed/broken Run of Mine ore on sloping impermeable pads (with
suitable low cost drainage of the leach solutions) and spraying the heaps with a
lixiviant, which dissolves the metal content. Sometimes the process is carried out
utilising low-grade ore which was previously stockpiled, as treatment through the
normal process route was uneconomic. Often the lixiviant used is the barren solution
from other primary leach operations. The metal-laden solution is collected for metal
recovery.

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Durability error – The difference between the intrinsic error over a period of use
and the initial intrinsic error of an instrument.

Electromagnetic Flow Meter – A flow meter, which creates a magnetic field


perpendicular to the flow, thus enabling the flow rate to be deduced from the induced
electromotive force produced by the motion of a conducting fluid in the magnetic field.

Electromechanical Belt Scale/Weigher – A mass measurement device whereby a


loaded belt is continuously weighed by mechanical means (load cells, levers) and the
measurement converted into an electronic signal that can be integrated (totalised)
and recorded.

Enrichment Ratio – The ratio of the metal grade in the concentrate to the metal
grade in the feed.

Equiprobable Opportunity – The requirement that every particle in a process


stream has an equal opportunity of being collected as part of a sample.

Error of Measurement – The result of a measurement minus the value of the


measurand (not precisely quantifiable because the true value lies somewhere
unknown within the range of uncertainty).

Estimated Recovery – Where redundant data are available, the estimated recovery
will depend on which measurement points are chosen as the basis of the calculation.
For example, the mass and grade of the saleable product is usually accepted as the
value agreed as part of a commercial transaction. If the mass and grade of the feed
to the process are known from measurement and sampling, an “input recovery” may
be calculated.

Evaluation – The process by which the data required for Metal Accounting is
acquired.

Exception Report – A report generated, in terms of this Code, whereby each non-
compliance with the requirements of this Code is motivated and approved.

Expanded Uncertainty – Obtained by multiplying the combined standard


uncertainty by a coverage factor.

Flexible Hose Sampler – A sampler where the material to be sampled is confined


within a hose which can be mechanically moved across a stationary sample cutter.

Gamma Belt Weighers – See Nuclear Belt Weigher.

Gantry scale – A scale where the load measuring elements are attached to a gantry
crane normally used for loading or offloading materials in bulk.

Hazops (Hazard and Operability Studies) - A process conducted during process


design in which the plant design is reviewed to eliminate or reduce hazards and
reduce operating difficulties.

Heap Leaching – Normally refers to the leaching of ores that have been crushed (to
an economic size) prior to placement on an impermeable pad on which suitable

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drainage lines have been placed for the collection of lixiviant that has been
percolated through the crushed and prepared ore. The crush size selected may vary
considerably but typically ranges between 12 and 50 mm.

Home and Away System (Double Sampling and Analysis) – A system where
batches/lots are weighed and sampled by both the sender and receiver. Data from
the analysis of the samples can then be statistically analysed to establish the
presence of biases in the sampling and/or analytical processes. In the “Half Home
and Away System” samples from even numbered batches of material are analysed
by the sampling sites laboratory (i.e. sender at sender’s laboratory and receiver at
receiver’s laboratory) and odd numbered batches are analysed at the other
laboratory (i.e. sender at receiver’s laboratory and receiver at sender’s laboratory).
Statistical analysis of the data can then establish the level of bias in either the
sampling or analytical procedures.

Hopper Scale – A scale designed for the weighing of granular materials in bulk,
whose load-receiving element is a self-cleaning hopper with an outlet gate.

Increment – A quantity of material collected in a single operation of a sampling


device. (AS 4433.2 – 1997)

Initial intrinsic error – The intrinsic error of an instrument as determined prior to


performance tests and durability evaluations.

In-motion weighing – The weighing of objects that are in-motion. Usually applied to
rail or road trucks.

In-process Inventory – The quantity of material contained in a process plant


through the various stages from the initial feed to the plant to the production of
product(s) from the plant. It does not include stocks of feed material or products
which are defined as Plant Stocks.

In-situ Leaching – A process whereby the metal contained in an ore body is leached
in-situ by pumping a lixiviant into the ore, which is normally naturally fractured or has
been broken by explosives and the pregnant solution withdrawn

Inter-leaved Experiments – To carry out interleaved sampling, a sampling system


must be capable of taking increments at twice the usual rate. Odd-numbered
increments are collected into one sample and the even-numbered ones are collected
into a second sample over the sampling period of interest. Both samples are, at the
end of the sampling period, nominally identical. If they are both separately prepared
and analysed in the same way, the difference between the results in an indication of
the precision of sampling. A substantial number of results from interleaved pairs of
samples can be accumulated over a period of time to arrive at a good estimate of the
average sampling precision. It is also possible to draw certain conclusions regarding
the distribution of the assay uncertainties.

Internal Working Reference Material (IWRM) – A carefully prepared, homogeneous


material whose assigned values have been obtained from a round-robin exercise
using accredited methods of analysis and by comparison to CRMs.

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International Unit of Mass – This is defined as the kilogram. The definitive
standard weight is held at the International Bureau of Weights and Measures in
France, which is also responsible for certifying National standards such as the
National Prototype Kilogram.

Intrinsic error – The error of an instrument under reference conditions.

Isokinetic Sampling – A sampling method, normally used for gas streams


containing dust, or effluent streams containing solids, whereby the sample is
withdrawn from a conduit, duct or stack in a manner that withdraws the sample
across the diameter of the conduit, so in such a way that there is no change in the
velocity of the sample stream as it enters the sampler. Also used for personal
sampling of ambient air.

K Factor (Belt Weighers) – The ratio of the result of the mass determined by a bulk
test, arrived at by passing a known weight of material over the weigher, as compared
to that obtained by the use of test weights.

Kyoto Protocol – A Protocol arising from the meeting of 160 nations, in terms of the
International Convention for Climate Change, which took place in Kyoto, Japan in
1997, whereby signatory countries agreed to reduce the emission of greenhouse
gases by certain percentages, relative to levels pertaining in 1990 during the period
2008 - 2012. It came into force on the 16th February 2005.

Level of Confidence – The probability that the value of the measurand lies within
the quoted range of uncertainty.

LIMS – Acronym for Laboratory Information Management System, a computer


system for gathering and analysing laboratory information. These systems are used
for:

• Automatic data collection. The LIMS may be interfaced directly to the


laboratory instruments, offering rapid data collection, while eliminating the risk
of transcription errors.
• Provision of electronic records of laboratory results. Electronic records
offer many benefits, such as the ability to link data together, search, retrieve
and report rapidly and backup and disseminate data easily through an
operation.
• Provision of a structured repository for laboratory data
Lixiviant – A solution containing acids, other chemicals, or bacteria used to dissolve
metals or metal compounds.

Load Cell (Sensor) – A device which produces an output signal proportional to the
applied weight or load. The load cell may utilise any physical principle included in the
field of, but not limited to, electricity, electronics, hydraulics, magnetics, mechanics
and pneumatics or combinations thereof.

Lot – A lot is a defined quantity of the material being measured to which the mass
and analysis is applicable. It may be a shipment, a production batch or production
over a defined time period, such as a shift or a day, or a fixed tonnage of material.

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For accounting purposes, a weighted average sample of all the production or
shipment batches making up that lot is prepared and submitted for analysis.

Lot/Batch – A certain quantity of material for determination of its average quality.


(See also Lot in the Glossary)

Mass Balancing – The process whereby input and process streams, or the
individual components of the streams, stocks and in-process inventory are
measured, sampled and analysed in order to calculate the mass of each and
reconcile the output to the input, plus or minus the stock change.

Materiality – It is what affects business decisions at the top level of management. It


is not a formally defined value but should be determined by senior management for
each company and/or operation. For metal accounting, a measurement for a
process flow or in-process inventory may be regarded as material if:

• The metal content is significant in value and/or


• The content is regarded as important with respect to the company’s or
operation’s risk profile, public perceptions or reputation and/or
• It will reflect on the balance sheet and financial statements
Material-run (bulk) Test – A method of calibrating a belt scale whereby a known
weight of the material (either pre or post weighed on a test scale) being weighed is
passed on the conveyor through the mass detection system.

Mathematically Exact Balance – A mathematically exact balance means a balance


where all of the balance flowsheet constraints are satisfied and total and component
masses are consistent across the complete balance with no unaccounted losses or
gains.

Matte – The upgraded product from a smelting furnace or converting operation for
sulphidic ores or concentrates which contains the majority of the metal values and a
lower proportion of gangue materials (a large proportion of which have been removed
in the slag). Furnace (green) matte still contains a high proportion of iron whilst in
converter (white) matte the iron content is much lower and the value metals higher.

Maximum Permissible Tolerance (Error) – The maximum difference, positive or


negative, permitted between the indication of an instrument and the corresponding
true value, as determined by verification standard masses, with the instrument being
at zero at no-load, in the reference position.

Mean (of data) – The mean of a set of n items of data is the arithmetic average of
the series of measurements xi. The mean is usually designated by x with a bar
above it.

Measurand – The specific quantity subject to measurement.

Mechanically Correct Sampling – Correct sampling of a particulate material from a


moving stream is achieved when the expected number fraction of the particles in the
sample is equal to the average number fraction of the particles in the process stream
during the time that it takes to extract the sample increment. To achieve this

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objective, the sampler must be correctly designed, installed, maintained and
operated. A sampler that is mechanically correct is unbiased. Where possible, the
correctness of the sampler and its freedom from a specified level of bias should be
confirmed by carrying out bias tests by the stopped belt method or other suitable
reference method of sampling.

Metadata – The term used to describe data about data. It describes who collects the
data, what the data contains, where (and how) the data is stored, when (and how
often), and why the data is collected,

Metal Accounting – The system whereby selected process data (pertaining to


metals of economic interest) is collected from various sources including mass
measurement and analysis and transformed into a coherent report format that is
delivered in a timely fashion in order to meet specified reporting requirements.

Metallurgical (Metal) Balance – The determination through measurement, analysis


and computation of the magnitude of each component of interest within each section
of a process flow sheet. A metallurgical balance is commonly referred to as a “metal
balance” or as a “metbalance”. The latter is preferred as the process is applicable to
any mineral based commodity – it is not restricted to metallic elements. A
metallurgical balance, which is suitable for reporting of metallurgical performance,
should be supplemented by defined errors associated with each determination.

Metrology – The science of Weights and Measures.

Microwave Gauge – An instrument that utilises microwaves to measure the moisture


content associated with a material.

Mine Call Factor – The ratio, expressed as a percentage, which the specific product
accounted for in the product recovered, plus that in tailings/residues, bears to the
corresponding product called for by the mine’s measuring and evaluation methods. It
is also the product of the Shaft and Plant Call Factors.

Momentum Mass Flow Meter (Impact Mass Flow Meter) – A device that detects
mass flow rate by measuring the momentum of a stream of material falling a definite
distance under gravity.

National Prototype Kilogram – The standard certified weight which is held by


individual countries and which has been certified by the International Bureau of
Weights and Measures. This standard weight is used to certify, by the national
Metrology organisation, the test weights used to certify all weighing equipment.

Neutron Gauge – A nuclear gauge that utilises an emission of neutrons to effect the
measurement.

Nominal Top Size – The mesh size that will allow 95% of the sample to pass
through.

Nomograph – A graphical presentation of related sets of data enabling specific


experimental conditions to be pre-determined, such as in the use of Sampling
Safety Line.

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Normal Distribution – A continuous distribution of a random variable, with mean µ
2
and variance σ and probability density:

1 ⎛ ( x - µ )2 ⎞
p(x) = exp ⎜ - ⎟
2πσ ⎜ 2σ 2 ⎟
⎝ ⎠

Nuclear Belt Scale/Weigher – A mass measurement device that continuously


integrates and records as a cumulative mass the load on a belt while it passes the
nuclear source by measuring the absorption of the gamma rays by the material on
the belt.

Nuclear Gauge – An instrument that emits a source of neutrons or radiation (usually


gamma rays) which pass through the material in a conduit, on a belt, or in a stockpile
or bin, and has a receptor that collects the radiation on the other side, thus enabling
a measurement of the adsorption and hence the moisture content or density of the
material.

P & ID – Process and Instrumentation Diagram.

Paired t-test – A single sample t-test appropriate for comparing two samples in
which individual are paired, and observed values within pairs are positively correlated.

Penetrometer – An instrument that measures in-situ density by measuring the


backpressure resulting from the penetration of a cone into the material being
measured. Usually applied to soils but is also utilised for stockpiles of material such
as coal of a relatively fine uniform size.

Permanent Inventory – In-process Inventory that has been absorbed into the
fabric of the processing plant, such as gold into concrete foundations, which is only
recovered when the plant is demolished at the end of it’s life.

PFD – Process Flow Diagram.

PGMs – Platinum Group Metals comprising of platinum, palladium, rhodium, iridium,


ruthenium and osmium.

Photogrammetry – The process of producing 3-D images by multiple photographs


of an object.

Pilot Plant – A small-scale plant to test a process or process stages on a specific


process, on a continuous basis.

Plant Call Factor – The mass of a species recovered to product and to tailings
divided by the mass of species fed to the plant, expressed as a percentage.

Plant Historian – A computer system for accurate operational data archiving and its
rapid recovery. The data historian accepts data input only, does not recognise
structures and procedures, and is strictly concerned with the accurate, efficient data
storage and recovery if required. Data historians perform three key functions:

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• Data compression
• Rapid data recovery
• Data save-set facility
Plant Inventory – The inventory can be stockpiles of feed, intermediates or products
(plant stocks) as well as transient and long-term in-process inventory.

Plant Recovery – The quantity of metal in the product stream from a plant, divided
by the quantity of metal in the feed to that plant, expressed as a percentage.

Plant Stocks – Any material received by a plant, from a previous processing


operation, but which has not yet entered a process stream, or any material produced
by that plant to dispatch standard quality, but which has not yet been dispatched.

Platform Scale – A compound lever scale whose load receiving element is a


platform that is supported by four or (rarely) more main bearings.

Precision – Of a measurement depends on the closeness of the outcomes of a


repeated measurement or test procedure. Hence it depends only on the distribution
of random errors and not on any relationship to a “true” value. It is usually expressed
as the standard deviation of the test results. That is, by a measure of imprecision.

Precise measurements have a dispersion about their mean value, which is lower
than a defined dispersion or indeed a probability density of a particular nature. The
level of dispersion or the nature of the probability density is defined with the purpose
of separating measurements that are entirely fit for a particular purpose or use and
those that are not. A precise measurement may not be accurate; its mean may differ
from the true value of the measured quantity by an arbitrary amount. Standards
often quantify the term precision as a value corresponding to the magnitude of a 95%
confidence interval around a result. If the n measurements of the quantity to be
estimated are normally distributed, the interval is ± ts, where t is the two-sided
Student-t value at 95% confidence and n-1 degrees of freedom and s is the estimate
of the standard deviation of the estimated quantity.

Pregnant Solution – A solution containing dissolved metals, (e.g. from a leaching


operation) which is normally the feed to further processing to extract the product
metals.

Primary Accounting – The metal balance across an entire plant as determined by


Check in-Check out.

Propagated Error – The error in succeeding steps of a process due to the


occurrence of an earlier error.

Quality – Degree to which a set of inherent characteristics fulfils requirements.

Quality Assurance (QA) – QA describes the overall measures that a laboratory


uses to ensure the quality of its operations.

Quality Control (QC) – The operational techniques and activities that are used to
fulfil the requirements for quality.

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Random Error – The component of the error of measurement, which in the course of
a number of measurements of the same measurand, varies in an unpredictable way.

Random Stratified Sampling – The taking of increments whereby the material being
sampled is divided into strata, one increment being taken at random within each
stratum. (AS 4433.1 – 1997)

Reconciliation – A metallurgical balance which relates production of saleable and


reject or waste materials from a process back to its source as ore or other feed
material. It should be provided with defined and stated errors as for any other
metallurgical balance.

Reconstitution – If the mass and grade of the process rejects are known from
measurement and sampling, then an estimate of the feed to the process can be
made by adding together product and waste. A recovery based on this calculation is
often referred to as an output recovery. Given that all measurements (mass,
sampling and analysis) are subject to random errors (and possibly biases) the
numerical values of input and output recovery are not expected to be equal although
they should agree to within the errors of measurement imposed on each calculation
process. That is, they may be statistically identical.

Recoverable Metal – The proportion of a metal in a feed material that has been
determined to be recoverable, by laboratory and/or pilot plant tests, by the chosen
process, with the remaining metal being defined as Non Recoverable.

Recovery – Of a particular component is defined as the proportion of that component


in the feed source, which is estimated to have reported to each process stream but
most commonly to the saleable product. Hence, recovery is a measure of
performance efficiency and is always a key performance indicator.

Reduction – The process of decreasing the dimension of pieces constituting the


sample, without modification of mass of the sample or of its composition. (AS 4433.2
– 1997)

Reference Material (RM) – Material or substance one or more of whose property


values are sufficiently homogeneous and well established to be used for the
calibration of an apparatus, the assessment of a measurement method, or for
assigning values to a material.

Relative Density – The relative density of a substance is the ratio of the density of
the substance at a specified temperature to the density of a reference substance at
the same or a specified different temperature (usually the reference substance is
water at a temperature of 4 ºC). Relative density is a dimensionless quantity and is
also referred to as specific gravity.

Relative Standard Deviation – Relative standard deviation is the standard deviation


of a measurement, normally expressed as a percentage of the mean of that
measurement.

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Repeatability – Repeatability is a measure of the extent to which measurements
made in the same laboratory with the same instrument will be similar. Australian
Standards define the repeatability of a measurement as the maximum acceptable
difference between duplicate determinations carried out in the same laboratory on
the same sample. If the absolute value of the difference between the two
determinations exceeds the repeatability, the duplicate assay must be carried out
again.

Repeatability of a measuring instrument is the quantity that characterises the ability


of the measuring instrument to give identical indications or responses for repeated
applications of the same value of the quantity measured under stated conditions of
use.

Repeatability of a measurement is a quantitative expression of the closeness of


agreement between successive measurements of the same value of the same
quantity carried out by the same method with the same measuring instrument at the
same location at appropriately short intervals of time.

Repeatability (in Mass Measurement) – The capability of producing anew a


previous indication when the previously applied loads or forces are again applied.

Representative – A sample can be said to be representative of the lot from which it


was taken if the mean square of the total sampling accuracy (uncertainty) is less than
some standard of representativeness. The accuracy includes both the bias and the
precision and its mean square has the expected value of σ2 + b2, where σ if the
standard deviation characterising the precision and b is the bias. The standard of
representativeness is a value chosen by the user to suit the circumstances and the
use to which the numbers are to be put.
Reproducibility – Reproducibility is a measure of the extent to which measurements
made in different laboratories will be similar. Australian Standards define the
reproducibility of a measurement as the maximum acceptable difference between the
mean of duplicate determinations carried out in one laboratory and the mean of
duplicate determinations carried out in a second laboratory on representative
samples taken from the same bulk sample, after the last stage of the reduction
process.

Reproducibility (in Mass Measurement) – The measure of the extent that weights
determined by two different instruments or methods will be similar.

Restore Methods – Methods for the restoration of electronic data or stored


documents from back-up media at the same or an alternate location, normally only
required in the event of a disaster.

Risk – The chance of an event occurring that will have an impact on objectives. A
risk may be quantifiable in terms of the likelihood of loss, less than expected returns
or an undesirable outcome. (The VALMIN Code, 2005 Edition).

Risk Assessment – A formal process for the identification and quantification of the
risks associated with the all the processes involved in metal accounting.

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Round Robin (Proficiency Testing) – An exercise where sub-samples of the same
material are circulated to a number of laboratories for analysis. The results are used
to establish an accepted value for analytes of interest or to measure the bias of a
laboratory from an already known accepted value.

Run of Mine (ROM) Ore – Ore produced from a mining operation, which has not
been subject to any size reduction or other processing.

Sample – A subset of a population chosen in such a way that it can be taken to


represent the population with respect to some characteristic.

Sampling Safety Line – Is usually constructed in a nomograph and relates the


minimum sample mass required at a particular particle size to achieve a specified
level of variance. Gy introduced the concept of a 'safety line', which is based on the
relationship between the introduced variance and the particle top size.

If the sampling constant is taken to be dependent only on particle top size and the
sampling constant is known at one particular state of comminution of the material, a
'sampling safety line' can be drawn for the particular analyte to which the sampling
constant applies.

Sampling Constant – The sampling constant for a material describes its


heterogeneity with respect to a particular analyte. The sampling constant is usually
proportional to the cube of the 95% passing size of the particles in the sample, but
this is not always true. Important exceptions to this rule occur when sampling
materials that are low-grade overall but in which the valuable component occurs as
relatively large blebs or nuggets of high-grade material. Diamond ores, alluvial gold
and PGM ore containing 'metallics' where the valuable component is present at
g/tonne levels are the most notable exceptions. Low-grade materials with small
inclusions of high-grade material can have very large sampling constants. The
sampling constant has units of mass, usually expressed in grams.

SCADA – Acronym for Supervisory Control And Data Acquisition, a computer system
for gathering and analysing real time plant data. SCADA systems are used in
industry to monitor and control plant status and provide logging facilities. As the
name indicates, it is not a full control system, but rather focuses on the supervisory
level. As such, it is a purely software package that is positioned on top of hardware
to which it is interfaced, in general via Programmable Logic Controllers (PLCs), or
other commercial hardware modules.

Secondary Accounting – Conducting mass balances over smaller sections of the


total plant circuit, to identify where lock-ups are occurring, time lags are involved or
where any measurement problems exist.

Semi-Permanent Inventory – In-process Inventory contained in process


equipment such as mills (including the liners) or furnaces (including the refractories)
that is only recovered periodically when the equipment is maintained or refurbished.

Sensitivity (as applied to a scale) – The responsiveness of a weighing element or


indicator to a change in the applied load or the ratio of the output response to a

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specified change in the input. The latter can be applied to any element in the
measuring chain.

Shaft (or Mine Section) Call Factor – The mass of a species delivered to a shaft
compared to the mass of that species calculated from sampling and surveying
procedures, expressed as a percentage.

Shewhart (Control) Graphs – These graphs are constructed by plotting the value of
a measurand about a central line of its accepted value. Control and Action lines are
usually drawn at ±2 and ±3 standard deviation levels respectively. Measurements
are said to be “In control” if they are within the 2 standard deviation limits, but
“Action” is required if they are outside 3 standard deviations.

Shipments – An amount of material transported as a defined entity such as a truck,


rail car or ship. It may contain several lots.

Slag – The product from a furnace, smelting or converting operation which normally
contains the gangue materials such as silica, alumina and magnesia in oxide form
and small quantities of the value metals, which is discarded or recycled. An
exception is the titania slag from the smelting of ilmenite which is a raw material for
titanium oxide production and is sold.

Smoothing – The process of removing or reducing fluctuations in data in order to


produce a result that is visually smooth. Typically this is performed by some form of
local averaging.

Sonic Drilling – A technique for drilling that utilises high frequency vibrations
generated from sound waves to penetrate the material being drilled and generate
core samples.

Sonic Drilling – A technique for drilling that utilises high frequency vibrations
generated from sound waves to penetrate the material being drilled and generate
core samples.

Specific Gravity – See relative density.

Splitting Limits – The limits within which values from procedures such as twin-
stream analysis or inter-laboratory analysis should agree.

Spurious Error – The error which invalidates a measurement. They generally have
a single cause such as the incorrect reading of one or more significant digits or the
malfunction of instruments.

Standard Deviation (SD) – The square root of the variance.

Standard Uncertainty – The estimated standard deviation.

Static Scale – A mass measurement device that converts a static load on a


weighbridge or on a platform, inside a hopper or suspended from a gantry scale into
a mass.

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Stopped Belt Sampling – An increment of particulate material is manually removed
from a conveyor belt using a correctly designed former.

Strata – Approximately equal parts of a lot or sub lot based on intervals of time,
mass or space. (AS 4433.1 – 1997)

Systematic Error – The component of the error of measurement which, in the


course of a number of measurements of the same measurand, remains constant or
varies in a predictable way.

Tailings (Rejects, Residues) – The material after the extraction of the maximum
economic amount of the value metals from the feed material such as ore,
concentrate or matte, by treatment processes such as concentration or leaching.

Tare – The mass of an empty container such as a drum, bin, or road or rail truck.

Test chains – A calibrating device of known certified weight consisting of a series of


rollers or wheels linked together to ensure their weight is uniform and they can move
freely (so that chain weight loss due to wear is minimised).

Theoretical Recovery – The ratio of the metal input to a plant, minus the measured
losses from that plant, divided by the metal input to the plant, expressed as a
percentage.

Three-Product Formula – Used in concentrators which produce more than one


concentrate product (eg: lead – zinc concentrators), to obtain a metallurgical balance
for process monitoring purposes, where the component analyses of the feed and
each product stream are known, as well as the mass flow of one of the streams
either entering or leaving the plant.

Tolerance – The limit of error or variance established by authority or usage or a


value fixing the limit of allowable error or departure from true performance or value.
(NIST Handbook)

Toll Treatment – The treatment, through a metallurgical plant, of material that has
been procured from third parties for processing under agreed contractual conditions.
The terms may include the charges for the treatment, recovery percentages for the
products, the time frame for production and penalties for deleterious impurities.

Totaliser – A device for counting and indicating or printing the algebraic sum of
successive inputs made on a serial entry basis. Inputs may represent counts, shaft
rotations etc.

Traceability – The property of the result of a measurement or the value of a


standard whereby it can be related to stated references, usually national or
international standards, through an unbroken chain of comparisons, all having stated
uncertainties.

Transducer – A device for converting energy from one form to another for
information or control purposes.

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Transient Process Inventory – Process inventory in process equipment such as
tanks and bins that is in a transient state and is moving through the equipment and
process on a continuous or regular batch basis.

Transparency – The method of measurement and analysis should be fully


documented.

Triple bottom line reporting – The triple bottom line (TBL) focuses corporations not
just on the economic value that they add, but also on the environmental and social
value that they add and destroy.

At its narrowest, the term 'triple bottom line' is used as a framework for measuring
and reporting corporate performance against economic, social and environmental
parameters.

At its broadest, the term is used to capture the whole set of values, issues and
processes that companies must address in order to minimize any harm resulting from
their activities and to create economic, social and environmental value. This involves
being clear about the company's purpose and taking into consideration the needs of
all the company's stakeholders - shareholders, customers, employees, business
partners, governments, local communities and the public.

t-test (Student’s t test) – A test used on the means of small random samples of one
of the following null hypotheses:

a That the sample has been drawn from a population with a given mean

b That two samples have both been drawn from populations with equal
means

The test compares two sets of results and establishes whether or not there are
statistically significant differences between them.

Two-product formula – Used in concentrators with minimal accumulation of


inventory to calculate plant recovery, where:

Plant Recovery = (Cc/Ff) x 100% = 100c(f – t)/f(c – t)


And C and F are respectively concentrate and feed tonnages
And c, f, and t are respectively concentrate, feed and tails grades.
Ultrasonic Transit Time Flow Meters – A flow meter utilising the principle that the
propagation velocity of sound waves within a fluid is directly influenced by the
velocity of that fluid.

Umpire Analyses – The analytical results obtained by an Umpire Laboratory.

Umpire Laboratory – A laboratory chosen, because of its expertise, to which


samples with disputed results can be sent for arbitration.

Unaccounted Loss or Gain (Metal Accounting Variance) – Any discrepancy


between actual recovery and the accountability over an accounting period.

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Uncertainty – A parameter, associated with the result of a measurement that
characterises the dispersion of the values that could reasonably be attributed to the
measurand.

Uncoupled In-Motion Weighing – The weighing in-motion of wagons that travel


independently across a load receptor (usually achieved by means of an incline of the
approach to the load receptor).

Valuation – The assignment of monetary values to the outputs of metal balances, as


a separate function from metal accounting.

Variance – The sum of the squares of the differences between each measured value
and the mean of the measured values divided by one less than the number of
measurements in the data set. This formula applies only when the individual
measurements are uncorrelated. Successive measurements during a day or several
days in a plant are often correlated, in which case a different formula must be
employed.

Weigh Carriage – A structure supporting the weigh idlers on a conveyor belt weigher,
which in turn transmits the weight through the carriage to the load sensor.

Weigh Idlers – Idlers positioned in the weigh carriage assembly so that they sense
the weight of material on the conveyor and transmit the weight through the carriage
to the load sensor.

Weighbridges – Weigh scales designed to weigh road trucks or rail wagons where
the lever system is usually below ground in a pit so that the vehicle or rail wagon can
pass over and stop on the scale. In a large capacity scale also refers to the
structural frame carried by the main bearing which supports the load-receiving
element.

Y-blenders – Mechanical mixing devices that are used to mix samples within
enclosed containers.

Yield – The quantity of coal (of the quality that one requires) obtained from Run Of
Mine Material expressed as a percentage. There are two subsets:

1 Theoretical Yield: obtained in a laboratory from washability curves. It is


higher than practical yield.
2 Practical Yield: obtained on a plant after losses due to process inefficiency.

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LIST OF ACRONYMS AND ABBREVIATIONS

AS Standards Association of Australia


ASME The American Society of Mechanical Engineers
ASTM American Society for Testing and Materials
BSI British Standards Institute
CITAC Cooperation on International Traceability in Analytical Chemistry
Eurachem Focus for Analytical Chemistry in Europe
ECE Economic Commission for Europe
EPA Environmental Protection Agency
IEC International Electrotechnical Commission
IFRS International Financial Review Society
ILAC International Laboratory Accreditation Conference (USA)
IPA International Petroleum Association
ISA International Society for Automation
ISO The International Organisation for Standardisation
JIS Japanese Industrial Standard (Japanese Standards Association)
NATA National Association of Testing Authorities (Australia)
NISA National Industrial Scale Association (USA)
NIOSH National Institute for Occupational Safety and Health
NIST National Institute of Standards and Technology (USA)
OIML International Organisation of Legal Metrology
SABS The South African Bureau of Standards
SAIMM South African Institute for Mining and Metallurgy
SANAS South African National Accreditation Service
UKAS United Kingdom Accreditation Service
UN United Nations
VAM Valid Analytical Measurement
VIM International Vocabulary of Basic and General Terms in Metrology
VML Vocabulary of Legal Metrology
WHO World Health Organisation

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APPENDICES
APPENDIX A – ACKNOWLEDGEMENTS
Contributions from the following companies and/or individuals by the provision of
information and to the compilation of this Code document are gratefully
acknowledged:

AMIRA International

Anglo American Corporation

Anglo Platinum Corporation

Anglo Research

Anglo Coal South Africa

Anglogold - Ashanti

Anglo Technical Division

BHP Billiton

Endress + Hauser (Pty) Limited

Impala Platinum Limited

JKMRC at the University of Queensland, Australia

Namakwa Sands

Northparkes Mines

Process Automation (Pty) Limited

Rio Tinto

SA Automation System (Pty) Limited

Zincor – A Division of Kumba Base Metals Ltd

The Research Teams:

University of Cape Town: Drs Dave Deglon and Aninda Chakraborty, Omari
Lukwichi, Paul Bepswa and Erica van Tonder

University of Stellenbosch: Dr Jacques Eksteen, Chris Cutler, A Nesbitt,


Busisiwe Madonsela, Elton Thyse and Makiwe Nkohla

University of Queensland: Dr Rob Morrison, Will Jansen

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P754 Project Management and Coordination:

Richard Beck, AMIRA International

Development of the original framework for the Code and contributions to the
section on Metal Balancing:

Dr Rob Morrison, University of Queensland

Statistical and Mathematical Review of Code and the section on Statistical


Theory of Sampling:

Dr Geoff Lyman, Sampling Consultant, Brisbane, Queensland, Australia (for


Anglo Platinum)

The Code Team:

Peter Gaylard, University of Cape Town


Ian Ralston, Anglo Technical Division
Neville Randolph, NSR Investments CC
Mike Wortley, Consultant

Review of and comments on Code and Guidelines Release 2:

Professor Tim Napier-Munn, University of Queensland


Dr Hugh Bartlett, Hugh Bartlett Consulting cc
Dr Ralph Holmes, CSIRO

Editorial preparation of Release 3:

Sally Burt, University of Cape Town

Permission to re-publish:

Lyman, G J, 2005. Sampling, Metallurgical Accounting and Reduction of


Balance Estimation Variance, in Proceedings Second World Conference on
Sampling and Blending, pp 127–135 (The Australasian Institute of Mining and
Metallurgy: Melbourne). Re-published with the permission of The Australasian
Institute of Mining and Metallurgy.

Cutler, C J, and Eksteen, J J, 2006. Variance Propagation in Toll Smelting


Operations Treating Multiple Concentrate Stockpiles, JSAIMM vol.106, pp
222–227. Re-published with the permission of the Southern African Institute
of Mining and Metallurgy.

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APPENDIX B – REFERENCES

B.1 MASS MEASUREMENT

Code and Guidelines: Section 3

1 Colijn, H. (1983). Weighing and Proportioning of Bulk Solids, Trans Tech


Publications, Germany
2 ibid, Chapter 7, pp 207-219
3 ibid, Chapter 6, pp 175-193
4 ibid, Chapter 5, pp 145-173
5 ibid, Chapter 6, pp 194-204
6 ibid, Chapter 7, pp 207-226
7 ibid, Chapter 7, pp 226-238
8 ibid, Chapter 7, pp 214-215
9 ibid, Chapter 10, pp 317-328
10 ibid, Chapter 9, pp 313-314
11 ibid, Chapter 2, pp 32-42
12 Crabtree, M. (2000). Flow Handbook, Crown Publications, South Africa
13 Furness, R.A., (1996). Outstanding and Contentious issues in Flow
Measurement and Recent Real Advances in Magnetic Flowmeters, ABB
Kent Measurement (Pty) Ltd.
14 Merks, J.W., (1985). Sampling and Weighing of Bulk Solids, Trans Tech
Publications, D-3392 Clausthal-Zellerfeld, Germany.
15 ibid, Chapter 8 pp. 304-307
16 16. National Industrial Scale Association, “Back Publications of the
National Industrial Scale Association”
17 Strauss, T., (2004), Flow Handbook, Endress+Hauser Flowtec AG,
Switzerland
18 ibid, Chapter 3, pp 50 – 51
19 ibid, Chapter 5, pp 319 – 322
20 ibid, Chapter 11, pp 407 – 410
21 ibid, Chapter 7, pp 292 – 293
22 Merks, J.W. (1988), “Sampling and Weighing of Mineral Concentrates”,
Bulk Solids Handling, 8(2), pp. 179-187
23 Colijn, H. (1991), “Weighing of Bulk Solids”, Bulk Solids Handling, 11(1),
pp. 113-119
24 Schmedt, R. (1992),”Measurement of Bulk Solids Flow”, Bulk Solids
Handling, 4(1), pp.81-84

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25 Boeck, Th. (1987), “Mass Flow Measuring System for Pneumatically
Conveyed Solids”, Bulk Solids Handling, 7(4), pp.539-545
26 Kochsiek, Glaser, (2000), “Comprehensive Mass Metrology,” Wiley VCH,
Section 3.6 “Determination of Mass in Practice”
27 Liptak, B.G., “Instrument Engineers’ Handbook, Volume 1, Fourth Edition:
Process Measurement and Analysis”
28 Johnson, G., “Slurry Flow Measurement”, Paterson and Cooke
Consulting Engineers (Pty) Ltd
29 Pomroy, J., “Selecting the Right Flowmeter”, Chemical Engineering
Vol.103, No5, May 1996, pp.96–102
30 Brown, N.P, Heywood N.I., “The Right Instrumentation for Slurries”,
Chemical Engineering, September 1992, pp.106-112
31 Moore, A., “Selecting a Flowmeter”, The Chemical Engineer, April 1986,
pp. 39-45
32 Merret, J., “Go with the Flow”, The Chemical Engineer, May 1996, pp.19-
22
33 Stumm, Dr. W., “Mass Flow: Part 1 Principles and Techniques”, Pulse Vol.
7 1989, pp. 45-51
34 Stumm, Dr. W., “Mass Flow: Part 2 Coriolis Measuring Characteristics”,
Pulse Vol 8 1989, pp. 44-48
35 Hall, J., “Improve plant efficiency with direct mass flow measurements”,
The Industrial and Process Control Magazine, Feb. 1983, pp 43-47
36 Labs, W., “Flowmeters: Accuracies are better, prices lower”, The
Industrial and Process Control Magazine, Feb. 1990, pp. 29-33
37 Benard, C., “ Flow Measurement in the Power Industry”, Power
International, April 1986, pp. 86-89
38 Yan, Y., “Flow Rate Measurement of Bulk solids in Pneumatic Pipelines;
Problems and Solutions”, Bulk Solids Handling, Vol 15,1995, pp.447-
456
39 Merks, J.W. and Merks E.A.T., Precision and Bias for Mass
Measurement Techniques, Matrix Consultants, Vancouver, 1992

B.2 MASS FLOW ON CONVEYORS

Guidelines: Section 3.4.3

1 National Industrial Scale Association, (Updated 1998) “Overview of


Conveyor Belt Scales”
2 Soderholm, A. (2000), “Conveyor Belt Scales – A Mechanical Dilemma”,
Bulk Solids Handling, 20(4), pp 534-537
3 Lockwood, F. (1981), “Continuous Belt Weighers”, Bulk Solids Handling,
1(2), pp. 235-237

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4 Allenberg, B. (1993), “Requirements on Continuous Weighers in a Quality
Assurance System”, Bulk Solids Handling, 13(2), pp. 314-318
5 Carpentier, P.T. (1983), “Conveyor Belt Certification: Weighing the various
Systems”, Coal Mining and Processing, November pp. 42-48
6 Abbott, J.A. (1989), “The Effect of Conveyor Belt Mistracking on Belt
Weighing Errors”, Bulk Solids Handling, 9(1), pp. 107-117
7 Abbott, J.A. (1986), “ The Effect of Idler Misalignment and Belt Stiffness
on Belt Weighing Errors”, Bulk Solids Handling, 6(1), pp. 121-128
8 Fristedt, K. (1986), “Belt Weighing Errors – From where do they Origin”,
Bulk Solids Handling, 6(5), pp. 963-968
9 Jost, G. (1986), “Comparison of Nuclear and Gravimetric Systems for the
Continuous Weighing of Bulk solid Flows”, Bulk Solids Handling, 6(6),
pp. 1191-1197
10 Lauber, F.R. (1990), “Alternative Weighing Technology for Belt Conveying
Systems”, Bulk Solids Handling, 10(3), pp. 333-335

B.3 BULK MASS MEASUREMENT: DRAUGHT SURVEYS

Code: Section 3.3 and Guidelines: Section 3.4.6

1 Beemster, J. (1992), “A critical look at the draft survey”, Bulk Solids


Handling, 12(2), pp. 264-265
2 Bhandary, N.S.C. (1992), “On draft surveys”, Bulk Solids Handling,
12(2), pp. 267
3 Kelly, J.P. (1991), “Trade by draft survey or by belt weighing”, Bulk
Solids Handling, 11(1), pp. 239-241
4 Kelly, J.P. (1992), “Draft survey versus legal weighing”, Bulk Solids
Handling, 12(2), pp. 259-260
5 Luyts, P. (1992), “The accuracy of draft surveys”, Bulk Solids Handling,
12(2), pp. 266
6 Merks, J.W. (1985). Sampling and weighing of bulk solids, Trans Tech
Publications, D-3392 Clausthal-Zellerfeld, Germany
7 Merks, J.W. (1992), “Precision and bias for draft surveys and belt scales”,
Bulk Solids Handling, 12(4), pp. 641-648
8 U.N. ECE (1992), “Code of Uniform Standards and Procedures for the
performance of Draught Surveys of Coal Cargoes” (although this applies
to coal the principles can be applied to many bulk commodities)
9 Australian Institute of Marine Surveyors, “Principles and Code of
Practice for Draft Surveys (undated)

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B.4 MASS IN STORAGE AREAS

Guidelines: Section 3.4.7

1 Ooms, M. (1981), “Determination of Contents in Storage Bins and Silos”,


Bulk Solids Handling, 1(4), pp. 651-665
2 Potts, A. (2001),“High Tech Surveying and Measuring,” Mining Magazine,
December2001, pp.270-275
3 Cahill, P., Wright, H., Strutt, S., Wragg, D., (2000), Application of On-Line
Laser Scanning Technology to Improve Unit Bunker Management in Coal-
Fired Power Stations”, Bulk Solids Handling, 20(3) pp. 289-294
4 Lightbody, G., (1983), “How British Steel Manage Stockpiles”, Iron and
Steel InternationaI, October 1983, pp178-182
5 McBride, W., Chambers, A.J., (1999), “Bulk Density Measurement Using a
Shear Box,” Bulk Solids Handling, 19(4) pp. 501-505
B.5 SAMPLING

Code and Guidelines: Section 4

1 Gy, P. (1979), Sampling Of Particulate Materials – Theory and Practice.


Elsevier.
2 Gy, P. (1982), Sampling Of Particulate Materials – Theory and Practice.
2nd Edition. Elsevier.
3 Merks, J.W. (1985), Sampling and weighing of bulk solids, Trans Tech
Publications.
4 Smith, R. and James, G. V. (1981), “The Sampling of Bulk Materials”, The
Royal Society of Chemistry.
5 Holmes R.J. (1992), “Sampling Processes in the Minerals Industry”
Sampling of Mineral Process Streams, November 1992.
6 Holmes R.J. (2004), “Correct Sampling and Measurement – The
Foundation of Accurate Metallurgical Accounting”, Chemometrics and
Intelligent laboratory Systems, pp 71–83.
7 Bartlett, H.E. (2001). “Avoiding Metal Accounting Problems Through the
Application of Statistics and Sample Design” Challenges in Metal
Accounting and Information Management August 2001.
8 Bartlett, H. E. (2002). “Design of primary samplers for slurries in
concentrators and statistical methods for measuring components of
variance in sampling”, The Journal of The South African institute of
Mining and Metallurgy, November/December 2002.
9 Bartlett, H. E. and Viljoen, R. (2002). “Variance relationships between the
masses, grades and particle sizes for gold ores from the Witwatersrand”,
ibid.
10 Francois-Bongarcon, D. and Gy, P. (2002). “Critical aspects of sampling in
mills and plants: a guide to understanding sampling audits”, ibid.

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11 Francois-Bongarcon, D. and Gy, P. (2002). “The most common error in
applying ‘Gy’s Formula’ in the theory of mineral sampling, and the history
of the liberation factor”, ibid.
12 Hunt, C. A. (2002). “Comment on D. Francois-Bongarcon and P. Gy
‘Critical aspects of sampling in mills and plants: a guide to understanding
sampling audits’ and H. E. Bartlett ‘Design of primary samplers for slurries
in concentrators and statistical methods for measuring components of
variance in sampling’”, ibid.
13 Pitard, F. F. (2002). “Practical and Theoretical Difficulties When Sampling
Gold” Mineral Processing Plant Design, Practice and Control – Volume 1,
Edited by L. Mular et al, Society of Mining, Metallurgy and Exploration.
14 Pitard, F. F. (1993). Pierre Gy’s Sampling Theory and Sampling Practice,
2nd Edition, CRC Press.
15 Merks, J. W. (2002). “Sampling in Mineral Processing”, ibid.
16 Lyman, G.J. (1993). Determination of bias in sampling systems, Minerals
Engineering, 6 99–105.
17 Pitard, F. F. (2005). "Sampling Correctness – A Comprehensive
Guideline," Proceedings of the Second World Conference on
Sampling and Blending, Brisbane, May 2005.
18 Bartlett, H.E. and Hawkins, D.M., Chapter 13, 'Process Evaluation' in "The
Extractive Metallurgy of Gold in South Africa" Vol 2, (1987) ed Stanley
GG

B.6 ANALYSIS

Code and Guidelines: Section 5.3

1 Barwick V. (2003). “Preparation of Calibration Curves. A Guide to Best


Practice”. LGC/VAM/2003/032
2 Hawkins DM and Olwell DH (1998). “Cumulative Sum Control Charts and
Charting for Quality Improvement”, Springer.
3 J. C. Sherlock et al., “Analysis – Accuracy and Precision?”, Chem. Br.,
1985, 21, 1019.
4 B. Griepink, “Certified Reference Materials (CRM’S) for the Quality of
Measurement”, Fresenius’ J. Anal. Chem., 1990, 337, 812.
5 M. Sargent, “Development and Application of a Protocol for Quality
Assurance of Trace Analysis”, Anal. Proc., 1995, 32, 71.
6 “Guidelines for Achieving Quality in Trace Analysis”, ed. M. Sargent and G.
A. MacKay, The Royal Society of Chemistry, UK, 1995. ISBN 0-85404-
402-7.
7 F. M. Garfield, “Quality Assurance Principles for Analytical Laboratories”,
Association of Official Analytical Chemists, 2nd edn, Arlington, VA, 1991.

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8 J. K. Taylor, “Quality Assurance of Chemical Measurements”, Lewis
Publishers, Chelsea, MI, 1987.
9 “Quality Assurance for Analytical Laboratories” ed. M. Parkany, Special
Publication no. 130, The Royal Society of Chemistry, UK, 1993, ISBN 0-
85186-705-7.
10 G. V. Roberts, “Quality Assurance in Research and Development”, Marcel
Dekker, New York, 1983.
11 J. K. Taylor and N. M. Trahey, “Handbook for SRM Users”, NIST Special
Publications 260-100, National Institute of Standards and Technology,
Washington, DC, 1989.
12 “Uses of Certified Reference Materials’, ISO/IEC Guide 33, Geneva, 1989.
13 Analytical Methods Committee, “Internal Quality Control of Analytical
Data”, Analyst (London), 1995, 120, 29.
14 E. Prichard, “Quality in the Analytical Chemistry Laboratory”, J. Wiley,
Chichester, UK, 1995, ISBN 0471-95541-8 (5).
15 M. Thompson, “Variation of Precision and Concentration in an Analytical
System”, Analyst (London), 1988, 113, 1579.
16 M. Thompson and R. Wood, “Harmonised Guidelines for Internal Quality
Control in Analytical Chemistry Laboratories”, Pure Appl. Chem., 1995, 67,
649.
17 A. F. Bissell, “CUSUM techniques for Quality Control”, Appl. Stat. (UK),
1969, 18, 1.
18 J. M. Lucas and R. B. Crozier, “Fast Initial Response for CUSUM Quality
Control Schemes: Give your CUSUM a Head Start”, Technometrics, 1982,
24, 199.
19 BS EN ISO 9001:1994, “Quality Systems – Model for Quality Assurance in
Design/Development, Production, Installation and Servicing”, BSI,
Chiswick, UK, 1994.
20 “General Requirements for the Competence of Calibrating and Testing
Laboratories”, ISO Guide 25, Geneva, 3rd edn., 1990.
21 “The OECD Principles of Good Laboratory Practice”, Environment
Monograph no. 45, OECD, Paris, 1992.
22 “Official and Standardized Methods of Analysis”, ed. C. A. Watson, The
Royal Society of Chemistry, Cambridge, UK, 3rd edn, 1994, ISBN 0-
85186-441-4.
23 J. K. Taylor, “Validation of Analytical Methods”, Anal. Chem., 1983, 55,
600A.

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B.7 METAL ACCOUNTING

Code and Guidelines: Section 7

1 R. Hantikainen and J. Alaluf, “Integrated Plant-wide Data Management in


Mineral Processing Industries”.
2 R. Cargill, N. Freeman and R. Gilbertson, “Metal Balance of a large
integrated operation using a Standard Industrial Software Package”,
Olympic Dam, WMC, Australia.
3 F. Flament, M. C. Mound, C. Colbert and L. Fradette, (2004) “Practical
integrated metallurgical accounting solutions for supporting production
decisions”, Minerals and Metallurgical Processing, 21(1), pp 1-8
4 A. Smit, “Development of an Integrated Asset Management System for a
Metallurgical Plant – Driefontein Gold Mine, Republic of South Africa”,
Value Tracking Symposium, Brisbane 7th – 8th October, 2002.
5 R. D. Morrison and A. Grimes, “Turning Process Data into Process
Information”, Challenges in Metallurgical Accounting and Information
Management, SAIMM Cape Town, 1st August 2001.
6 J. M. Richardson, “Reconciliation of Mine Site, Mineral Processing Plant,
Concentrate and Tailings Inventories,” Chapter 8
7 R. D. Morrison, “Material Balance Techniques,” Chapter 20
8 R. D. Morrison and M. E. Dunglison, “Improving DMS Operations Through
Corporate Data Reconciliation,” Dense Media 2005, Paarl, South Africa,
March 2005
9 J. A. Jones, R. D. Delster II, C. W. Hill, R. Barker and P. B. Crummie,
“Process Control at Doe Run’s Fletcher Concentrator,” Mining
Engineering, Dec 1991
10 R. D. Morrison, Y. Gu, W. McCallum, “Metal Balancing from Concentrator
to Multiple Ore Sources,” Value Tracking Symposium, Brisbane, 7-8
October, 2002
11 D. O’Sullivan and L. Barnes, ”The Development of KPI and Metallurgical
Accounting Systems at Nabalco,” Value Tracking Symposium, Brisbane,
7-8 October, 2002
12 A.F.Taggart, 1945. Handbook of Mineral Dressing.
13 Vendors of Metal Accounting Software:
13.1 Algosys Inc, Quebec, Canada.
13.2 CitectIIM, Citect, South Africa.
13.3 Knowledge Manager – Industrial IT for Metal Accounting, ABB.
13.4 JKMetAccount, JK Institute, Australia.
13.5 Assaynet – Custom systems, Assaynet.
13.6 Uniformance PHD – Metal Accounting Solution using a data historian
as the basis, Honeywell.

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14 Mine Metallurgical Managers Association of South Africa Circular 1 95
Gold Lock-up in Plants
15 M.L. Fitzgerald, “Metallurgical Accounting and Control,” Trans IMM,
Vol.69, 1959-60, pages 19-42
16 P Guerney, M Dunglison and P M Cameron. "Leveraging Accuracy and
Precision – Multi-Phase Mass Balancing and Reconciliation as a Tool for
Quality Data Management", Proceedings of the Second World
Conference on Sampling and Blending, Brisbane, May 2005.

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APPENDIX C – STANDARDS
C.1 MASS MEASUREMENT

C.1.1 STATIC MASS MEASUREMENT

1 SABS 1649:1995: Non-automatic self-indicating and semi-self-indicating


weighing instruments. (Annexure B gives the requirements for verification
and shows maximum tolerances that are permissible for new installations
as well as instruments in service)
2 SABS 1697:1998: Verification Standards for Verification of Mass-
Measuring Instruments, including commercial standard mass pieces
3 SABS 0259:1990 (ISO/IEC Guide 25:1990): General requirements for the
competence of Calibration and Testing laboratories and ARP 023
Recommended practice for the Application of SABS 0259 to the
Verification of mass measuring instruments under the trade Metrology Act,
1973
4 NIST Handbook 44: Specifications, Tolerances and other Technical
Requirements for Weighing and Measuring Devices Section 1 General
and Section 2.20 Scales
5 OIML R51-1 and 2: Automatic Catch Weighing Instruments Part 1 & 2
6 OIML R60 2000: Metrological Regulation for Load Cells
7 OIML R76-1and 2 1992: Non-Automatic Weighing Instruments Part 1 & 2
8 OIML R107-1and 2: Discontinuous totalising Weighing Instruments
(totalising Hopper Weighers) Part 1and 2
9 ISO 10251: Procedure for the determination of moisture.
10 ISO 12743: Procedure for the taking of samples for the determination of
moisture
11 ISO 12745: Copper, Lead and Zinc Ores and Concentrates--Precision and
bias of mass measurement techniques
12 ISO 13543: Copper, Lead and Zinc Sulphide concentrates--Determination
of mass of contained metal in a lot
13 ISO 17025:1999 General Requirements for the Competence of Testing
and Calibration Laboratories
14 VIM 1993: International Vocabulary of Basic and General Terms in
Metrology
15 VML 1978: Vocabulary of Legal Metrology
16 BS 8422 2003: Force measurement. Strain gauge load cell systems.
Calibration Method
Although standards 11 and 12 apply to base metal concentrates, the basic principles
can be applied to most materials and the calibration methodology can be applied to
any mass measurement.

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C.1.2 IN-MOTION WEIGHING

1 NIST Handbook 44 Section 2.20


2 OIML R106-1and 2 1993/1997: Automatic Rail bridges Part 1 and 2
3 OIML R134-1and2 2003/4: Automatic in-motion Road weighing Part 1 and
2
C.1.3 BELT WEIGHERS

1 NIST Handbook 44 Section 2.22


2 OIML R50-1 and 2 1997: Continuous totalising weighing instruments (Belt
Weighers)
3 ISA-RP74.01-1984: Application and Installation of Continuous-Belt
Weighbridge Scales
4 JISB 7606: Belt Weighers
5 South African Trade Metrology Act And Regulations (77/93) Section 44

C.1.4 MASS FLOW IN CONDUITS

1 ISO Guide: Guide to the expression of Uncertainty in measurement First


Edition 1995 International Organisation for Standardisation
2 ISO 2186: Connections for pressure signal transmissions
3 ISO 2714: Volumetric measurements by displacement meter systems
other than dispensing pumps
4 ISO 2715: Volumetric measurement by turbine meter systems
5 ISO 4006:1991: Measurement of fluid flow in closed conduits - Vocabulary
and Symbols
6 ISO 4064-2: Meters for cold potable water
7 ISO 4185:1993: Measurement of liquid flow in closed conduits – Weighing
method
8 ISO 5167-1:2003:Measurement of fluid flow by means of pressure
differential devices inserted in circular cross-section conduits running full –
Part 1:General principles and requirements
9 ISO 5167-2:2003: Measurement of fluid flow by means of pressure
differential devices inserted in circular cross-section conduits running full –
Part 2: Orifice Plates
10 ISO 5167-3:2003: Measurement of fluid flow by means of pressure
differential devices inserted in circular cross-section conduits running full –
Part3: Nozzles and Venturi Nozzles
11 ISO 5167-4:2003: Measurement of fluid flow by means of pressure
differential devices inserted in circular cross-section running full - Part4:
Venturi tubes

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12 ISO/TR 5168:1998: Measurement of fluid flow – Evaluation of uncertainty
13 ISO 5725:1994, parts 1-6: Accuracy (trueness and precision) of
measurement methods and results
14 ISO 6817:1992: Measurement of conductive liquid flow in closed conduits
– Method using electromagnetic flow meters
15 ISO/TR 7066-1:1997: Assessment of uncertainty in calibration and use of
flow measurement devices - Part 1: Linear calibration devices
16 ISO/TR 7066-2:1997: Assessment of uncertainty in calibration and use of
flow measurement devices - Part 2: Non-linear calibration relationships
17 ISO 7278: Dynamic measurement. Proving systems for volumetric meters;
Part 2: Pipe provers
18 ISO 8316:1987: Measurement of fluid flow in closed conduits – method by
the collection of the liquid in a volumetric tank
19 ISO 9104:1991: Measurement of fluid flow in closed conduits- Methods of
evaluating the performance of electromagnetic flow-meters for liquids
20 ISO 9300: Measurement of gas flow by means of critical flow venturi
nozzles
21 ISO 9368: Measurement of liquid flow in closed conduits by the weighing
method. Procedures for checking installations. Part 1: Static weighing
systems
22 ISO 9951: Measurement of gas flow in closed conduits – turbine meters
23 ISO 10790: 1999/2003: Measurement of fluid flow in closed conduits-
Guidance to the selection, installation and use of Coriolis meters (mass
flow, density and volume flow measurements)
24 ISO 11605: Calibration of variable area flow meters
25 ISO 11631:1998: Measurement of fluid flow – Methods of specifying flow
meter performance
26 ISO/TR 12764: Flow rate measurement of fluid flow means of vortex
shedding flow meters
27 ISO /TR 12765: Methods using transit time ultrasonic flow meters
28 ISO 12767: Guidelines to the effect of departure from the specifications
and operating conditions given in ISO 5167
29 ISO 13359: Flanged-type electromagnetic flow meters – overall lengths
30 ASME MFC-1M: Glossary of terms used in measurement of fluid flow in
pipes
31 ASME MFC- 2M: Measurement uncertainty of fluid flow in closed conduits
32 ASME MFC-3M: Metering flow by means of orifices, nozzles and venturis.
33 ASME MFC-6M: Metering flow in closed conduits by means of vortex-type
meters

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34 ASME MFC-10M: Method of establishing installation effects on flow
meters
35 ASME MFC-11M-2003: Measurement of fluid flow by means of Coriolis
Mass Flow meters
36 ASME MFC-16M-1995: Measurement of fluid flow in closed conduits by
means of Electromagnetic flow-meters
37 ASME MFC-18M: Metering flow by means of variable area meters
38 ASME PTC-19.5: Application of fluid meters
39 AS 2360.1.2 1993 (BS 1042: Section 1.2:1993): Measurement of Fluid
Flow in Closed Conduits. Part 1.2: Pressure differential methods—
Measurement using orifice plates or nozzles- Conduits with diameters less
than 50mm.
40 AS 2360.1.3 1993 (BS 1042: Section 1.4 1992): Measurement of Fluid
flow in Closed Conduits. Part 1.3: Pressure differential methods—
Measurement using orifice plates, nozzles or Venturi tubes – Guide to the
use of methods specified in Parts 1.1 and 1.2.
41 OIML R 10: 1993: Direct Mass Flow Measuring Systems for Quantities of
Liquids.
42 OIML P17: Guide to the expression of uncertainty in measurement (GUM)
43 OIML D25: Vortex meters (used in measuring systems for fluids
44 OIML R105C: Direct mass flow measuring systems for quantities of liquids
45 BS EN 7405: Guide to the selection and application of flow meters for the
measurement of fluid flow in closed conduits
C.1.5 MASS FLOW IN OPEN CHANNELS

1 ISO 748: Measurement of liquid flow in open channels – Velocity-area


methods
2 ISO 1438-1:1980: Water flow measurement in open channels using weirs
and venturi flumes – Part1: Thin plate weirs
3 ISO 2537: Liquid flow measurements in open channels – Rotating
element current meters
4 ISO 4377: Hydrometric determinations – Flow measurement in open
channels using structures – Flat-V weirs
5 ISO/TR 8363:1997: Measurement of liquid flow in open channels- General
guidelines for selection of method
6 ISO 9555: Measurement of liquid flow in open channels – tracer dilution
methods for measurement of steady flow
7 ISO 9826: Measurement of flow in open channels; Parshall and SANIIRI
flumes
8 ISO/TS 15768: Measurement of liquid velocity in open channels – Design,
selection and use of electromagnetic current meters.

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C.2 SAMPLING

C.2.1 GENERAL

1 JIS M 8100:1992 Particulate Materials – General Rules for Methods of


Sampling
2 JIS M 8702:2002: Iron Ores – Sampling and Sample Preparation
Procedures
3 JIS Z 8816:2001 Particulate Materials – General Requirements for
Methods of Sampling
4 AS 2884.1–1997 Heavy mineral sand concentrates – Sampling. Part 1:
Moving Streams
5 AS 4433.1–1997 Guide to the Sampling of Particulate Materials. Part 1:
Sampling Procedures
6 AS 4433.2–1997 Guide to the Sampling of Particulate Materials. Part 2:
Preparation of Samples
7 AS 4433.3–2002 Guide to the Sampling of Particulate Materials. Part 3:
Estimating Sampling Precision
8 AS 4433.4–2001 Guide to the Sampling of Particulate Materials. Part 4:
Checking for Bias
9 AS 4433.5–2001 Guide to the Sampling of Particulate Materials. Part 5:
Sampling of Slurries
10 AS 4433.6–2000 Guide to the Sampling of Particulate Materials. Part 6:
Inspection of Mechanical Sampling Systems
11 ISO 11648–2:2001 Statistical Aspects of Sampling from Bulk Materials –
Part 2 Sampling of Particulate Materials

C.2.2 COAL

1 ISO 1953:1994 Hard Coal - Size analysis by sieving


2 ISO 1988:1975 Hard Coal - Sampling
3 ISO 13909 – 1:2001 Hard Coal and Coke – Mechanical Sampling Part 1
General Introduction
4 ISO 13909 – 2:2001 Hard Coal and Coke – Mechanical Sampling Part 2
Coal – Sampling from moving streams
5 ISO 13909 – 3 Hard Coal and Coke – Mechanical Sampling Part 3 Coal
Sampling from stationary lots
6 ISO 13909 – 4 Hard Coal and Coke – Mechanical Sampling Part 4 Coal
Preparation of test samples
7 ISO 13909-7:2001 Hard Coal and Coke - Mechanical Sampling Part 7
Methods for Determining the Precision of Sampling, Sample Preparation
and Testing
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8 ISO 20905:2004 Coal Preparation – Determination of dust/moisture
relationship for coal
9 ASTM D2013: Standard Practice of Preparing Coal Samples for Analysis
10 ASTM D3302a: Standard Test Method for Total Moisture in Coal

C.2.3 IRON ORES AND FERROALLOYS

1 ASTM E877 – 03: Standard Practice for the Sampling and Sample
Preparation of Iron Ores and Related Materials.
2 ISO 3082:2000 Iron Ores – Sampling and Sample Preparation
Procedures
3 ISO 3083:1973 Iron Ores – Preparation
4 ISO 3085:2002: Iron Ores – Experimental Methods for Checking the
Precision of Sampling, Sample Preparation and Measurement
5 ISO 3086:1998: Iron Ores – Experimental Methods for Checking the Bias
of Sampling
6 ISO 3087:1998 Iron Ores – Determination of the Moisture Content of a Lot
7 ISO 3713:1987 Ferroalloys – Sampling and preparation of samples –
General Rules
8 ISO 3852:1988 Iron Ores – Determination of Bulk Density
9 ISO 4551:1987 Ferroalloys—Sampling and Sieve Analysis
10 ISO 4552-1 Ferroalloys: Sampling and Sample Preparation
11 ISO 4552-2 Ferroalloys: Sampling and Sample Preparation for Chemical
analysis
12 ISO 7087:1984 Ferroalloys – Experimental methods for the evaluation of
the quality variation and methods for checking the precision of sampling
13 ISO 7347:1987 Ferroalloys – Experimental methods for checking the bias
of sampling and sample preparation
14 ISO 7373:1987 Ferroalloys Experimental methods for checking the
precision of sample division
15 ISO 7764:1985 Iron Ores – Preparation of Pre-dried Test Samples for
Chemical Analysis
16 ISO 8049:1988 Ferronickel shot – Sampling for analysis
17 ISO 8050:1988 Ferronickel ingots or pieces – Sampling for analysis
18 ISO 10836:1994: Iron Ores – Method of Sampling and Sample
Preparation for Physical Testing
19 ISO 14284:1996 Steel and Iron – Sampling and preparation of samples
for the determination of chemical composition

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C.2.4 NON-FERROUS MATERIALS

1 JIS M 8101:1998: Methods of Sampling, Preparation and Determination of


Moisture Content in Non-ferrous Metal Bearing Ores
2 JIS M 8108:1992: Chromium, Manganese and Ferruginous Manganese
Ores – Sampling and Determination of Moisture Content and Size
Distribution
3 ASTM E2293-03: Standard Practice for Drying Metal Bearing Ore
4 ISO 12742:2000: Copper, Lead and Zinc Sulphide Concentrates –
Sampling Procedures for the Determination of Metal and Moisture Content
5 ISO 12743: Copper, Lead and Zinc Sulphide Concentrates – Sampling
Procedures for the Determination of Metal and Moisture Content
6 ISO 12744:1997: Copper, Lead and Zinc Sulphide Concentrates –
Experimental Methods for Checking the Precision of Sampling
7 ISO 12745:1996: Copper, Lead and Zinc Sulphide Concentrates –
Precision and Bias of Mass Measurement Techniques
8 ISO 13292:1997: Copper, Lead and Zinc Sulphide Concentrates –
Experimental Methods for Checking the Bias of Sampling
9 ISO 13543:1996 Copper, Lead and Zinc Sulphide Concentrates –
Determination of Mass of Contained Metal in a Lot
10 ISO 20081:2005 Zinc and zinc alloys – Method of sampling –
specifications
11 ISO 1811 – 1:1988 Copper and copper alloys – Selection and preparation
of samples for chemical analysis – Part 1 Sampling of cast unwrought
products
12 ISO 1811 – 2:1998 Copper and copper alloys – Selection and preparation
of samples for chemical analysis – Part 2 Sampling of wrought products
and castings
13 ISO 4296 – 1:1984: Manganese Ores – Sampling Part 1. Increment
Sampling
14 ISO 4296 – 2:1983: Manganese Ores – Sampling Part 2. Preparation of
samples
15 ISO 4299:1989 Manganese Ores – Determination of Moisture Content
16 ISO 6140:1991: Aluminium Ores – Preparation of Samples
17 ISO 6153:1989: Chromium Ores – Increment Sampling
18 ISO 6154:1989: Chromium Ores – Preparation of Samples.
19 ISO 6208:1992 Nickel and nickel alloy Plate, sheet and strip
20 ISO 7156:1991 Refined Nickel: Sampling

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21 ISO 8541:1986: Manganese and Chromium Ores – Experimental Methods
for Checking Bias of Sampling and Sample Preparation
22 ISO 8542:1986: Manganese and Chromium Ores – Experimental Methods
for Evaluation of Quality Variation and Methods for Checking Precision of
Sampling
23 ISO 8685:1992: Aluminium Ores – Sampling Procedures
24 ISO 8868 Fluorspar: Sampling and Sample Preparation
25 ISO 10226:1991 Aluminium Ores – Experimental Methods for Checking
Bias of Sampling
26 ISO 10227:1995: Aluminium Ores – Experimental Methods for Checking
Precision of Sampling

C.3 ANALYSIS

C.3.1 ISO STANDARDS

1 ISO 17025:1999 General requirements for the competence of testing and


calibration laboratories
2 ISO Guide 30:1992 Terms and definitions used in connection with
reference materials
3 ISO Guide 31:2000 Contents of certificates of reference materials
4 ISO Guide 32:1997 Calibration of chemical analysis and use of certified
reference materials
5 ISO Guide 33:2000 Uses of certified reference materials
6 ISO Guide 34:2000 General requirements for the competence of
reference material; producers
7 ISO Guide 35:1989 Certification of reference materials-General and
statistical principles
8 ISO/REMCO Document N330 List of producers of certified reference
materials. Information by Task Group 3 “Promotion”
9 ISO 9000:2000 Quality Management Systems – Fundamentals and
vocabulary
10 ISO Guide to the Expression of Uncertainty in Measurement
11 ISO/CASCO 193 (Rev. 2) – ISO/CASCO discussion paper providing up-
to-date references on terminology between full updates of ISO Guide 2
12 ISO Guide 2:1996 Standardisation and related activities – General
vocabulary
13 ISO 8402:1994 Quality – Vocabulary
14 ISO 10011-1:1990 Guidelines for auditing quality systems. Part 1:
Auditing

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15 ISO 10011-2:1991 Guidelines for auditing quality systems. Part 2:
Qualification criteria for quality system auditors
16 ISO 10011-3:1991 Guidelines for auditing quality systems. Part 3:
Management of audit programmes
17 ISO 3534-1:1993 Statistics – Vocabulary and symbol – Part 1: Probability
and general statistical terms
18 ISO 3534-2:1993 Statistics – Vocabulary and symbol – Part 2: Statistical
quality control
19 ISO 3524-3:1985 Statistics – Vocabulary and symbol – Part 3: Design of
experiments
20 ISO 7870:1993 Control charts – General Guide and Introduction
21 ISO 7873:1993 Control charts for arithmetic average with warning limits
22 ISO 7966:1993 Acceptance control charts
23 ISO 8258:1991 Shewhart control charts
24 ISO VIM International vocabulary of basic and general terms in metrology,
2nd ed., 1993
25 ISO 11095:1993 Linear calibration using reference materials

C.3.2 ILAC PUBLICATIONS

1 ILAC-I1: 1994 Legal Liability in Testing


2 ILAC-I2: 1994 Testing, Quality Assurance, Certification and Accreditation
3 ILAC-I3: 1996 The Role of Testing and Laboratory Accreditation in
International Trade
4 ILAC-I4: 1996 Guidance Documents for the Preparation of Laboratory
Quality Manuals
5 ILAC-G2: 1994 Traceability of Measurement
6 ILAC-G3: 1994 Guidelines for Training Courses for Assessors
7 ILAC-G4: 1994 Guidelines on Scopes of Accreditation
8 ILAC-G8: 1996 Guidelines on Assessment and Reporting of Compliance
with Specification
9 ILAC-G9: 1996 Guidelines for the Selection and Use of Certified
Reference Materials
10 ILAC-G10: 1996 Harmonised Procedures for Surveillance &
Reassessment of Accredited Laboratories
11 ILAC-G11: 1998 Guidelines on Assessor Qualification and Competence
12 ILAC-G15: 2001 Guidance for Accreditation to ISO 17025

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13 ILAC-G17: 2002 Guidance for Introducing the Concept of Uncertainty of
Measurement in Testing in Association with the Application of the
Standard ISO 17025

C.3.3 CITAC/EURACHEM PUBLICATIONS

1 CITAC/EURACHEM Guide CG1: 2002 Guide to Quality in Analytical


Chemistry
2 CITAC/EURACHEM Guide CG4: 2000 Quantifying Uncertainty in
Analytical Chemistry
3 CITAC/EURACHEM Guide 2003 Traceability in Chemical Measurement
4 CITAC/EURACHEM Quality Assurance for Research and Development
and Non-Routine Analysis
5 CITAC/EURACHEM Guide The Fitness for Purpose of Analytical Methods

C.3.4 UKAS PUBLICATIONS

1 UKAS Publication ref:LAB 7 Group Laboratories Accreditation


2 UKAS Publication ref:LAB 12 The Expression of Uncertainty in Testing
3 UKAS Publication ref:LAB 13 Guidance on the Application of ISO 17025
Dealing with the Expressions of Opinions and Interpretation
4 UKAS Publication ref:LAB 14 Calibration of Weighing Machines
5 UKAS Publication ref:LAB 15 Traceability: Volumetric Apparatus
6 UKAS Publication ref:LAB 27 Accreditation for Chemical Laboratories
7 UKAS Publication ref:LAB 39 Guidance on the Implementation and
Management of Flexible Scopes of Accreditation within Laboratories

C.3.5 ASTM PUBLICATIONS

1 ASTM E1479 – 99: Standard Practice for Describing and Specifying


Inductively-Coupled Plasma Atomic Emission Spectrometers.
2 ASTM E1577 – 95 (2000): Standard Guide for Laboratory Information
Management Systems (LIMS).
3 ASTM E1587 – 94 (1998) Standard Methods for Chemical Analysis of
Refined Nickel.
4 ASTM E1601 – 98 (2003) e1: Standard Practice for Conducting an Inter-
laboratory Study to Evaluate the Performance of an Analytical Method.
5 ASTM E1691 – 95 (2001): Standard Guide for X-ray Emission
Spectrometric Analysis.

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6 ASTM E1691 – 95 (2001): Standard Guide for Evaluation and
Assessment of Analytical Chemical Laboratories.
7 ASTM E1724 – 95 (2001): Standard Guide for Testing and Certification of
Metal and Metal Related Reference Materials.
8 ASTM E1763 – 98 (2003): Standard Guide for Interpretation and Use of
Results from Inter-laboratory Testing of Chemical Analysis Methods.
9 ASTM E1950 – 98 (2003): Standard Practice for Reporting Results from
Methods of Chemical Analysis.
10 ASTM E2028 – 99 Standard Practice for Receiving, Testing and
Reporting Results of Investigations of Metal, Ore or Metal Related
Samples that Are or May Be Involved in Litigation.
11 ASTM E2053 – 00: Standard Guide for Planning, Carrying Out and
Reporting Traceable Chemical Analysis of Metals, Ores and Related
Materials.
12 ASTM E2066 – 00: Standard Guide for Validation of Laboratory
Information Management Systems.
13 ASTM E50- 00: Standard Practices for Apparatus, Reagents and Safety
Considerations for Chemical Analysis of Metals, Ores and Related
Materials.
14 ASTM E882 – 87 (2003): Standard Guide for Accountability and Quality
Control in the Chemical Analysis Laboratory.
15 ASTM D6091 Standard Practice for 99%/95% Inter-laboratory Detection
Estimate (IDE) for Analytical Methods with Negligible Calibration Error

C.3.6 NATA PUBLICATIONS

1 NATA December 2002 Laboratory Assessment Worksheet


2 NATA May 2003 17025 Checklist with Interpretive Comments

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APPENDIX D – CHECK-LISTS
D.1 MASS MEASUREMENT

D.1.1 GENERAL

CRITERIA EXPLANATION
Certification The procedure, which is a legal requirement, whereby a mass
(Assizing) or volume measuring instrument is approved as usable for
Custody Transfer and trade purposes and, in terms of this
Code, for Primary Metal Accounting, which must be performed
at laid down intervals by the relevant government authority or
their authorised agents. Procedures are laid down in National
Metrology Acts.
Calibration The procedure (as per National Metrology Acts, OIML
Recommendations, the NIST Handbook, ISO or other
applicable standards) for checking a mass or flow measuring
device, which must be performed at periodic intervals and at a
sufficient frequency, to measure the error in the result reported
by the device against a standard known mass or volume. This
is in order to ensure that the reported mass or flow
measurements remain within the required precision stipulated
for Primary Metal Accounting or Custody Transfer.
Exception Report Required for all mass/flow measurements in cases where the
Code requirements cannot be adhered to. Must be fully
motivated with reasons, a plan for improvement and approved
by Senior Management.
Non-Conformance Required for all mass/flow measurements in cases where an
Report internal or independent Metal Accounting Review has found
that the Code requirements have not been met and/or where
there is no Exception Report approved. It must contain the
reasons why the Code requirements have not been met and
recommendations for improvements and it must be signed off
by the Internal audit team leader or the Competent Person (if
as a result of an independent Metal Accounting Review).
Records Records of all certification and calibration test results must be
kept for five years. These records must show all the results and
measured errors and document any alterations and
adjustments made to the instrument and installation.

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D.1.2 STATIC AND IN-MOTION WEIGHING

CRITERIA EXPLANATION
Test Weights Static weights, and in the case of In-Motion weighing, weighed
railway wagons, used for calibration must have been weighed on
a test facility and certified to be accurate to the required
tolerance. In the case of Weigh Bins/Hoppers and Gantry
Scales, facilities for loading and unloading the test weights on to
the framework are required.
Support Structure The structure supporting Weigh bins/Hoppers must be robust
for Bins enough to minimise deflection and to ensure that the load is
transferred evenly onto the load sensors.
In-Motion Truck speed must be limited and controlled to ≤8 km/hr, rail
Weighing trucks to be weighed empty (tared) on the weigher on every
occasion before/after filling or emptying. The rails must be
straight and firmly held in concrete in the vicinity of the weigher.
Track must be well maintained to limit impact, shocks and
vibration
Preferred Method Static weighing is the preferred method for all primary
accounting if feasible, as it is the most precise and it has greater
sensitivity

D.1.3 CONVEYOR BELT WEIGHING

CRITERIA EXPLANATION
Type of Weigher Whether the weigher is nuclear or electromechanical (approach-
retreat, pivoting or fully suspended), fitted with counterweight or
not, type and number of load sensors, the number of weigh idlers,
the method of belt speed pickup and sensing and the type of
micro processor. Nuclear weighers are not suitable for Primary
Metal Accounting or Custody Transfer.
Calibration Procedures such as bulk (material) tests, test chains, belt cuts,
certified static weights or electronic procedures used to check the
precision of conveyor belt weighers. For Primary Metal
Accounting, bulk tests as per approved standards are mandatory
and thus facilities for accurate check pre- or post-weighing of the
bulk material passing over the weigher are required. Calibration to
include zero and span checks over 20-100% of the operating
range, for ten minutes or three belt revolutions whichever is the
greater, repeated three times to check repeatability as specified in
OIML Recommendations, the NIST Handbook or other applicable
standards. No ISO standard exists for conveyor belt weighers.
Conveyor Belt Endless, with smooth spliced joints and as flexible as possible,
sized to give a minimum loading of 20% and an operating range

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CRITERIA EXPLANATION
of 60-80% of capacity.
Class of Weigher The three classes as per OIML 50 with specified maximum errors
on verification and in service. For Primary Metal Accounting belt
weighers must meet the requirements of OIML 50 Class 0,5 (a
maximum permissible error in service of ± 0,5%).
Conveyor System To facilitate obtaining the required accuracy, the conveyor system
should meet as many as possible of the Best Practice
requirements, in the Code and Standards, for design, installation,
operation and maintenance, with respect to the conveyor layout
and structure, position of the weigher in relation to factors which
may affect it (such as curves in the belt, the feed system, skirting,
training idlers), feed system, idlers, gravity/automatic take-up, and
protection from the environment. In general these requirements
are in order to ensure as low a tension in the belt as possible, a
steady feed with no overloading of the belt, rigid construction of
the conveyor and weigh suspension with little deflection, careful
alignment of belt and weigh idlers, protection from wind and
weather and cleanliness of the weigh suspension.
Belt Speed By cylinder or wheel directly in contact with belt surface, near the
Pickup weigh span, installed at 90 degrees to the direction of belt travel
in such a manner as to minimise slip. To be kept clean at all
times.
Integrating Computes, indicates, totals and records the mass flow of material
System over the belt and the instantaneous flow rate, from the mass on
the belt and the belt speed.

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D.1.4 FLOW MEASUREMENT

CRITERIA EXPLANATION
Type of Flow Careful selection and specification from many types to suit the
meter specific application. For Metal Accounting the choice for slurries is
limited to Electromagnetic flow meters, or in a few cases, Coriolis
or Ultrasonic types. All except the Coriolis, measure volume flow
and thus require relative density/specific gravity measurement
(See E.1.6), which can introduce significant error. Manufacture,
selection and installation must adhere to the applicable standards
(ISO 6817, ISO 9104, ISO10790, ISO 13359, ASME MFC-11M-
2003, ASME MFC-16M-1995)
Specifications The uncertainty of the instrument must be specified in terms of
and Performance ISO 11631 with traceability back to the approved test
meter/facility preferably according to Group A but at least Group
B.
Certification The initial calibration and certification to be in terms of ISO 4185
or ISO 8316, in a facility accredited in accordance with ISO
17025, and the uncertainty assessed in terms of ISO 7066 and
5168.
Calibration For Primary Accounting the meters must be calibrated, on the
material being measured, on a regular basis utilising the
principles in ISO 4185 or 8316. This requires accurate
volumetric/weighing tanks and an efficient diversion system to
obtain flow rate comparisons. Relative density/specific gravity
measurement is as important as the flow (See E.1.6.).

D.1.5 STOCKS AND INVENTORY

CRITERIA EXPLANATION
Stockpiles Reduce to zero to establish absolute value and/or manage to
measure mass of receipts and withdrawals accurately to calculate
stock by difference. Use of parallel stockpiles to enable regular
emptying. Volumetric surveys only to be used where the above is
impossible on the understanding that the results will only be as
good as sampling and bulk density determination and accuracy
allow. No international standards exist.
Process Inventory “Bubble method” for high value materials and use of parallel
streams or vessels, to facilitate emptying
Audits Internal and Independent audits to check and recommend
corrections, if any, for approval by Competent Person.

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D.1.6 DENSITY AND MOISTURE MEASUREMENT

CRITERIA EXPLANATION
Moisture Required in all cases as mass measurement instruments measure
wet mass. Sampling for moisture must conform with this Code,
ensuring that the assigned moisture is applicable to the material
being weighed.
Density of Density gauges must be calibrated on the actual material being
Slurries measured and accurate relative densities of both solid and liquid
phases are required.
Bulk Density Variable even for the same material as it is affected by many
factors such as particle size and compaction. Most reliable
method is measurement of the mass of a known volume.

D.2 SAMPLING

CRITERIA EXPLANATION
Type of sampler Whether the primary sampler is a cross-stream sampler from a
conveyor belt or slurry stream, a hammer sampler or an auger
sampler. If it is a cross-stream sampler, what are the design
criteria of the system e.g. gap size, cutter speed, radial or
parallel etc.?
Multi-stage If it is a multi-stage sampling system: The number of stages,
Sampling system whether there is sample reduction between stages and the
percentage cut at each stage, together with the total percentage
cut. Experimentation undertaken to ensure sample division does
not introduce excessive variance.
Sampling Interval The basis of the time interval between increments.
Batch Size The basis of the batch size i.e. is it on a time (shift) or tonnage
(lot) basis.
Sub-sampling Whether any further sample division is done on the plant and, if
so, details of how this is done.
Drying conditions If sample drying is carried out on the plant, the drying
temperature and duration.
Sample labelling Label type and sample identification details.
Quality checks Whether the sample weight at each stage is related to the
expected weight based on process flows, cutter gap, cutter
speed and sampling interval.
Inspections The frequency of inspections and level of employee.
Fault reporting The procedure for reporting faults, their rectification and the
and rectification signing-off by management.

Exception Reports on non-compliance with the Code must contain the


Reports reasons for non-compliance, action plans to reach compliance

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CRITERIA EXPLANATION
and be signed-off by the Competent Person.

D.3 SAMPLE PREPARATION

CRITERIA EXPLANATION
Sub-sampling The mass and top particle size of the sample received by the
laboratory. Whether further sample division is necessary before
drying and, if so, details of how this is done.
Drying conditions Drying temperature and duration
Sample reduction Type of equipment used e.g. jaw crushers, pulverisers, ring and
puck mills etc. Action taken to guard against dust loss,
contamination from the equipment e.g. iron, chromium and
cobalt and cross-contamination.
Sample division Type of equipment used e.g. spinning rifflers, turning tube
dividers etc. Experimentation undertaken to ensure that
excessive variance is not introduced by sampling division.
Action taken to guard against dust loss and cross-
contamination.
Sample mixing Type of equipment used e.g. Y-blenders, cube blenders etc.
and duration.
Sample storage Details of container and storage conditions. Duration of storage
and authorisation level for disposal.
Quality checks Contamination from sample reduction equipment. Particle size
analysis after each reduction stage. Splitting ratios from the
sample division equipment.
Inspections The frequency of inspections and the level of employee.
Fault reporting The procedure for reporting faults, their rectification and the
and rectification signing-off by management.

Exception Reports on non-compliance with the Code must contain the


Reports reasons for non-compliance, action plans to reach compliance
and be signed-off by the Competent Person.

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D.4. ANALYSIS

CRITERIA EXPLANATION
Accreditation The nature, quality and appropriateness of the analytical
procedure must be confirmed by accreditation to ISO 17025.
Twin-stream Details of the twin-stream system, preferably different analysts
(Independent on different days, and the measured reproducibility.
Parallel) analysis
Reference Whether the RMs are in-house or CRMs. In particular how the
Materials accepted values were obtained and verified.
Instrument The number of standards used, linearity of the calibration
calibrations range, reproducibility of the calibration, frequency of re-
calibration. Use of internal standards. Frequency of preparation
of the standards and their storage conditions. Source of the
primary standards.
QC procedures Use of QC samples, splitting limits between duplicates.
QA procedures Round-robin exercises.
Umpire laboratory Selection of the umpire laboratory, steps taken to maintain
quality of analysis.
Maintenance Maintenance contracts, maintenance records.
Fault reporting The procedure for reporting faults, their rectification and the
and rectification signing-off by management.

Exception Reports Reports on non-compliance with the Code must contain the
reasons for non-compliance, action plans to reach compliance
and be signed-off by the Competent Person.

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D.5. REPORTING

CRITERIA EXPLANATION
Metal Balance Desired constituents over the reporting period, timeously to
Plant Management and Financial Accountants
Key Performance Feed and product tonnages and grades; recoveries,
Indicators (KPI’s) accountabilities; reported against target figures; error levels of
all reported outputs; historical comparisons to assist monitoring
of long-term trends
Traceability To all sources of inputs
Data sources Manual entries to be minimised and automatic data collection
from SCADA or LIMS systems maximised
Preparation Adequately trained personnel, who understand source and
meaning of the inputs
Adjustments or Only with written authorisation of responsible person and
alterations recorded for review purposes
Mass balance Only via an approved procedure to identify inputs subject to
reconciliation illegitimate (spurious) errors, to determine bias and to facilitate
remedial action
Approval Reviewed and signed off by Metal Accounting Committee, or
equivalent, for subsequent approval by Audit Committee

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D.6. AUDITING

CRITERIA EXPLANATION
Compliance with Suitably trained outside of the area they are examining must
Code carry out audits. They must ensure that the requirements of the
Code as listed in Check Lists E.1. to E.6. have been adhered to.
Audit Types There are four types of audit:
Inspections by operating staff – These must be carried out
daily and should cover areas such as cleanliness, operational
problems and calibration.
Internal Audits – These must be carried out at least monthly by
supervisory staff or suitably trained staff from other sections.
External Audits – These must be carried out on a “surprise”
basis at least twice a year by suitably trained and qualified staff,
preferably including a financial auditor, who are independent of
the facility being audited, but more frequently if conditions of
bias or malpractice have been found. These audits must contain
both horizontal audits, where the auditor will examine in detail
single aspects of the quality system e.g. calibration, and vertical
audits, where the auditor will select a sample and follow its
progress from mass measurement to storage and/or disposal.
The management of stockpiles, especially any reduction to zero
or sudden change in process inventory, must be commented
on.
Stock-takes – These must be witnessed by an external audit
team and preferably be based on the bubble method.
Audit Reports Audit Reports should be based on pre-designed hard-copy
checklists, which must be retained as a record for at least 5
years. Recommended examples may be found in the Australian
Standard AS 4433.6 – 2000, for sampling equipment, and
CITAC/Eurachem Guide CG1 – 2002, for laboratories.
Non-Conformance Non-Conformance Reports must be issued, with appropriate
Reports comments, for each instance of non-conformance. The
appropriate operational management must comment on these
reports before they are submitted to higher management.
Exception Reports Exception Reports should be examined and any progress, or
lack of, on the elimination of problems commented on.
Metal Accounting The whole metal accounting system must be reviewed on at
Reviews least an annual basis by senior management to establish that it
is still fulfilling its function. The review findings must be signed-
off by the Audit/Risk Committee and endorsed by the
Competent Person.

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APPENDIX E – MASS BALANCING TECHNIQUES
E.1 SIMPLE EXAMPLE

(R.D.Morrison, private communication)

One objective of metal balancing calculations is to carry out calculations which can
utilise all of the available data. The calculation process will both expose
inconsistencies in the data and identify the likely source of the inconsistency. It will
also provide a way to link data from many sources, to integrate the data in a
structured manner and to provide a key source of tested, verified or certified
information which can be used as a basis for sound decision-making. The use of
redundant information will necessarily produce differences, raising the question as to
how these differences should be treated.

The following simple example illustrates the principles outlined in Section 7 using
unsophisticated mathematical techniques. The example is drawn from Morrison, Gu
and McCallum (2002).

This example demonstrates how a mass balancing problem can be solved in two
stages. Although it is not necessary to use a two-stage solution, it is often easier to
understand the process in two stages. The first stage estimates the best-fit values of
the flow rates. The second stage estimates the required component assay
adjustments which are compatible with the best fit flow rates. The second stage of
the process is also useful for Reconciliation to the mine or ore body where flow rates
may be well defined and assays only defined by an ore body model. In this case, the
adjustments are essentially an allocation of differences and they are not really a best-
fit solution – simply a check on plausibility.

The general problem looks quite daunting. It will first be defined and then a simple
example will be worked through for illustrative purposes.

The main aim of the balancing process is to achieve a set of self consistent stream
flows and assays, which are in some way a best estimate of the true situation. Self
consistent means that total ore and metal flows in and out of each node must be
equal to within specified numerical criteria.

Consider a flowsheet which has a number of streams indicated by subscript “i”. Some
stream masses “M” are measured over a specified time interval and some streams
are sampled and assayed for “j” assays “a”

For this problem, three kinds of numbers can be defined:

Actual assay and mass flow values which are perfectly self consistent but essentially
unknowable M i * and a ij * .

Measured values Mi for streams and aij for assays. These values are always
inconsistent.

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Measured values have a measurement variance or standard deviation σ or SD
associated with them. The glossary provides definitions as well as those for accuracy
and precision.

The adjusted data M i and aij may estimate the “true” value to within some defined
level. Adjusted data are the outcome of the balancing process.

It is important to have a realistic measure of experimental variance or standard


deviation for each measured value or Mi or aij .

It is also important to eliminate (or at least measure) bias within accounting balances.
This topic will be considered later.

The usual criteria for this method of analysis is to minimise the weighted sum of the
squares of the difference between each measured and adjusted value divided by our
estimate (standard deviation SD or σ ) of its accuracy. This value is usually called
the weighted sum of squares WSSQ.

There are two common ways to consider this problem. The simplest problem to solve
is to consider the differences between flows of ore and metals in and out of each
node.

In mathematical terms minimise

2
⎛ M - Mi ⎞
WSSQ = ∑ ⎜⎜ i ⎟⎟ for mass flows
i ⎝ σ Mi ⎠

⎛ (Μ i aij − Μ i aij )2 ⎞
+ ∑⎜ ⎟ for assay flows
⎜ a σ 2
+ Μ σ 2 ⎟
ij
⎝ ij Μ i i a ij ⎠

subject to the constraint that the flowsheet must add up for total stream flows and
component stream flows.

After finding the “best” flows, the adjusted assays can be recalculated.

Another standard approach is to minimise

2
⎛ aij − aij ⎞
WSSQ = ∑ ⎜ ⎟

ij ⎝ σ aij

where aij now refers to all measured mass flows and assays.

As before, adjusted data must be self consistent. That is, it must satisfy the
constraints imposed by the flowsheet network.

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There are many standard numerical methods which can be used to solve either
variation of the problem. A simple example using the first approach is provided in
Appendix E2. However more general solutions are beyond the scope of this note.

A general approach developed by Morrison is detailed in Lynch, 1977 Chapter 7.


Refer to Napier-Munn et al 1996, Chapter 5 for some worked examples. A more
detailed description of the balancing process is given by Richardson,1991 and
Richardson and Morrison, 2003

For our simple case, let us consider a separator which has a feed stream containing
mass A over a specified time period and which produces a concentrate B and a
tailing stream C.

As noted earlier, three kinds of numbers can be defined for this problem:

• Actual assay and mass flow values which are perfectly self consistent but
essentially unknowable A*,B* and C* and ai* , bi* and ci*

• Measured values A, B and C for streams and ai bi and ci assays. These


values are always inconsistent. Each measured value has an associated
measurement variance or standard deviation σ or SD. The measurement
variance can be estimated by repeated measurement or repeated sampling
and assay.
• Adjusted data A, B and C and a, b and c which may estimate the “true” value
to within some defined level. Adjusted data is the outcome of the balancing
process.

A B

The example process is a flotation bank. Each stream is sampled and assayed for
several metals. These assays are designated ai, bi and ci, where i represents one of
n components.

For any given feed-rate, the product flows can be ratioed to the feed rate to simplify
the calculation.

1 β

1-β
For perfect data:

ai* = β bi* + (1 − β )ci* (


which implies that β = ai* − ci* ) (b
*
i − ci* )

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This is the basis of the well-known two-product formula. It is worth noting that even
for perfect data, there is no useful balance around a splitter (or a separator which
does not separate) where a=b=c and then β is equal to zero divided by zero which
is undefined and can take any value.

For measured data, adding a component flow error ∆ balances the equation for a
given value of β

∆i = ai − β bi − (1 − β ) ci

To simplify the calculation, assume the standard deviation estimate (SD) for each ∆
is one. Then the weighted sum of squares is:

SSQ = Σ∆i2 = Σ ( ai − β bi − (1 − β ) ci )
2

If an estimate of SD is available for each component, it can be used to scale the error
for each component (i.e. divide each error by its standard deviation) and it makes the
answer a little more complicated, as is addressed later.

To find the minimum sum of squares, take the derivative of the SSQ with respect to
beta and set the answer to zero.

∂SSQ / ∂β = 2Σ ( ai − β bi − (1 − β ) ci ) ( ai − ci )

which simplifies to

β = Σ ( ai − ci ) Σ ( bi − ci )( ai − ci )
2

when the derivative is equal to zero.

(Note that a splitter which works as a splitter still produces Σ0/Σ0 which can take any
value.)

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E.2 NUMERICAL EXAMPLE

Considering a simple numerical example may clarify some aspects. As β is the only
variable, a direct search provides a way to consider dependencies in the solution.

Figures 1 and 2 show variation in the sum of squares for β values from 0 to 1 in
steps of 0.05 for the data shown in Table 1 below:

Sample Rougher Feed Rougher Conc Rougher Tail Beta


A B C 0.168
%Cu 2.92 6.9 1.9 0.204
%Pb 3.15 7.5 1.61 0.261
%Zn 6.6 27.4 2.7 0.158
%Fe 14.15 16.8 13.8 0.117
Table 1: β values for the component analyses

1000

100

10 %Cu
1 %Pb
SSQ

%Zn
0.1 %Fe
SSQ
0.01

0.001

0.0001
Beta 0-1

Figure 1: Sum of Squares vs β Values: Log axis

500

450

400

350
%Cu
300
%Pb
SSQ

250 %Zn
%Fe
200 SSQ
150

100

50

Beta 0-1

Figure 2: Sum of Squares vs β values: Linear scale

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The minima are well defined for each assay but they do not lie at the same value or
at the best-fit value of 0.168 from the equation above. However, no matter what SDs
are applied, the best fit value cannot move outside the range covered by these
minima. Clearly, if all of the estimates of beta β are essentially the same, the mass
split is well defined.

In mathematical terms, how well β is defined depends on how sharply the SSQ
curves at the minima. Hence, the assay (Zn) with the largest difference between feed
and products and the most accurate data (smallest SDs) will dominate the combined
results and produce the best estimate.

If the separation process encompasses the complete plant, the assay differences will
be larger than for any single separation and they will be better defined. In short, even
if the overall circuit balance is well defined, the internal balances may be poorly, or
not at all, defined.

It is clearly shown in Figure 1 that the smaller the SSQ at the minima, the sharper the
curvature and the better the flows are defined.

Data Adjustment

Given a “best” set of flow rates, the next step is to allocate the flow component errors.

As in the first stage, minimising the SSQ of the adjustments is a useful strategy. For
each assay at the best value of β , there is a mass flow error:

∆ i = ai − β bi − (1 − β )ci
If the small change required in each assay is defined as ∆ai , ∆bi and so on, then

0 = ( a − ∆ai ) − β ( b − ∆bi ) − (1 − β )( c − ∆ci )

and by difference

∆ i = ∆ai − β∆bi − (1 − β )∆ci

The objective function for each assay is

SSQ = ∆ai2 + ∆bi2 + ∆ci2

subject to the constraint that the adjustments add up to the required component error.
A standard technique to add a constraint to a minimisation is to use a Lagrange
multiplier λ for each constraint. The constraint equation must be arranged to equal
zero. Hence the modified sum of squares becomes:

SSQ = ∆ai2 + ∆bi2 + ∆ci2 + 2λ ( ∆ai − β∆bi − (1 − β )∆ci )

To find the minimum values, take the derivatives with respect to each adjustment and
the Lagrange multiplier and equate to zero.

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∂SSQ ∂∆ai = 2∆ai + 2λ = 0

∂SSQ ∂∆bi = 2∆bi + 2λβ = 0

∂SSQ ∂∆ci = 2∆ci + 2λ (1 − β ) = 0

∂ SSQ ∂ λ = 2 ( −∆ai + β∆bi + (1 − β )∆ci ) = 0

This yields four equations in four unknowns.

∆ai = −λ

∆bi = λβ

∆ci = λ (1 − β ) and substituting for each adjustment yields

(
λ = −∆i 1 + β 2 + (1 − β )
2
)
This implies that apportioning the error according to the flow rate is the least squares
solution when the SDs for each measurement are equal. This is intuitively reasonable.
If each assay has its own SD estimate, the algebra is a bit more cluttered but not
very different and the assay with the smallest SD is adjusted least.

Table 2 shows a set of adjustments at the best-fit mass split of 16.8% to concentrate.

This method gives a set of adjustments for any value of mass split. Therefore, the
numerical derivative of β with respect to SSQ can be taken and iterated to the best
solution. This solution will usually be close to the simply weighted analytical solution
detailed above. If the data is accurate, the minima will closely coincide and the two
methods will provide essentially identical solutions. In this case the solution will be
insensitive to different SD estimates.

As noted earlier, an estimate of the curvature at the minima of β provides an


estimate of how well the flow split is defined. The sum of all of the adjustments
squared in this case is 0.25

There are twelve measurements and four constraints in this case. Following the
comments in Morrison, Gu and McCallum (2002), an expected value of the SSQ with
good SD estimates would be 8 (i.e. 12–4).

Therefore, the measured data in this case probably has much smaller SDs than the
assumed value of unity for each.

A standard way to present this type of data is measured data (flows, assays or
component flows) against adjusted data. If most of the points lie along the diagonal
from zero, then the data and the adjustment procedure and probably working well.

All in all, the method of weighted least squares applied to the mass balancing
problem provides a great deal of useful information.

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Table 2: Adjustments for Assay Data

Component Feed Tails Concentrate Weighted Sum Adjustment


Adj. A, λ Adj. B, λ Adj.C, λ
% Cu -0.104523 0.017564 0.086959 -0.179821
% Pb -0.319849 0.053746 0.266103 -0.550269
% Zn 0.145597 -0.024466 -0.121132 0.250486
% Fe 0.089577 -0.015052 -0.074524 0.154108

Including measurement SDs in a least squares solution.

The weighted least squares case is a little more complex but follows the same path
as the data adjustment method.

If it is assumed that any measurement biases are small, then the required data
adjustments should be drawn from the probability distribution of variation associated
with each measurement as are the experimental or measured values – or at least a
very similar distribution. Therefore, on average, it can be expected that the weighted
adjustments ∆ ai σ ai , ∆ bi σ bi etc, have an average value of about one and the
weighted sum of squares (WSSQ) of adjustments have a value approximating the
number of measurements.

Hence, the magnitude of each weighted adjustment provides a good indication of


data consistency at each point.

The weighted sum of squares for each assay adjustment is:

WSSQ = (δ ai σ ai ) + (δ bi σ bi ) + (δ ci σ ci )
2 2 2

subject to exactly the same constraint as the unweighted case. That is

2λ ( −∆ i + ∆ai − β∆bi − (1 − β ) ∆ci )

is added to the sum of squares and minimise with respect to λ as well.

The derivatives are also quite similar. The adjustment is scaled by dividing it by the
SD.

∆ai = λσ ai2

∆bi = λβσ bi2

∆ci = λ (1 − β )σ ci2
The derivative with respect to the La Grange multiplier stays the same but the scaled
values are substituted back in to calculate it.

(
λ = − ∆i σ ai2 + βσ bi2 + (1 − β ) σ ci2
2
)
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NB the denominator for the LaGrange multiplier turns out to be an estimate of the
standard deviation (SD) for ∆ i Therefore, the mass flow error for each measured
component can be weighted and iterated to a weighted best fit value of beta. If the
data is even slightly reasonable, the unweighted estimate of beta cn be used as a
starting point and iterated to a stable solution. Obviously the component with the
largest change in value (between con and tail) and the lowest relative SD for ∆ i will
tend have a flow split very close to the best fit weighted beta.

If the mass has been measured for more than one stream, a weighted stream
adjustment can also be added to the weighted sum of squares. If only measured one
stream has been measured, the flow ratio can be used.

Even for this simple case, the analytical solution is quite complex and it is much
easier to use MS Excel and Solver to find the best values. In this case the weighted
SSQ for all components plus flows can be added together, if appropriate.

The objective for Solver to minimise is the total WSSQ.

There is only one flow split β but there is a λ for each constraint to identify as
variables for Solver to adjust to achieve the minimisation.

Evaluating the weighted balance


The important advantage gained by this additional complexity is that the expected
value of each adjustment is simply “one”. If the required adjustment is less than plus
or minus one SD, then there is a two thirds chance that the adjustment is within
measurement variation. If the adjustment lies outside plus or minus two SDs, then
there is very likely to be a problem in the data and that adjusted data point is where
to start looking at measurement or assay.

However, if the adjustments all lie within plus or minus two SDs, the adjusted balance
is probably as good as can be expected – subject to the checks for bias outlined next.

If the measurement and balancing process were to be repeated many times, the
adjusted data can be expected to exhibit a lower variance than that of the measured
data. For some examples see Deglon and Chakraborty, (2005).

Hence, the adjusted data can be compared with those to be used any Check in-
Check out strategy. If the data adjustments for the streams and masses which are
part commercial transfers, the Check in-Check out values can be assigned a very low
variance and the weighted adjustment procedure run again to derive a set of data
which are both technically self consistent and consistent with commercial value
transfers.

This approach can also integrate the primary and secondary data strategy used by
some precious metal operations.

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Detecting Bias
One of the disadvantages of using least squares adjusted data is that the adjustment
process can make some types of bias more difficult to detect. However, it helps to
identify some other types.

In general, the detection of bias requires examination of a number of accounting


periods. The classical approach is compare cumulative sums (or cusums) of masses
and component masses entering and leaving the system. Over an extended period
(weeks to months) the contribution made by a bias will grow while the random errors
should be both positive and negative and tend to cancel out as the sum accumulates.

Calculating cusums monthly or quarterly should be a standard component of any


metal accounting strategy. However, they are always “after the fact”. The least
squares analysis can often be used (if there is enough redundant data) as a problem
detector over a shorter time frame.

For example, if the multi-assay based mass split estimate is highly self consistent
and does not match the measured mass split, then each mass measurement system
needs to be checked. Mass measurement systems can very easily acquire bias due
to a build up of material on a weigh frame or a simple fault (such as idler wheel slip)
in belt speed measurement.

Allowing a sample to lose moisture between collection and measurement is another


way to introduce a bias.

For multiple mass or multiple stream cases, in any single data set the data
adjustment procedure will distribute both random variation and bias in one
measurement across others of the same type which share the same constraint.
However, over several data sets the biased measurement can be expected to require
more adjustment in a particular direction than measurements which only exhibit
random variation. In an unbiased system (where the measurement distribution is also
symmetrical), the arithmetic sum of the weighted adjustments should be close to zero
for each set and approximate zero when any selected data point is considered
across multiple data periods. This is most easily checked graphically as many
adjustment can be examined using a single trend graph.

A yet more sophisticated technique is to add a “fittable” bias to a suspect


measurement and repeat the analysis process across a sequence of data sets. This
technique is plausible for one suspect measurement but applying it to several
measurements can easily lead to serious self deception.

To be detectable at all, a bias must persist long enough for its accumulated effect to
be larger than measurement or balanced data variance. A so called “variable bias” is
a system measurement problem and is not correctable by any mathematical
technique – the underlying measurement problems simply must be rectified.

The best way to guard against “variable bias” is for the person responsible for metal
to visually inspect each mass measurement and sample point at least several times
per week - daily if possible. Mathematical massaging can only conceal these
problems when many of them are very easy for a trained eye to “see”.

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In Conclusion
These methods provide a powerful way to analyse metal accounting data and to
detect certain problems.

The adjusted data provide a self consistent set which can be used to calculate key
performance indicators such as metal recovery in a consistent manner – no matter
which adjusted data is selected as the basis of the calculation.

A second stage of adjustment can be used to align commercial and technical data –
when and only when the data have been fully analysed and the hypothesis that the
only variation is statistical is well supported.

This technique also allows data from many sources within a processing system to be
integrated for performance analysis and reporting.

These methods are powerful but should be supported by cusums of total mass and
key components to detect bias.

Last but not least, regular physical examination of each measurement and sample
point will detect many problems that mathematical techniques will not.

RICHARDSON, J. M. and MORRISON, R. D. (2003). Metallurgical Balances and


Efficiency. Principles of Mineral Processing. M. C. Fuerstenau and Han, K. N. E. pp
363-389, SME, Littleton , Colorado, USA.

Chakraborty A and Deglon D, 2006. Measurement Network Design For Metallurgical


Accounting: A Heuristic Methodology. In Proceedings MPMSC Conference, Sudbury
6–7 June.

Bepswa, P, Deglon, DA and Chakraborty, A, 2006. Heuristic methodology for


designing measurement networks for metallurgical accounting. In Proceedings of
XXIII International Minerals Processing Congress, Istanbul, 3-8 September

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E.3 SAMPLING, METALLURGICAL ACCOUNTING AND REDUCTION OF
BALANCE ESTIMATION VARIANCE

GJ Lyman, AusIMM, Sampling and Blending Conference, Sunshine Coast, QLD 9-12
May 2005

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Sampling, Metallurgical Accounting and Reduction of Balance
Estimation Variance
G J Lyman1

ABSTRACT INTRODUCTION
A metallurgical balance drawn around a mineral processing plant or Large metallurgical processing and refining operations are
smelter must involve all process streams crossing the plant boundary. increasingly concerned with the measurement of their
Modern sampling theory, as formulated by Gy, and sound statistical performance. The availability of powerful on-line measurement
method can be used to determine the uncertainties in the observed assays systems, cheap networked computing power and the ability to
for the set of balance analytes and in the mass flow rates of the process
manage large databases of information collected across the
streams for the balance period. These uncertainties can then be used
together with the material balance equations to arrive at adjusted operation make it possible to construct systems that a manager
component mass flows that satisfy the material balances exactly. To can use to view and analyse any part of the operations at a range
determine whether or not the data is consistent with the level of of scales or levels.
uncertainty in the data and with the material balance equations, a The determination of a material balance around an operation is
goodness of fit test is applied. This goodness of fit criterion is the the most fundamental calculation that can be carried out, but
principal tool to quantify the quality of the material balances. balances and recovery estimates are subject to uncertainties that
The mathematical structure of the statistical material balance problem derive from uncertainties in the measured assays and mass flows.
poses a number of challenges. For example, while the variances of the For high value materials, balances with the corresponding
adjusted component mass flows do not vanish, the variances of the sums statistical analysis may also be used to evaluate the possibility
of the adjusted component mass flows about each balance node do
vanish, simply because the balancing computation demands that the
that theft of material from the process has taken place, if all the
balances close exactly. Even though it can be shown that the variances of measurement processes are well-understood and controlled
the adjusted component mass flows are always lower than the estimates throughout the balance period.
for the corresponding unadjusted component flows, it is still not possible The method of calculating a balance around a particular
to construct a confidence interval on the component mass flow into (and metallurgical operation is usually one that has evolved over time.
out of) a balance node using the adjusted component flows. On the face It is common to find that the balance calculations rely on
of it, such a confidence interval is exactly what is most desired from the
‘assumptions’ about the characteristics of some of the process
balance calculations. The problem arises because the balance problem is
a data adjustment rather than a parameter estimation problem. streams or stock levels within the process. The common origin of
It is possible, however, to calculate the recovery of a component to a
the assumptions is a missing or unreliable sample for the
product stream and determine a confidence interval for the recovery particular process streams or a mass flow measurement that is
value. It is also possible to calculate an uncertainty in the mass flow of considered unreliable, that is, of high variance. For example, the
any balance species in any process stream, before and after balancing. moisture content determination of the material may be deemed
Balance results have little meaning without the confidence interval unreliable and therefore an ‘historically determined’ or ‘agreed’
estimates. Having invested in the manpower and procedures that make a figure for the moisture is used in the calculations. The impact of
statistically valid balance on an operation possible, the management may the assumption is usually unknown.
find that the levels of uncertainty associated with the balances are rather
The traditional methods of balancing also tend to rely upon or
higher than they would like. The obvious solution to the wide confidence
intervals is to reduce the uncertainty in the assays and mass flow rates on focus upon a single chemical or physical species in the
the principal process streams. The cost of this uncertainty reduction may calculations. There are generally two reasons for this. First, the
be quite significant, as it will involve reduction in analytical variances or target species is the one of primary value and second, the use of a
reduction in sampling and preparation variances which may require single species avoids the disconcerting fact that balances based
investment in and development of new sampling hardware or routine on additional species may provide different results and the
duplication of assays to reduce the assaying variance. technically appropriate method of reconciling the results of the
A second strategy for uncertainty reduction can be proposed which disparate balances is not known to the staff of the organisation.
involves the use of additional sampling points to provide material balance
nodes internal to the processing operation. The information required to If an operation has developed a corporate and economic
make these internal balances may well exist within the operation, but it justification for carrying out technically correct material balances
may not be recognised as being of value or the standard of sampling and on an operation, it is necessary to review all sources of data that
assaying may not be deemed to be sufficient to use the data for are used in the balance calculations and then eliminate the
metallurgical accounting purposes. The marginal cost of elevating the ‘assumptions’ involved and replace them with statistically sound
existing sampling systems to metallurgical accounting standards may statements of the uncertainties involved in the measured
well be smaller than that to improve the sampling and assaying on the quantities. The review of the data must scrutinise all sampling
boundary streams.
and analytical procedures that are used to acquire information
This paper presents a statistical analysis of an uncomplicated form of and develop realistic descriptions of the uncertainties involved in
the balance calculations that permits exploration of accuracy issues and
the advantages that come from additional internal balancing nodes for the
all measurements. Ideally, the total variance will be divided into
process flow sheet. The calculations are based on a relatively simple flow two components, the first due to due sampling and preparation
sheet of common structure, but are of general applicability. The objective and the second due to analysis. It is usually necessary to review
is to reveal broad issues. While each process flow sheet and sampling and the operation of the monitoring systems that are in place to
analysis system requires individual analysis to reveal precisely where the ensure that sampling systems functioned as required and that
gains can be made most economically, a general result can be laboratory quality control systems remained in place during the
demonstrated which provides an estimate of the limit to the variance balance period. Ensuring that a large analytical facility carrying
reduction which can be achieved by adding internal balance nodes.
out diverse assays operates within specification accuracy on a
routine basis is a great challenge that demands the goodwill,
1. Sampling Consultant, 17 Diosma Street, Bellbowrie Qld 4070. cooperation and diligence of a large team of skilled persons.

Sampling and Blending Conference Sunshine Coast, QLD, 9 - 12 May 2005 127
G J LYMAN

Competently carried out, the review will usually identify While the theory behind SMB that permits the optimal
effective means of actually increasing the amount of information estimation of balances can become very complex in a general
that can be extracted by the balances. The traditional view of a case and particularly when some uncertainties in assays or mass
mechanical sampler defines it as a device for acquiring a flows do not follow Gaussian (normal) distributions, it can be
representative sample of the material flowing past it; the sample quite simple in some cases and can be used to very great
is sent for analysis to determine the content of various analytes advantage to estimate how accurate balances will be, given the
of interest and the analyte contents are used in the balance level of uncertainty in the data going into the balance and the
calculations. However, as Gy has pointed out many times, a structure of the balance. It can therefore be used to investigate
correct mechanical sampler will also operate in such a way as to alternate balance structures and data quality scenarios and the
provide a sample whose mass is proportional to (that is, quality of the information that will arise from the balance. The
representative of) the total mass of material that passed the theory behind SMB in fact provides a design tool for sampling
sampling point during the period of sampling. The use of and material balance networks. A metallurgical operation would
mechanically correct sampling equipment to determine mass certainly not invest in a new process without making substantial
flow estimates is a means of acquiring information that continues efforts to determine the quality of product it will ultimately
to be grossly overlooked. provide. However, operations often construct sampling and
material balance systems without an appropriate understanding
The review of the sampling systems in place and the data of the quality of the data that will be produced.
available for balance calculation has to be linked to a
This paper has the objective of showing how the simplest SMB
consideration of how the balances should be calculated. In the
theory can be used to estimate the quality of the balance results
simplest case, where all inputs, outputs and changes in stock
that will be obtained, prior to any final decision on a sampling
levels are to be reconciled over an accounting period (month or system and material balancing system design. A simple case is
quarter, say) the structure of the balance is fixed and it remains to studied in which all uncertainties are assumed to follow Gaussian
decide which species will be used in the balance and whether or distributions. The scenario is one in which an overall balance on
not certain mass flows will be computationally estimated at the an operation is needed, but an option exists to include internal
same time as the mass flow rates and/or assays are adjusted to process balances in the SMB calculations. The statistical
provide an exact closure of the balance. advantage that can be obtained by including the internal balances
It would be unusual to find that all the sampling systems and in the calculations is quantified. This scenario is one that is
data monitoring procedures needed to provide the data for a accessible to many operations and the marginal cost of reducing
complete and statistically sound balance were already in place. It sampling variance for the perimeter streams may be far higher
would also be surprising if all systems provided data with than making relatively simple changes in procedures and taking
uncertainty levels that were deemed acceptable. Most operations advantage of samplers that already exist for the internal process
have no quantified knowledge of the accuracy of their sampling streams.
and assaying; the determination of the accuracy of sampling The flow sheet chosen for consideration is also a simple one
is a prerequisite to deciding how to best use the data that but one that is common to flotation as well as smelting
arises from the sampling. An understanding of the constitutional operations. Structurally, it corresponds to the flow sheet that was
and distributional heterogeneity of all process streams at the employed at Bougainville Copper in their flotation circuit
range of levels of comminution involved in the sampling and (Hinckfuss, 1976) and is also a common smelting flow sheet in
analysis for all analytes of interest is not common. which final slags are retreated to recover entrained values. The
Faced with the problem of enlarging the sampling system and flow sheet is shown in Figure 1 together with the stream
doing something to decrease the levels of uncertainty in the data, numbers, process deportments and nominal balance data. For a
the best way of investing in equipment or additional analyses smelting flow sheet, stage 1 corresponds to a furnace producing a
may not be immediately obvious. For some process streams, matte and slag, stage 2 corresponds to a converting process and
there will be little choice; a new sampler will have to be stage 3 to a converter slag scavenging process, recycling a matte
installed. However, the sampling frequency to be employed for material to the converters. The mass flow basis is 100 units of
mass input. In order to keep the problem simple, internal
that stream will dictate the accumulated primary increment
accumulation in the process has been ignored. Stock build-up or
masses and the need for more or less expensive sample handling
drawdown can have a dominant impact on balance variances
equipment and secondary or tertiary sample division at the
when not determined with adequate accuracy.
sample point. The sampling frequency used will also control the
variance component due to distributional heterogeneity (DH),
and, if the material sampled has a high intrinsic (constitutional) STATISTICAL DEVELOPMENT
heterogeneity with respect to analytes of interest, the variance
due to intrinsic heterogeneity (IH) may be important as well. Data model
Statistical material balance (SMB) methods, in which all
The development of a statistical model of the data is the first step
available data are used and are weighted in the calculations
in any statistical analysis problem. The problem considered here
according to their accuracy, have two advantages over traditional
is taken as one in which the processing operation receives
ad hoc balance calculations. First, the method provides a balance
consignments of feed material on a daily basis and a daily
that closes exactly for all species and mass flows involved and
composite sample is prepared for assay. Daily dry solids inputs
second, SMB permits the statistical interpretation of the data and
are determined from a wet tonnage delivered and a moisture
the results of the calculations. In particular, it is possible to
determination on the as-received solids. Outputs are similarly
determine confidence intervals or even full statistical
determined, using daily or weekly composites or assays and
distributions for computed results, where the variables of interest
weights of final product (stream 4) consignments. To keep this
have not had their variance suppressed by the balance
case simple, build-up or draw-down of internal stock of
calculations. It is possible to quantify, for example, the
in-process material will be ignored. Accounting for these stocks
probability that the output of valuable exceeded the balance
would modify external flows and add some internal flows.
value by a given number of grams, ounces or tonnes. It is also
possible to quantify the probability that the recovery of SO2 to At the end of the month, the net input of a species is a sum
the scrubbers fell below a target figure. over the periodic inputs and the net output is a similar sum over
outputs.

128 Sunshine Coast, QLD, 9 - 12 May 2005 Sampling and Blending Conference
SAMPLING, METALLURGICAL ACCOUNTING AND REDUCTION OF BALANCE ESTIMATION VARIANCE

Stage 1 (Rougher)
1 Rec. to 98.00% 2
Conc. 80.00%
Species mass conc 40.00% mass conc
1 1.000 1.00% 10.00% 0.020 0.02%
2 11.000 11.00% 3.00% 2.200 2.64%
3 12.000 12.00% 1.00% 7.200 8.63%
4 13.000 13.00% 11.700 14.03%
5 5.000 5.00% 4.850 5.82%
6 58.000 58.00% mass conc 57.420 68.86%
100.000 100.00% 0.980 5.90% 83.390 100.00%
8.800 52.98%
4.800 28.90%
3 1.300 7.83%
0.150 0.90%
0.580 3.49%
16.610 100.00%

mass conc mass conc


1.086 4.55% 0.106 1.46%
10.173 42.59% 1.373 18.87%
10.435 43.68% 5.635 77.43%
1.429 5.98% 7 0.129 1.77%
0.155 0.65% 0.005 0.06%
0.610 2.55% 0.030 0.41%
23.888 100.00% 7.278 100.00%

Stage 2 (Cleaner) Stage 3 (Cleaner Scavenger)


Rec. to 90.00% 5 Rec. to 98.00% 6
Conc. 85.00% Conc. 90.00%
40.00% mass conc 90.00% mass conc
10.00% 0.109 1.09% 10.00% 0.002 0.08%
1.00% 1.526 15.36% 3.00% 0.153 5.75%
2.00% 6.261 63.04% 5.00% 0.626 23.59%
1.286 12.95% 1.157 43.60%
0.153 1.54% 0.148 5.59%
mass conc 0.598 6.02% 0.568 21.39%
0.978 7.01% 9.932 100.00% 2.654 100.00%
8.647 61.96%
4 4.174 29.91%
0.143 1.02%
0.002 0.01%
0.012 0.09%
13.956 100.00%

FIG 1 - Process flow sheet for balances, with process unit species deportments and balanced mass flows and concentrations.

When internal flows are also to be taken into account, a similar The measured assay for species k on day i and in stream j is
accounting procedure is common. For example, in a smelting denoted as aijk . The uncertainties in the mass flows are µ ij and
circumstance, furnace matte would be sampled when tapped and in the assays, α kij .
then weighed as charged to the converters; if granulated, it can be Sampling theory combined with knowledge of material IH and
readily sampled and weighed as it is conveyed to the holding DH and testwork can be used to quantify the uncertainties. In the
bins ahead of the converters. In a flotation operation, the ideal present circumstances, these uncertainties will be taken to have
means of determining the mass flows is proportional sampling of Gaussian distributions with zero mean (unbiased sampling and
the slurry streams, with daily or shift samples for assay. For the assaying). The statistical properties of the uncertainties are then
sake of discussion, daily composites and monthly balances completely described by the variance and covariance of the
(30 days) will be assumed. random quantities. Because a species mass flow for the month
This mode of material movement and sampling is modelled by depends on both assays and daily lot masses, all monthly species
measured masses of daily flows denoted by mij for stream j and mass flows within a given stream will be correlated and all
day i. The total measured mass flow of the process stream j over species flows in that stream will correlate with the total mass
the month is then Mj: flow. However, daily mass flow measurement uncertainties will
not tend to correlate with assay uncertainties unless the process
Nj stream assay correlates strongly with the mass flow and the
M j = ∑ mij (1) primary sampling frequency is lower than dictated by sound
i=1 sampling system design.
On the above basis, the monthly total and species mass flows
where: can be written as:
Nj is the number of daily lots involved for the stream Nj

The total mass flow of species k over the month for stream j is M j = ∑(m
~ +µ )
ij ij
given by: i=1 (3)
j N
~
Nj = M j + ∑ µ ij
A kj = ∑ mij aijk (2) i=1

i=1

Sampling and Blending Conference Sunshine Coast, QLD, 9 - 12 May 2005 129
G J LYMAN

Nj

Aijk = ∑ ( m
~ + µ )( a~ k + α k ) MkT is the transpose of a column vector of the flow of species k
ij ij ij ij
i=1
in process streams 1 to Ns
(4)
~
N
j A tilde will again be used to denote the true values, no mark
= Aijk + ∑ ( m
~ α k + a~ kµ + µ α k )
ij ij ij ij ij ij will be used to denote the measured values and the statistically
i=1 adjusted values will be denoted by a caret (^). To write the
material balances concisely, an expanded version of the C matrix
where mathematical symbols with a tilde (~) denote the true, and is needed. Construct an ( N c + 1)( N n ) × ( N c + 1)( N s ) matrix,
thus unknown, value of a flow or assay and Greek symbols where Nn is the number of balance nodes or rows of C, by
denote discrepancies of observed values from true values. The locating copies of the C matrix down the diagonal and call this
variances of the monthly total and species mass flows are then: matrix G:

{ }= N σ
Var M j j
2
µj (5) C
0
0 0 0
C 0 0
G=  (11)
and 0 0 O 0
0 0 0 C

{ }= N m 2 σ 2 + a k
( )σ + σ α2 k σ µ2 j 
2
Var A kj 2
(6)
j
 j α j j µj

k
j

The material balance that is to be satisfied is then:


and it has been assumed for convenience that all daily flows and
Gz$ = 0 (12)
assays can be taken to have average values m j and a jk without loss
of significance of the calculations. The daily mass flows are
assumed to have nominally equal variances of σ 2µ j and the assays The vector of adjusted mass flows is the sum of the measured
flows and adjustments ξ:
similarly nominally equal variances of σ 2α k . This assumption is not
j
necessary; it simply makes the notation less cumbersome. The
covariance between the total mass flow and the species mass flow z$ = z + ξ (13)
is:
Note also that the true values must satisfy the material balance
equations so that Gz~ = 0.
{
Cov M j , A k
j }= N a σ j
k
j
2
µj (7)
Method of determination of optimal adjustments
and between the species mass flows is:
The best method of determination of the adjustments to the mass
flows is the method of maximum likelihood (ML). This method
{
Cov A , A k
j
l
j }= N a a σj
k
j
l
j
2
µj (8) finds adjustments from knowledge of the probability
distributions of the measurement uncertainties. The particular
Note that the species mass flows remain correlated even if a advantage of ML methods is that, when the data set is large
balance on total mass flow is not included in the calculations. enough (and this fact can be easily checked by Monte Carlo
simulations of the data structure), the ML estimators are
unbiased and have the lowest variance of any estimator that
Material balance model might be reasonably constructed. When all uncertainties in the
The material balances are conveniently captured by a matrix C data are normally distributed (Gaussian), the ML estimators are
(connection matrix) which has number of rows equal to the the same as the weighted least-squares estimators.
number of material balance nodes and number of columns equal Having assumed Gaussian data, the least squares solution to
to the number of process streams involved in the balance. In each this adjustment problem is optimal.
row, an element is one if the stream flows into the node and -1 if The next step is to construct the data covariance matrix Σ for
it flows out of the node. The elements are otherwise zero. all the process mass flows. Given the way that the vector z is
The simple balance around the flow sheet of Figure 1 would constructed, the covariance matrix will be banded as illustrated
first require renumbering of the streams from 1 to 4 (change 4 to figuratively in the next equation. Each submatrix has Ns rows and
3 and 6 to 4). The C matrix for this case has one row with entries columns.
[1 – 1 – 1 – 1] whereas balances around each stage of the process
(with stream numbering as on the Figure) has three rows: total flows species 1 species Nc

1 −1 −1 0 0 0 0 

C = 0 0 1 −1 −1 0 1 
total flows
(9)
 

0 0 0 0 1 −1 −1

To deal with all the material flows at once (total flow and
species flows), it is convenient to adopt a more compact notation. … species 1

All mass flows are put into a vector z such that: =

z T = [ M T M 1T M 2T K M N c T ]

(10)

where:
species Nc
MT is the transpose of a column vector of total process flows in

streams 1 to Ns

130 Sunshine Coast, QLD, 9 - 12 May 2005 Sampling and Blending Conference
SAMPLING, METALLURGICAL ACCOUNTING AND REDUCTION OF BALANCE ESTIMATION VARIANCE

The weighted least squares formulation requires minimisation therefore subject to less uncertainty than the measured values.
of the quadratic form ξ T Σ −1 ξ, subject to the requirement that For a scalar function of the adjusted flow rates, f ( z$ ), such as a
Equation 12 be satisfied. It is also useful to note that: recovery value, the variance of the function is, approximately:

δ = Gz (14) Var{ f } = ∇f T Σ a ∇f (21)

is a vector of the extent to which the measured values fail to This expression is exact only if the function f is linear in the
satisfy the material balance and is called the vector of node assay adjusted mass flows; ∇f is the gradient vector of the function f.
residuals. Equation 12 is then: Equation 20 shows that the covariance matrix depends only on
the structure of the material balance as captured by the C matrix
Gξ = −δ (15) and the uncertainties in the measurements. The covariance of the
results does not depend on the particular values of the measured
The minimisation of the quadratic form subject to the above mass flows as long as the covariance matrix of the measurements
linear constraints is solved by the method of Lagrange multipliers does not change greatly as the mass flows change. For a
and has a linear solution. The solution is: processing operation that does not have large variations in
relative process species mass flows from one month to the next,
ξ = − ΣG T (GΣG T )−1 δ (16) the covariance matrix of the adjusted values is, to a first
approximation, constant.
If the measurements are unbiased, this result is unbiased. This last result is very significant as it means that once
realistic estimates of the uncertainties in the mass flow and assay
Statistical results measurements have been established, it is possible to study
various balance configurations to see which configuration
It is not difficult to demonstrate that:
provides the greatest reduction in variance between the measured
and adjusted mass flows. While the calculations above may seem
Cov{δ} = E{δδ T } = (GΣG T ) (17) to be daunting, they are actually trivially simple in comparison to
the task of establishing the real measurement accuracies for the
The operator E{} denotes the statistical expectation of the process streams.
quantity.
In the context of this paper, the above result will be used to
Note that this covariance is that of the node assay residuals study the impact of balance configuration and the influence of
before data adjustment. The covariance of the node assay measurement accuracies in key process streams on the accuracy
residuals after adjustment is identically equal to zero. The of adjusted species flow estimates.
method of solution forces the adjusted node assay residuals to be
zero regardless of the data and the outcome of every calculation
is zero node assay residuals. CASE STUDY
The covariance matrix of the adjustments to the mass flows is:
Data adjustment
Cov{ξ} = E{ξξ T } = ΣG T (GΣG T )−1 GΣ (18)
The figures used for the deportments of the species are entirely
fictional but have been developed to include both ‘gangue’ or
and the minimal value of the weighted sum of squares is: ‘slag components’ and valuables in the balances. Table 1 proves
the deportments and comment on the nature of the species it is
WSSQ = ξ T Σ −1 ξ = δ T (GΣG T )−1 δ (19) intended to represent. The species represent a range of
deportments including one that is not well separated in stage 1
This quantity depends on the data and is therefore a random and 2. Species 6 is a mixture of elements for which no assay is
variable. It can be shown to have a chi-squared distribution with determined; it can be regarded as the ‘balance of the sample’.
N n ( N c + 1) degrees of freedom. This fact can be used to carry out
The nominal measurement relative standard deviations for
a test of goodness of fit of the data to the mass balance equations.
If this test fails, it means that either the data do not obey the either total mass flow or analytes one to five within a daily
balance equations or the estimates of the measurement variances sample are provided in Table 2. The figures given are
are incorrect. This test is the principal means by which to percentages and are realistic in the author’s experience.
evaluate the quality of the data and the validity of the balance. To ensure that the estimate of the covariance matrix originates
The weighted sum of squares can be partitioned into components from a realistic data set, that is, one on which the balances do not
due to each species to determine the contribution of each analyte close exactly the base data from Figure 1 were perturbed
to the total. according to the monthly variances and covariances.
Finally, the covariance matrix of the adjusted mass flows is The balance based on all seven streams and three balance
given by: nodes and the first five species leads to the variance estimates of
Table 3. The inclusion of the all six species in the process stream
Cov{z$} = Σ a = Σ − ΣG T (GΣG T )−1 GΣ (20) would lead to a singular solution to the balance, as the sum of all
species must always equal the total mass flow. To determine the
This equation shows that the variance of the adjusted mass mass flow of the last species, the five balance species are
flows must always be less than that of the measured flows as the subtracted from the balanced total mass flow.
matrix being subtracted is a positive definite covariance matrix. To ensure that the estimate of the covariance matrix originates
The fact that the covariance of the adjusted values is a simple from a realistic data set, that is, one on which the balances do not
difference between the covariance matrix of the observed values close exactly the base data from Figure 1 were perturbed
and the covariance of the adjustments is a consequence of their according to the monthly variances and covariances and when
statistical independence which derives from the general structure this perturbed data set was re-balanced, it was taken to be the
of linear least-squares problems. The adjusted mass flows are true base case.

Sampling and Blending Conference Sunshine Coast, QLD, 9 - 12 May 2005 131
G J LYMAN

TABLE 1
Species, deportments and comment.

Species Deportment to product Comment


Stage 1 Stage 2 Stage 3
1 98 90 98 Primary valuable, well recovered to the product stream and closely associated with secondary valuable
2 80 85 90 Secondary valuable, quite well recovered to product
3 40 40 90 Neutral species not well separated in stage 1 and 2 but recovers well in cleaner scavenger
4 10 10 10 Low level gangue or slag component moderately rejected to waste
5 3 1 3 Minor gangue or slag component well rejected to waste
6 1 2 5 Major gangue or slag component strongly rejected to waste in stage 1 and 2

Estimation of component recovery


TABLE 2
Because the balance is calculated in terms of the component
Relative standard deviations of daily mass flow and assay mass flows, the calculation of a recovery figure is simply the
measurements. The tabulated figure is a percentage.
ratio of the mass flow in the product stream to that in the
incoming stream and the uncertainty in the recovery can be
Component Stream determined by application of Equation 21. For the balance with
1 2 3 4 5 6 7 internal nodes, stream 4 is the product stream carrying the
Total mass 2.5 5.0 3.0 2.2 2.1 5.1 3.2 species of primary interest (species 1). Species 2 is also of
interest and species 5 is of interest in terms of its recovery to
1 6.1 10. 5.1 4.1 6.0 12. 6.0
waste streams.
2 5.2 6.1 4.1 4.0 5.1 5.0 5.0 Table 5 provides the recoveries and their uncertainties for the
3 5.9 5.9 4.9 5.1 5.9 4.0 5.0 species and streams noted. The recovery values for both balance
4 3.1 3.1 3.0 5.9 6.0 3.1 3.1 types are very similar, and in all cases the standard deviation of
the recovery estimate is smaller when the three node balance is
5 5.1 4.9 6.1 7.0 5.0 5.1 6.9
used. Only in two cases do the extra nodes in the balance
substantially decrease the uncertainty in the recovery values.
The recovery of the primary valuable species (1) to product
The results of perturbing a base set of data by adding (stream 4 or 3) is determined with apparent great accuracy and
appropriately correlated random components of a prescribed the accuracy does not improve very much at all when the more
covariance structure and re-balancing the data in a least squares complex balance is used. It is only the gangue (5) recoveries to
sense are provided in Table 3. The perturbed values are called waste (stream 2) and to product (stream 6) that benefit
‘measured values’. The full covariance matrices for each stream significantly from the more complex balance.
are not provided. Instead, the square root of the diagonal However, it is important to realise that it is not the accuracy of
elements of Σ, the standard deviations of the measured the recovery that is the critical quantity. If the mass flow of the
component flows (SDM) are provided both as absolute values component in the feed stream were known with absolute
and relative values (RSD as a per cent) are given. At the same certainty, the recovery uncertainty would be the critical figure.
time, the calculated standard deviations of the adjusted assays But the feed stream mass flow carries an uncertainty, so the
(SDA) can be determined from Equation 20 and tabulated as quantity of interest to the metallurgist is actually the uncertainty
well. The last column of Table 3 provides the ratio of the in the mass flow in the product stream. For species 1, this
variance of the adjusted flow to that of the unadjusted component uncertainty for the overall and three node balance are found
flow. This figure is the measure of decrease in the component within Tables 4 and 3. In both cases, the RSD for the measured
flow uncertainty that can be attached to the mass balancing flow in the product stream (3 or 4) is the same, but the adjusted
procedure. Ideally a balance procedure would reduce this ratio to mass flows show RSDs of 0.37 per cent and 0.30 per cent for the
zero but, here, the average ratio is ~0.5. Note finally that the one node and three node balances, respectively. This represents a
WSSQ value for the adjustment is 14.2, with an expected value 20 per cent reduction in SD or a 36 per cent reduction in
of 18, which leaves no doubt that the material balance equations variance.
are satisfied.
Table 4 provides the corresponding results for a single overall Sensitivity of results to measurement uncertainty
balance. The adjusted component flows for the perimeter streams and flow sheet structure
are essentially identical. Note that the stream numbering has
To determine the sensitivity of the balance to the accuracy of the
changed: change four to three and six to four.
measured values, consider a doubling of the standard deviation
However, in this case the reduction in variance from the of the all measurements on the internal streams. When the full
measured uncertainties to the balanced component flows is only three node balance is carried out, one might expect the balance to
30 per cent rather than 50 per cent. be degraded by the low precision data. On average, this is what
While the variance reduction has been calculated from theory, takes place, as the average variance reduction remains as it was
a Monte Carlo study involving the repetitive perturbation of a for the initial balance at about 50 per cent (Table 3; average
base data set followed by adjustment of each of the data sets variance ratio). Figure 2 plots the variance reduction ratios that
would lead to precisely the same result in the variance reduction. arise as a result of the balancing process. It is clear that some
Such an exercise is not difficult but is unnecessary in a case of variances are degraded while others are improved. However, the
weighted least-squared data adjustment, which is an entirely average variance reduction ratio, as previously stated, remains
linear problem. the much the same.

132 Sunshine Coast, QLD, 9 - 12 May 2005 Sampling and Blending Conference
SAMPLING, METALLURGICAL ACCOUNTING AND REDUCTION OF BALANCE ESTIMATION VARIANCE

TABLE 3
Results for least squares adjustment of component flows with variances using three balance nodes. The WSSQ value is 14.2 and the
average variance ratio is 0.49.
Stream Flows Measured Adjustment Adjusted SDM RSD (%) SDA RSD (%) Var ratio
1 mass 99.5172900 0.3584135 99.8757040 0.4542322 0.45 0.3624343 0.36 0.64
1 0.9975235 0.0070499 1.0045734 0.0120095 1.20 0.0049690 0.49 0.17
2 10.8411280 0.1105074 10.9516350 0.1142302 1.04 0.0533312 0.49 0.22
3 11.9086810 0.1365811 12.0452620 0.1393566 1.16 0.0794091 0.66 0.32
4 12.9694230 0.0134608 12.9828840 0.0943178 0.73 0.0694370 0.53 0.54
5 4.9862954 0.0143167 5.0006122 0.0517201 1.03 0.0373300 0.75 0.52
2 mass 83.6325490 -0.3799723 83.2525770 0.7634572 0.92 0.3581939 0.43 0.22
1 0.0208311 -0.0000987 0.0207324 0.0004256 2.05 0.0003917 1.89 0.85
2 2.2212457 -0.0142280 2.2070177 0.0320104 1.45 0.0265272 1.20 0.69
3 7.3236451 -0.0687750 7.2548701 0.1034831 1.43 0.0759617 1.05 0.54
4 11.7113400 -0.0260468 11.6852930 0.1258338 1.08 0.0692866 0.59 0.30
5 4.8689083 -0.0189101 4.8499982 0.0622700 1.28 0.0373225 0.77 0.36
3 mass 16.6528370 -0.0297098 16.6231270 0.0912113 0.55 0.0465734 0.28 0.26
1 0.9848403 -0.0009993 0.9838410 0.0106426 1.08 0.0049480 0.50 0.22
2 8.8081249 -0.0635076 8.7446173 0.0817230 0.93 0.0475216 0.54 0.34
3 4.8061904 -0.0157982 4.7903922 0.0504319 1.05 0.0313239 0.65 0.39
4 1.3066553 -0.0090642 1.2975910 0.0101236 0.78 0.0063122 0.49 0.39
5 0.1480575 0.0025565 0.1506140 0.0018382 1.22 0.0009678 0.64 0.28
4 mass 13.9745220 -0.0129900 13.9615320 0.0561305 0.40 0.0425430 0.30 0.57
1 0.9835847 -0.0019182 0.9816665 0.0065377 0.67 0.0049468 0.50 0.57
2 8.5839360 0.0087002 8.5926362 0.0715575 0.83 0.0474234 0.55 0.44
3 4.1633568 -0.0065558 4.1568010 0.0422279 1.02 0.0309195 0.74 0.54
4 0.1399171 0.0001824 0.1400995 0.0016089 1.15 0.0015704 1.12 0.95
5 0.0015772 -0.0000019 0.0015754 0.0000211 1.34 0.0000207 1.32 0.96
5 mass 9.9287668 0.0139440 9.9427109 0.0380675 0.38 0.0287047 0.29 0.57
1 0.1082153 -0.0007784 0.1074368 0.0012562 1.17 0.0008919 0.83 0.50
2 1.5189549 0.0074900 1.5264450 0.0152984 1.00 0.0105447 0.69 0.48
3 6.3229750 -0.0363283 6.2866467 0.0723102 1.15 0.0455585 0.72 0.40
4 1.2664532 0.0207463 1.2871995 0.0147014 1.14 0.0062253 0.48 0.18
5 0.1537728 -0.0001663 0.1536065 0.0015228 0.99 0.0009687 0.63 0.40
6 mass 2.6890580 -0.0274629 2.6615950 0.0250386 0.94 0.0151470 0.57 0.37
1 0.0021955 -0.0000210 0.0021745 0.0000523 2.41 0.0000497 2.29 0.90
2 0.1535941 -0.0016130 0.1519811 0.0020041 1.32 0.0016511 1.09 0.68
3 0.6399527 -0.0063615 0.6335911 0.0075767 1.20 0.0059033 0.93 0.61
4 1.1677094 -0.0102179 1.1574915 0.0127284 1.10 0.0062073 0.54 0.24
5 0.1522891 -0.0032505 0.1490386 0.0020067 1.35 0.0009669 0.65 0.23
7 mass 7.2794283 0.0016875 7.2811158 0.0425291 0.58 0.0274504 0.38 0.42
1 0.1043722 0.0008902 0.1052624 0.0012963 1.23 0.0008917 0.85 0.47
2 1.3783868 -0.0039229 1.3744639 0.0149447 1.09 0.0105225 0.77 0.50
3 5.6260314 0.0270241 5.6530556 0.0609982 1.08 0.0454820 0.80 0.56
4 0.1297311 -0.0000231 0.1297081 0.0010555 0.81 0.0008866 0.68 0.71
5 0.0045662 0.0000017 0.0045679 0.0000634 1.39 0.0000602 1.32 0.90

It is of interest to determine whether or not there is some is of interest. Recognising that the expressions involve matrices
general statement that can be made about the improvement in and using Equation 20, the quantity of interest is:
variance that can be achieved by introducing additional balance R = Σ −1 [ Σ − ΣG T (GΣG T )−1 GΣ ]
streams and nodes. The ratio that has been calculated is the ratio
of the variance of the adjusted component flow to its measured = I − G T (GΣG T )−1 GΣ
variance. In general terms, a ratio of the nature:
To simplify the structure of the uncertainties, let it be assumed
Σ that all measurement uncertainties are statistically independent.
R= a
Σ In such a case, the matrix Σ is diagonal. Then the ratio of the

Sampling and Blending Conference Sunshine Coast, QLD, 9 - 12 May 2005 133
G J LYMAN

TABLE 4
Results for least squares adjustment of component flows with variances using a single balance node. The WSSQ value is 2.4 (expected
value 6) and the average variance ratio is 0.70.

Stream Flows Measured Adjustment Adjusted SDM RSD (%) SDA RSD (%) Var ratio
1 mass 99.5172900 0.3239744 99.8412650 0.4542322 0.45 0.3664377 0.37 0.65
1 0.9975235 0.0066914 1.0042149 0.0120095 1.20 0.0057209 0.57 0.23
2 10.8411280 0.0755441 10.9166720 0.1142302 1.05 0.0644001 0.59 0.32
3 11.9086810 0.1305750 12.0392560 0.1393566 1.16 0.0820157 0.68 0.35
4 12.9694230 0.0128725 12.9822950 0.0943178 0.73 0.0698344 0.54 0.55
5 4.9862954 0.0135906 4.9998861 0.0517201 1.03 0.0374113 0.75 0.52
2 mass 83.6325490 -0.4331022 83.1994470 0.7634572 0.92 0.3609159 0.43 0.22
1 0.0208311 -0.0001119 0.0207191 0.0004256 2.05 0.0003919 1.89 0.85
2 2.2212457 -0.0138327 2.2074130 0.0320104 1.45 0.0265553 1.20 0.69
3 7.3236451 -0.0727133 7.2509318 0.1034831 1.43 0.0763607 1.05 0.54
4 11.7113400 -0.0366727 11.6746670 0.1258338 1.08 0.0698590 0.60 0.31
5 4.8689083 -0.0228845 4.8460237 0.0622700 1.28 0.0374251 0.77 0.36
3 mass 13.9745150 -0.0216839 13.9528310 0.0561305 0.40 0.0522713 0.37 0.87
1 0.9835833 -0.0022829 0.9813004 0.0065377 0.67 0.0057010 0.58 0.76
2 8.5839255 -0.0282493 8.5556762 0.0715574 0.84 0.0602064 0.70 0.71
3 4.1633542 -0.0148434 4.1485108 0.0422278 1.02 0.0404544 0.98 0.92
4 0.1399166 -0.0002047 0.1397119 0.0016089 1.15 0.0015961 1.14 0.98
5 0.0015772 -0.0000024 0.0015748 0.0000211 1.34 0.0000210 1.33 0.99
4 mass 2.6890580 -0.0000715 2.6889865 0.0250386 0.93 0.0249522 0.93 0.99
1 0.0021955 -0.0000001 0.0021953 0.0000523 2.38 0.0000523 2.38 1.00
2 0.1535941 -0.0000116 0.1535825 0.0020041 1.30 0.0020005 1.30 1.00
3 0.6399527 -0.0001391 0.6398136 0.0075767 1.18 0.0075567 1.18 0.99
4 1.1677094 0.0002074 1.1679167 0.0127284 1.09 0.0126607 1.08 0.99
5 0.1522891 -0.0000016 0.1522876 0.0020067 1.32 0.0020030 1.32 1.00

TABLE 5
Recovery of selected species with uncertainties in the recovery values: comparison of single and mutli-node balances. Stream numbers
relate to the three node balance configuration.

Species Stream With internal balance Overall balance only


From To Recovery SD RSD (%) Recovery SD RSD (%)
1 1 2 0.0206380 0.0003938 1.9083 0.0206322 0.0003979 1.9286
1 1 4 0.9771974 0.0003984 0.0408 0.9771817 0.0004038 0.0413
1 1 6 0.0021646 0.0000504 2.3263 0.0021861 0.0000534 2.4447
2 1 4 0.7845984 0.0021559 0.2748 0.7837257 0.0023094 0.2947
5 1 2 0.9698809 0.0002936 0.0303 0.9692268 0.0004581 0.0473
5 1 4 0.0003150 0.0000047 1.5057 0.0003150 0.0000048 1.5192
5 1 6 0.0298041 0.0002918 0.9790 0.0304582 0.0004570 1.5003

Tr[G T (GΣG T ) GΣ ] = Tr[(GΣG T )-1 GΣG T ]


-1
variance of an adjusted component flow to that of the
corresponding measured component flow is simply the
corresponding diagonal element of R. The sum of these ratios is = dimension of [GΣG T ] = N n ( N c + 1)
the sum of the diagonal elements of R, which is known as the
trace of the matrix. The result is:
The average ratio is then the trace divided by the number of
Tr{R} = N s ( N c + 1) − N n ( N c + 1) (22)
diagonal elements, that is, the size of the matrix R. R has a size
N s ( N c + 1). The trace of the identity−1matrix is then N s ( N c + 1).
The trace of the matrix G T (GΣG T ) GΣ is found by using the and the average value is found by dividing by N s ( N c + 1),
rule that to evaluate the trace of a matrix, it is permitted to rotate providing:
the order of multiplication of the matrices. One rotation
provides:  Var{adjusted component flow}  Nn
Average   =1 − N (23)
 Var{measured component flow}  s

134 Sunshine Coast, QLD, 9 - 12 May 2005 Sampling and Blending Conference
SAMPLING, METALLURGICAL ACCOUNTING AND REDUCTION OF BALANCE ESTIMATION VARIANCE

= 29 per cent. Cast in these terms, the return on the investment in


1.00
internal balances is rather good. The internal balances also
Variance Reduction (lower accuracy) Boundary provide additional insight into the process performance by
Internal allowing reliable calculation of recoveries for the three internal
0.75
units.
It also follows from the above result that if the internal process
streams have measurement variances larger than two to three
times the measurement variances associated with the boundary
0.50 streams, there is a risk that the introduction of the internal flows
will degrade the balance. However, this effect can be studied
without actually having to calculate balances simply by using the
expression in Equation 20, and the marginal cost of upgrading
0.25 the quality of the internal stream data can be easily studied.
It is important to note that in a flow sheet with a large number
of identifiable feed streams, the real, single, feed to the process is
the weighted average of all feeds.
0.00
0.00 0.25 0.50 0.75 1.00
CONCLUSIONS
Variance Reduction (higher accuracy)
The simplified statistical analysis of the least-squares mass flow
adjustment problem presented herein demonstrates that there is a
FIG 2 - Variance reduction ratios for balance with low accuracy substantial advantage to be had from the introduction of internal
internal stream measurements. balance nodes when calculating a material balance around a
processing operation. The introduction of internal balances to the
For the one node balance with four process streams, the value common flow sheet under study here provides an average
is 0.75 and for seven process streams with three balance nodes, reduction in component flow variances of about 50 per cent in a
the value is 0.57. The observed values for the calculations were practical situation. This reduction is achieved regardless of the
~0.7 and ~0.5, somewhat better than expected from the measurement variances associated with the streams. The single
simplified theory. The difference of the result from the simplified node balance reduces component flow variances by only 30 per
theory is due to the fact that the covariance matrix is not cent.
diagonal. The above derivation demonstrates that the improved While caution must be exercised when the relative variances of
mass flow variances that arise when using more process streams the measurements for the internal streams exceed two to three
is no accident. This result is entirely valid as long as there is no times those for the boundary streams, the introduction of internal
covariance between measured component flows and is balances provides a variance reduction benefit similar to the
approximately valid when there is covariance. The result here is duplication of all boundary stream assays. On top of this benefit,
remarkably simple and does not depend on the relative for the common flow sheet under study, the internal balances also
magnitudes of the variances or the detailed structure of the flow permit calculation of the recoveries for three unit operations
sheet. where this was impossible with a single node balance.
The unfortunate aspect of this result is that the ratio of nodes It is probable that the benefits proven for the simplified data
to streams cannot be increased much past 0.5. In fact, the flow covariance structure extend to somewhat more complex data
sheet under study may have the maximal variance reduction. structures.
If the total variance of sampling, including sample preparation, The methodology presented here permits the evaluation of
is nominally equal to the analytical variance for all streams, flow sheets and data structures of quite general forms.
duplication of all assay determinations will reduce the total
variance by 25 per cent, yielding a variance improvement after REFERENCES
single node balancing of 25 per cent. As long as the overall
variance of the existing internal stream data is not more than Hinckfuss, D A, 1976. The Bougainville Copper Limited concentrator, in
Flotation, A M Gaudin Memorial Volume (ed: M C Fuerstenau),
double or treble that of the boundary streams, the introduction of Vol 2, pp 1125-1144 (American Institute of Mining, Metallurgical
internal balance nodes, as in this example, will reduce the and Petroleum Engineers Inc: New York).
variance of the adjusted component flows by 100 × (1 - 0.5/0.7)

Sampling and Blending Conference Sunshine Coast, QLD, 9 - 12 May 2005 135
136 Sunshine Coast, QLD, 9 - 12 May 2005 Sampling and Blending Conference
APPENDIX F – DETERMINATION OF THE SAMPLING
CONSTANT
INDIVIDUAL PARTICLE ANALYSIS (50-PIECE EXPERIMENT)

This experiment is based on the one detailed in “Sampling of Particulate Materials –


Theory and Practice” by Pierre Gy (1979). It involves the collection of fifty or more of
the largest pieces of material to be sampled and it measures their mass, volume and
metal contents. The data is used in the following formulae to calculate the bias and
variance associated with the sample.

For an alternative version of this experiment as applied to gold ore sampling, see
Bartlett and Hawkins.

Fundamental Bias:
m(FE) = -Y[1/MS – 1/ML]

Fundamental Variance:
σ2(FE) = Z[1/MS – 1/ML]

where: MS = Mass of sample (g)


ML = Mass of Lot (g)

When in the normal situation ML >> MS the equations can be written as:

m(FE) = -Y/MS

σ2(FE) = Z/MS

It can be shown that:

Y = {(0,25v)/(aQMQ)}{Σq(aq – aQ) Mq2/Vq}

Z = {(0,25v)/(aQ2MQ)}{Σq(aq – aQ)2Mq2/Vq}
where:
Mq = Mass of individual pieces (g)
Vq = Volume of individual pieces (cm3)
aq = Analytical value of individual piece (e.g. % Cu)
MQ = Σq Mq
v = (Σq Vq)/q
q = Number of pieces
aQ = Σq aqMq/MQ

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Using the data from the book by Pierre Gy (pp 276–278):

%Fe Mass Density Volume aqMq aq-aQ W X


55.310 163.0 3.88 42.00 9015.53 17.4000 11007.1571 191524.5343
21.330 121.0 2.75 44.00 2580.93 -16.5800 -5516.9950 91471.7771
37.860 116.0 2.97 39.00 4391.76 -0.0500 -17.2513 0.8626
45.620 127.0 3.26 39.00 5793.74 7.7100 3188.5792 24583.9459
13.910 78.0 2.69 29.00 1084.98 -24.0000 -5035.0345 120840.8276
50.860 102.0 3.92 26.00 5187.72 12.9500 5181.9923 67106.8004
42.650 60.0 2.61 23.00 2559.00 4.7400 741.9130 3516.6678
44.130 142.0 2.96 48.00 6266.46 6.2200 2612.9183 16252.3520
26.910 105.0 3.09 34.00 2825.55 -11.0000 -3566.9118 39236.0294
36.840 119.0 2.64 45.00 4383.96 -1.0700 -336.7171 360.2873
43.220 61.0 3.21 19.00 2636.42 5.3100 1039.9216 5521.9836
4.110 149.0 2.61 57.00 612.39 -33.8000 -13164.8035 444970.3586
6.040 95.0 2.57 37.00 573.80 -31.8700 -7773.6959 247747.6898
7.330 95.0 2.44 39.00 696.35 -30.5800 -7076.5256 216400.1541
43.910 198.0 2.57 77.00 8694.18 6.0000 3054.8571 18329.1429
53.140 107.0 3.96 27.00 5685.98 15.2300 6458.0841 98356.6204
61.580 172.0 4.00 43.00 10591.76 23.6700 16284.9600 385465.0032
62.720 120.0 4.14 29.00 7526.40 24.8100 12319.4483 305645.5117
38.200 119.0 3.61 33.00 4545.80 0.2900 124.4452 36.0891
44.480 104.0 3.71 28.00 4625.92 6.5700 2537.8971 16673.9842
44.930 121.0 3.67 33.00 5436.53 7.0200 3114.5400 21864.0708
47.560 91.0 2.84 32.00 4327.96 9.6500 2497.2391 24098.3570
63.520 148.0 3.70 40.00 9400.96 25.6100 14024.0360 359155.5620
7.300 52.0 2.60 20.00 379.60 -30.6100 -4138.4720 126678.6279
53.830 189.0 3.86 49.00 10173.87 15.9200 11605.6800 184762.4256
43.910 157.0 3.27 48.00 6893.87 6.0000 3081.1250 18486.7500
38.660 116.0 2.76 42.00 4484.56 0.7500 240.2857 180.2143
38.090 66.0 2.75 24.00 2513.94 0.1800 32.6700 5.8806
6.010 141.0 2.66 53.00 847.41 -31.9000 -11966.1113 381718.9511
39.910 128.0 3.28 39.00 5108.48 2.0000 840.2051 1680.4103
21.360 138.0 2.76 50.00 2947.68 -16.5500 -6303.5640 104323.9842
22.800 89.0 2.87 31.00 2029.20 -15.1100 -3860.8487 58337.4240

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%Fe Mass Density Volume aqMq aq-aQ W X
45.730 150.0 3.57 42.00 6859.50 7.8200 4189.2857 32760.2143
4.790 100.0 2.44 41.00 479.00 -33.1200 -8078.0488 267544.9756
47.550 208.0 3.47 60.00 9890.40 9.6400 6951.0827 67008.4369
41.390 127.0 3.26 39.00 5256.53 3.4800 1439.2031 5008.4267
48.580 146.0 2.98 49.00 7092.68 10.6700 4641.6678 49526.5949
59.070 117.0 3.90 30.00 6911.19 21.1600 9655.3080 204306.3173
20.530 102.0 2.68 38.00 2094.06 -17.3800 -4758.4611 82702.0531
10.380 71.0 2.45 29.00 736.98 -27.5300 -4785.4734 131744.0840
44.820 81.0 2.79 29.00 3630.42 6.9100 1563.3279 10802.5960
3.400 82.0 2.28 36.00 278.80 -34.5100 -6445.7011 222441.1453
41.280 105.0 3.39 31.00 4334.40 3.3700 1198.5242 4039.0265
48.130 116.0 3.52 33.00 5583.08 10.2200 4167.2824 42589.6264
46.830 110.0 3.55 31.00 5151.30 8.9200 3481.6774 31056.5626
7.640 67.0 2.58 26.00 511.88 -30.2700 -5226.2319 158198.0403

where:
W = (aq – aQ)*Mq2/Vq
X = (aq – aQ)2Mq2/Vq
by calculation:
MQ = 5371
aQ = 37.91
v = 37.67
Y = 1.8
Z = 5.9 (Sampling Constant)
using the relationship for Fundamental Variance, given previously:

σ2 = Z/MS

the following minimum sample masses (kg) can be calculated at the indicated
variances.

Variance 10% 5% 3% 1%
(Relative)
Mass 2.4 9.4 26.2 236

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APPENDIX G – ERROR AND VARIANCE PROPAGATION IN
TOLL SMELTING OPERATIONS TREATING MULTIPLE
CONCENTRATE STOCKPILES
Chris J. Cutler, Jacques J. Eksteen*

JSAIMM, Vol.106, pp 222–227. Re-published with permission of:


The Southern African Institute of Mining and Metallurgy

Department of Process Engineering, University of Stellenbosch, Private Bag X1,


Matieland, 7602, South Africa

*Corresponding Author, E-mail: jeksteen@sun.ac.za

Abstract

Metallurgical accounting for toll treatment smelters pose a number of challenges.


Multiple feed stockpiles have to be accounted for as part of the monthly recovery
estimation. Moreover, multiple metallurgical intermediates make up part of the in-
process inventory, which also influence the monthly recovery calculation. Errors
propagate from the measurements of volumes, assays, moisture fractions and bulk
densities in the various material types through multiple steps up to the point where
the final recovery is calculated. These errors contribute non-linearly to the variance in
the final recovery estimate. This paper develops the mathematical formulation for
variance propagation in toll smelting operations, including the effect of in-process
inventory, assuming measurement biases have been eliminated beforehand.
Operational data from a Southern African copper smelter is used for a case study.

The method of propagation of variance showed that uncertainties in stockpile assays


were the main contributors to variance in the recovery estimate. Variance in the
volume and bulk density uncertainties contributed a secondary, yet significant,
proportion to the overall recovery variance. It was determined, for the given case
study, that the recovery variance depended on the calculation method used and that
variance propagation via the two-product formula was smaller than recovery
variances calculated via the standard recovery formula. However, the probability that
the two product formula will give inaccurate (versus imprecise) results is significantly
more due to the practical difficulty of equiprobable sampling of tailings streams from
smelter plants (which includes materials such as slags and flue dust).
Recommendations are made on how to achieve a reduction in overall uncertainty for
toll treatment smelters.

Keywords: Metallurgical Accounting, Copper Smelters, Pyrometallurgy, Variance


Propagation, Errors, Precision, Sampling

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Introduction

Improvements in metallurgical accounting systems are often motivated by the drive to


improve corporate governance and transparency. Many non-ferrous smelter
managers are confronted with widely varying recovery estimates, depending on the
calculation method used and the range of possible bases from which recovery is
estimated. This has lead to recovery being a poorly defined, but highly significant
number (“Key Process Indicator”) bandied about by metallurgists, managers and
investors, all with a different perception as to what is really meant.

In this paper it is shown how variance propagate through plant material balances. As
stockpiles of raw materials, products and inventory always fall within the battery limits
of a smelter plant they make up part of the working capital, a figure directly reflected
on the balance sheet of each smelter. The cumulative effect of uncertainty in the
measurement of stockpile volumes, moisture levels and bulk densities propagates
non-linearly through to the variance in average plant feed assays and estimated
recoveries. There is little published information on what precision can be ascribed to
the copper recovery from concentrate to anode or blister over a given metallurgical
accounting period.

Where the mine and the smelter are an integrated unit the overall recovery from mine
to metal is of primary importance and changes can be made either at the mill or the
smelter to maximize the overall recovery. Where the smelter recovery is extremely
important is when concentrates are purchased or tolled because of the contract
structures where the payable metal values mean that the smelter must achieve a
certain minimum recovery in order to break even.

This paper is an attempt to quantify the variance in the recovery from first principles
using plant data where the accounting principles are based on a “check in – check
out” system (Wills, 2005) which is often used for pay-metal accounting on a smelter.
However, the “check in-check out” system becomes impractical at smelters for
nonpay-elements and volatile elements such as sulphur (also elements such as
arsenic, antimony, zinc) where bulk quantities are not transported via a checkpoint
and continuous and variable losses occur via flue gases and fugitive emissions (such
as from Pierce Smith converters, and molten matte transport in ladles).

Various calculation strategies are now considered for a range of typical metal
accounting approaches. In the discussion below, bias (due to gross or systematic
measurement error) has been ignored. In other words, all listed plant measurements
are assumed to be unbiased. A number of methods exist for bias detection, such as
the “cusums method” (Bartlett, 2005) for a lumped, plant-wide test, or through
statistical tests (François-Bongarçon, 2005) on individual sampling points using
paired t-tests. Should biases be found to be present, they should be eliminated
through proper calibration, maintenance, or repair (such as leaks) as required.
Sometimes total redesign of the sampling system is required according to the
principles of representative sampling.

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Recovery Calculation from Assays only: Application of The Two Product
Formula

If the weights of monthly smelter feed, blister copper (product) and discard slag (tails)
are F , P and T respectively and their corresponding assays f ,p, and t then :

F =P+ T
(1)

i.e. : total material input = total material output, over the period of a month, and

F ⋅ f = P⋅p + T ⋅ t
(2)

i.e. : the valuable metal, in this case copper, is balanced.

The bar above the feed and tailings variables indicate representative quantity over
the monthly period, with inclusion of stocpiles for all feed or tailings material types.

It follows that:

F ⋅ f = P⋅p + ( F – P) ⋅ t
(3)

which gives the split fraction to the product stream as:

P (f − t)
=
F (p − t )
(4)

Subsequently, the metal recovery (Cu in this case) can be defined as :

p⋅P
R= ⋅ 100%
f ⋅F or:
(5)

p⋅( f − t)
R= ⋅ 100%
f ⋅ (p − t )
(6)

The variance in any calculated amount (say recovery, or calculated stockpile mass,
or average concentration) can be found from the variances in the measured
quantities (such as assays, volumes, measured weights, etc.) through the summation
of the squared partial derivatives of the calculated variable with respect to the
independent measured quantities each multiplied with the respective variance in the
measured quantity. The mathematical proof can be found in many a good text on
mathematical statistics, such as Kreyszig (1970) and is based on the Taylor series
expansion of the error of a multivariable function. This relationship is usually referred
to as the “Propagation of Variance” or the “Law of Propagation of Error (LPE)”. This

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paper applies this principle to smelter plants treating multiple material types, where
stockpiles and in-process inventories are present.

Xiao and Vien (2003) has noted that the addition of the second Taylor series term
may be required in cases of large relative standard deviations of measurements.
They state that the law of propagation of error (variance) is only an approximation,
because second- and higher-order derivatives are neglected. For the non-linear
variance propagation case, the precision of the approximation increases with
decreasing relative variance, i.e. for small relative errors. Therefore, the truncation of
the Taylor series approximation after the first term becomes less accurate when
double digit relative standard deviations are measured on the plant, such as often
found for slags and dusts (Eksteen et al., 2004). Additionally, it is assumed that the
measurements are independent, which may not be the case in practice.

The variance of a calculated variable (such as recovery) is a summation of the first


derivative squared multiplied by the respective variances if the measurement
variables are independent. For correlated measured variables, the covariances
should be included in the error propagation estimate of recovery variance. Xiao and
Vien (2003) did not consider the effect of stockpiles, but did show that Monte Carlo
based methods estimated recovery variances to be of the same order but slightly
larger than the variance propagation methods. Moreover, the Monte Carlo based
methods allows one to see the effects of multiple normal and / or non-normal
measurement distributions on the recovery distribution. As long as knowledge of the
shape of the distribution is well defined, the Monte Carlo method is superior to
variance-propagation. However, this knowledge is often not available, or can only be
obtained at great cost, and plant metallurgists are often not inclined to perform Monte
Carlo simulations on their desktop computer when a simpler formula-based
estimation of variance is available.

The variance in plant recovery, R, based on the derived two product formula
(Equation 6), can be found from it’s derivatives as follows:

2 2 2
⎛ ∂R ⎞ ⎛ ∂R ⎞ ⎛ ∂R ⎞
V R = ⎜⎜ ⎟⎟ V f + ⎜⎜ ⎟⎟ V p + ⎜ ⎟ Vt
⎝ ∂f ⎠ p ,t ⎝ ∂p ⎠ f ,t ⎝ ∂t ⎠ p , f
(7)

where VR , V f , Vt and Vp are the variances in R, f , t and p respectively (for the


month). For the two product formula, the derived propagated variance in recovery in
term of assays and assay variances only, is:

⎡ p2 ⋅ t2
V R = ⎢ 2 Vf +
( f − t )2 ⋅ t 2 V + ( p − f )2 ⋅ p 2 V ⎤⎥ ⋅ 1002
⎢⎣ f ( p − t )2 p ( p − t )2 t ⎥⎦ f 2 ( p − t )2
(8)

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Recovery Calculation from Masses and Assays: Traditional Recovery Estimate
(Excluding Inventory)

p⋅P
As copper recovery is defined by equation 5: R = ⋅ 100% where P, p, F , and
f ⋅F
f are defined as in Equations 1 and 2.

Then, as R = f(F, P, f, p),

the variance of R can be found from the partial derivatives with respect to each
variable:

2 2 2 2
⎛ ∂R ⎞ ⎛ ∂R ⎞ ⎛ ∂R ⎞ ⎛ ∂R ⎞
V R = ⎜⎜ ⎟⎟ Vf + ⎜ ⎟ VF + ⎜⎜ ⎟⎟ Vp + ⎜ ⎟ VP
⎝ ∂f ⎠ F , p ,P ⎝ ∂F ⎠ f , p ,P ⎝ ∂p ⎠ f ,F ,P ⎝ ∂P ⎠ p , f ,F
(9)

where VR , V f , VF , VP and Vp are the variances of R , F , f , P and p respectively. If


the derivatives are evaluated equation 9 becomes:

⎡⎛ − p ⋅ P ⎞ 2 ⎛ − p⋅P ⎞
2
⎛ P ⎞
2
⎛ p ⎞ ⎤
2

V R = ⎢⎜⎜ ⎟ V f + ⎜⎜ 2
2 ⎟
⎟⎟ VF + ⎜⎜ ⎟⎟ V p + ⎜⎜ ⎟⎟ VP ⎥ ⋅ 1002
F⋅f ⎠ ⎝F ⋅f ⎠ ⎝F⋅ f ⎝F⋅ f
⎣⎢⎝ ⎠ ⎠ ⎦⎥
(10)

Recovery Calculation from Masses, Assays and Inventory Change

When inventory changes are to be incorporated, over and above new metal bearing
material, the copper recovery is defined as follows:

p⋅P
R=
f ⋅F + ∑ ∆m a
i
i i

(11)

where mi and ai represents the change in copper of inventory item i based on


opening (o) and closing (c) masses and assays respectively, and the bar superscripts
referring to actual monthly feed assay and net weight (all material types) fed to the
smelter. Note that the there are different inventory material types to feed material
types.

The net change in in-process inventory, per material type i, between month end and
beginning is:

∆mi ai = (mi ai ) − (mi ai )


o c

(12)

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The associated variance in copper mass in inventory stockpiles over a month is:

⎡ ∂ (∆mi ai )⎤ ⎡ ∂ (∆mi ai )⎤ ⎡ ∂ (∆mi ai )⎤ ⎡ ∂ (∆mi ai )⎤


2 2 2 2

V ∆miai= ⎢ ⎥ Vao + ⎢ ⎥ Va c + ⎢ ⎥ Vmo + ⎢ ⎥ Vmc


⎣ ∂ai ⎦ mio ,mic ,aic ⎣ ∂ai ⎦ mio ,mic ,aio ⎣ ∂mi ⎦ aio ,mic ,aic ⎣ ∂mi ⎦ mio ,aio ,aic
o i c i o i c i

(13)

The sum of the variances for the total inventory change (all material types) is then the
sum of the variances for the individual items (as they are statistically independent),
i.e.:

V∆maT = ∑Vi
∆mi ai

(14)

Estimation of Variances in Feed Masses and Assays each per Material Type

The calculation for each material treated in the smelter is in two parts:

• calculation of opening and closing stock variance


• calculation of receipts variance
The net change in mass of ore material/concentrate type k for a one-month period is:

∆Fk = M dkr + M ko − M kc
(15)

The variance in feed mass is simply the sum of the opening and closing stockpile
variances and the receipts variance, as the variances in opening, closing, and receipt
masses are statistically independent (However, independence is questionable if there
is a bias in stock measurement):

V∆Fk = VM r + VM o + VM c
dk k k

(16)

where the superscripts o , c and r refer to the opening stocks, closing stocks and
receipts respectively.

Opening and Closing Stock Variance per Material Type

The mass of a given stockpile (opening or closing) is defined by the following


equation:

M k = Volk BDk (1 − mf k )
(17)

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where Mk , Volk and BDk are the dry weight, volume and bulk density stockpile of
material type k, and mfk is the moisture fraction of material k (% moisture divided by
100).

The variance of the dry weight of stockpile Mk is defined by the following equation :

2 2 2
⎛ ∂M k ⎞ ⎛ ∂M k ⎞ ⎛ ∂M k ⎞
VM k = ⎜⎜ ⎟⎟ VVolk + ⎜⎜ ⎟⎟ VBDk + ⎜⎜ ⎟⎟ Vmf i
⎝ ∂Volk ⎠ BDk ,mf k ⎝ ∂BDk ⎠Volk ,mf k ⎝ ∂mf k ⎠ BDk ,Volk
(18)

Then from the partial differentials:

VM k = [BDk (1 − mf k )] VVolk + [Volk (1 − mf k )] VBDk + (Volk BDk ) Vmf k


2 2 2

(19)

Receipts Variance per Material Type

The dry weight of a shipment of material k is represented by the Eq. 18 :

M dkr = (1 − mf k ) ⋅ M wkr
(20)

where Mdkr is the dry weight of the shipment, Mwkr is the as-received (wet weight) as
measured on a weigh bridge and mfk is the moisture fraction as previously defined.
The corresponding variance of the dry weight of the receipt is defined by the Eq.19:

2 2
⎛ ∂M dkr ⎞ ⎛ ∂M dkr ⎞
VM r = ⎜⎜ ⎟⎟ VM r + ⎜⎜ ⎟⎟ Vmf k
⎝ ∂M wk ⎝ ∂mf k
r
⎠ mf k ⎠ M wkr
dk wk

(21)

Then from the partial differentials:

VM r = (1 − mf k ) ⋅ VM r + (M wk ) ⋅Vmf i
2 r 2

dk wk

(22)

Feed Assay Variance in Overall Feed (All Material Types)

Average assay and associated variances for one material type over month
duration

The check in – check out system of accounting defines the average feed assay fk for
one material type as follows:

akr M dkr + ako M ko − akc M kc nett mass of copper fed of material type k during a month
fk = =
M dkr + M ko − M kc total mass of material type k during a month
(23)

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where M dkr , M ko and M kc are the dry tonnages for receipts, opening and closing
stocks respectively and a kr , a ko and a kc are the receipt assays, opening assays and
closing assays for copper respectively. This gives the average copper assay, per ore
or concentrate type, over the duration of one month, taking into account receipt and
the open and closing stockpiles.

The variance of the average assay is then:

2 2 2 2 2 2
⎛ ∂f ⎞ ⎛ ∂f ⎞ ⎛ ∂f ⎞ ⎛ ∂f ⎞ ⎛ ∂f ⎞ ⎛ ∂f ⎞
V f k = ⎜⎜ kr ⎟⎟ Va r + ⎜⎜ ko ⎟⎟ Va o + ⎜⎜ kc ⎟⎟ Va c + ⎜⎜ kr ⎟⎟ VM r + ⎜⎜ k o ⎟⎟ VM o + ⎜⎜ k c ⎟⎟ VM c
⎝ ∂a k ⎠ ⎝ ∂a k ⎠ ⎝ ∂a k ⎠ ⎝ ∂M dk ⎠ ⎝ ∂M k ⎠ ⎝ ∂M k ⎠
k k k dk k k

(24)

where VM r , VM o and VM c are the variances of M dkr , M ko and M kc respectively


dk k k

and Va r , Va o , Va c are the variances of a kr , a ko and a kc respectively.


k k k

The partial differentials with respect to mass and assay are illustrated by the
following:

⎛ ∂f k ⎞ M dkr
⎜⎜ r ⎟⎟ = r
⎝ ∂ak ⎠ M dk + M k − M k
o c

(25)

and similarly through partial derivation with respect to a ko and a kc .

⎛ ∂f k ⎞ akr ⋅ (M ko − M kc ) − (ako M ko − akc M kc )


⎜⎜ ⎟⎟ =
⎝ ∂M dk
r
⎠ (M dkr + M ko − M kc )2
(26)

and similarly through partial derivation with respect to M ko and M kc .

Average assay for a blend multiple materials

A copper smelter usually treats more than one concentrate type and in some cases a
variety of mattes and purchased scrap as well. The monthly average assay, as fed to
the furnace (i.e. the equivalent of all stockpiles combined and fed via belt conveyor
into the furnace over a one-month period) can be defined as follows:

∑ f ∆F k k

f = k

∑ ∆F k
k

(27)

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The total mass fed from new metal bearing material for the month (total mass
excluding inventory change) is:

F= ∑ ∆F
k
k

(28)

The variance of the average feed copper is defined as follows:

2 2
⎛ ∂f ⎞ ⎛ ∂f ⎞
Vf = ∑ k
⎜⎜
⎝ ∂f k
⎟⎟ V f k +


k
⎜⎜
⎝ ∂∆Fk
⎟⎟ V∆Fk

(29)

The partial differentials with respect to mass and assay are illustrated by the
following:

⎛ ∂f ⎞ ∆Fk
⎜⎜ ⎟⎟ =
⎝ ∂f k ⎠ ∑ ∆F k
k

(30)

n n

⎛ ∂f ⎞
fk ∑ ∆F − ∑ f ∆F k k k

⎜⎜ ⎟⎟ = k =1 k =1

⎝ ∂∆Fk
2
⎠ ⎛ n





k =1
∆Fk ⎟


(31)

For a total of k=1..n material types (concentrates fed to smelter).

So that the variance in the average feed assay, including the effect of stockpiles is
given by:

2
⎛ n n ⎞

∑ ∑ ⎟
2
⎛ ⎞ ∆Fk − f k ∆Fk ⎟
⎜ ∆F ⎟ ⎜ fk
Vf = ∑∑ ⎜

k

∆Fk
⎟ Vf +
⎟ k ∑ ⎜

k =1

⎛ n
k =1


2
⎟ V∆F
⎟ k

⎜ ⎟

⎜ ∆Fk ⎟
k k
⎝ k ⎠ ⎜ ⎟
⎜ ⎜ ⎟ ⎟
⎝ ⎝ k =1 ⎠ ⎠
(32)

Product Weight Variance

In the case considered here the product blister is weighed on an assized weighbridge
with an accuracy of ±20kg in 100 tones. Any weight measurement on this bridge has
a relative standard deviation (RSD) is 0.01. Assuming a normal distribution of
measurement uncertainties, the standard error can be said to be ±1.96×σ, within a
95% confidence interval (Kreyszig, 1970).

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NS

∑ (m − m )
j =1
2

Where: σ =
n −1
(33)

and NS is the number of weight determinations during calibration.

Product Assay Variance

The RSD was calculated by analysis of assay results from multiple spoon samples
taken from the same ladle during blister copper pouring. The RSD was determined
as 0.047.

Discard Slag Assay Variance

Although the RSD for copper in discard slag was not directly measured, work done
by Eksteen et al. (2004) as well as within the AMIRA P754 project suggests that the
RSD is likely to be in the range 15 - 20% for metal/matte elements, where the
element/species can be entrained (e.g. Cu in this case). The RSD is much smaller for
dissolved metal losses than for entrained metal losses in slags. Due to the difficulty
of achieving equiprobable sampling for melts, there is a significant risk of introducing
bias due to the sampling process. This bias is also difficult to assess as finding the
“true” value is not economically viable. There is therefore a very good reason for
using feed and product assays only, rather than including waste materials (such as
slags and dusts). However, the inclusion of waste does aid in material balancing
(using data reconciliation), but only if the composition can be determined without
significant bias.

Worked Example

The base data for the following cases is July 2005 actual data for a Southern African
copper smelter A. For confidentiality reasons the sources of the materials treated are
not given.

Recovery and Variance Calculation from Assays using the 2-product formula:

Actual Input Data

f : average copper assay in feed mix : 32.95%

p : copper assay in blister copper : 98.85%


t : copper assay in discard slag : 1.30%
V f : variance in average % copper in feed mix : 0.58

Vp : variance in % copper in blister copper : 0.0021


Vt : variance in % copper in discard slag : 0.0676

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Then by substitution in Eq. 6:

R = 97.32%

and using Eq. 7: VR = 147.18 Vf + 1.65 Vp + 43572.40 Vt

which on substitution with the values given above gives:

VR = 0.008 + 0.0000003 + 0.295 = 0.303

and therefore the σR = 0.55, and the standard error with 95% confidence limits =
±1.1%

From this calculation the recovery at the 95% confidence level will be 97.3% ± 1.1%.

In this case the recovery variance is dominated by the variance in copper in the
discard slag with a small contribution coming from the variance in the average copper
in feed mix.

Recovery and Variance Calculation from Masses and Assays

Actual Input Data

f : average copper assay in feed mix: 32.95%

p : copper assay in blister copper: 98.85%


t : copper assay in discard slag: 1.30%
V f : variance in average % copper in feed mix: 0.58

Vp : variance in % copper in blister copper: 0.0021


Vt : variance in % copper in discard slag: 0.0676
F : total dry tones of feed: 8103 mt
P : blister copper produced: 2703 mt
VF : variance in the weight of feed: 11771 mt2

VP : variance in the weight of blister copper: 0.0729 mt2

Then by substitution:

R = 100.1%

and VR = 0.00015 VF + 0.0014 VP + 92265.5 Vf + 10251.7 Vp

VR = 1.80 + 0.0001 + 5.34 + 0.002 = 7.14

and therefore σR = 2.67

From this calculation the recovery at 95% confidence limits is: R = 100.1% ± 5.2%

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In this case the variance in the recovery is significantly influenced by the feed assay
variance and less so by the feed mass variance. The calculated recovery is not
meaningful from a practical perspective, because it does not yet take inventory
change into account.

Recovery Calculation from Masses, Assays and Inventory Change

Input Data

f : average copper assay in feed mix: 32.95%

p : copper assay in blister copper: 98.85%


t : copper assay in discard slag: 1.30%
V f : variance in average % copper in feed mix: 0.58

Vp : variance in % copper in blister copper: 0.0021


Vt : variance in % copper in discard slag: 0.0676
F : dry tones of feed: 8103 mt
P : blister copper produced: 2703 mt
VF : variance in the weight of feed: 11771 mt2

VP : variance in the weight of blister copper: 0.0729 mt2

∑ ∆m a
i
i i = copper in inventory change: 80 mt

V∑ ∆miai : variance in copper in inventory change : 219 mt2


i

Then by substitution :

R = 97.2%

and VR = 0.0116 VF + 0.0013 VP + 286.3 V f + 9663.9 Vp + 0.0353 V∑ ∆mi ai


i

VR = 1.6 + 0.00009 + 4.72 + 0.002 + 0.27 = 6.59

and σR = 2.6

For this case the inventory variance has some significance but the feed assay
variance is still dominant.

Discussion of Results

This work was undertaken to try and understand why the recovery numbers and
unaccounted losses in smelter A varied by up to 5% in any month accounting period
when the process streams and recycles were accounted for and the flowsheet was
closed except for discard slag.

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While the calculation of recovery variance from assays (two-product formula) gives
good numerical results, it is certainly the least accurate because of the difficulties in
practice of estimating the tailings assay variance which in this case is discard slag.
Moreover, due to the difficulty of implementing equiprobable sampling practice for
melts, there is a significant probability of introducing bias through systematic error
due to poor sampling. The calculation is relatively insensitive to feed assay variance
mostly due to the totally overpowering effect of tailings variance.

It is preferable to go back to the calculations based on mass and assays including


change in inventory which are inherently more accurate, because reasonable
estimates can be put around the basic parameters. The recovery calculation in this
case does not rely on any variances associated with weights or assays of discard
slag where the sampling technique is paramount and furnace conditions need to be
stable at all times for the discard slag assay to mean anything.

In the case of the mass estimates the variances in stock pile volumes, bulk densities
and moisture levels can be established in the field. In the case of assays the
sampling and analytical errors are reasonably well known. The major contributor to
the feed assay variance is the assay variability between lots and within lots which
comes back to the performance of the concentrator at the mine. The initial
assumption in this analysis was that the variance in copper assay between lots of
nominally 400 tones would be representative of the variance within a lot. This was
checked using 10 sequential lots of the individual concentrates and 10 wagons within
a lot. The results are shown in Table 1.

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Table 1 - Concentrate Assays and measured? Standard Deviations

Material Type Lot Average Cu % σ Wagon Average Cu % σ


Concentrate A 23.70 0.92 23.97 1.48
Concentrate B 51.65 3.1
Concentrate C 29.39 1.1
Concentrate D 21.76 2.7 20.50 3.1
Concentrate E 30.84 2.7 31.62 3.0

Table 2 is a summary of sensitivities against the base case as calculated using


masses, assays and inventory change.

Table 2 – Contributions to variance: Comparison Against Base Case

Base % % % %
Comp Case Cont Case 1 Cont Case 2 Cont Case 3 Cont Case 4 %

VF 1.60 24 1.60 42 0.04 1 0.04 2 2.43 29

VP 0.00009 0 0.00009 0 0.00009 0 0.00009 0 0.00009 0

Vf
4.72 72 1.90 50 4.32 93 1.80 85 5.63 68

Vp 0.002 0 0.002 0 0.002 0 0.002 0 0.002 0

V∑ ∆mi ai
i 0.27 4 0.27 7 0.27 6 0.27 13 0.27 3

VR 6.6 3.8 4.6 2.1 8.3

σR 2.6 1.9 2.2 1.5 2.9

The 5 cases in Table 2 are as follows:

• The Base Case is the actual case as observed for a given month for smelter
A.
• Case 1 assumes that the copper assay variance for concentrate A was
applicable for all concentrates
• Case 2 assumes that all concentrates received during the month were treated
during the month
• Case 3 is the “best” case where there are no opening and closing stocks and
the assay variance for concentrate A applies to all concentrates

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• Case 4 assumes that there are opening and closing stocks for all
concentrates treated during the month
In all cases the average feed assay variance is the major contributor to the recovery
variance although the mass variance becomes significant where there are opening
and closing stocks for each concentrate type. As for all stockpiles, managing
between empty piles is a practical way to control this problem. Piles which almost
never empty are convenient – especially for hiding problems.

In all cases the contributions of variance of both the product weight (blister copper)
and the product assay were insignificant, due to the high degree of precision.

Conclusions

The following conclusions could be drawn from the analyses presented above.

• A variance propagation model has been formulated for a copper toll treatment
smelter. This variance propagation model took into account changes in
stockpiles, as well as changes in inventories.
• It was determined that, despite the 2-product formula being more precise (i.e.
smaller variance in recovery estimate), it is inherently less accurate, due to
challenges associated with the sampling of melts, dusts and gases in cases
when these become the “tailings”, or waste of a smelter.
• The assay variance in feedstocks was always the largest contributor to
variance in recovery, and was always greater than the contribution due to
variances in net masses fed (which includes stockpile and inventory
changes).
• The large observed variances in recoveries could be explained through the
variance propagation model.
• The actual observed case (Base Case) showed that the standard deviation in
the recovery estimate was 2.6%. The standard error in the monthly recovery
estimate is therefore +/- 1.96 × 2.6% = ±5.1% with 95% confidence.
• There is therefore a clear business case to improve sampling practice and
instrumentation on this specific toll treatment smelter. However, the most
effective way to reduce the recovery variance is to reduce the assay
variability between stockpiles. Subsequent to the reduction in assay
variability, is the reduction in the variability in stockpile masses due to
variability in volumes, bulk densities and moisture fractions. Good control over
blending might go a look way in achieving this goal, i.e. variation between
material type assays can be reduced through proper blending based on
known assays of all material types being blended. However, doing this well
usually requires a major capital investment.
• Bulk density variation can be reduced through the use of a narrow particle
size distribution, volume variances can be reduced through improved
surveying techniques and the variance in moisture fractions can be reduced
by, for example, shielding the stockpiles from environmental changes in
moisture (e.g. using a shed).

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• As the variance in recovery is known, it serves as a baseline for developing
improved material balance closure (data reconciliation) techniques, such as
least squares (Narasimhan and Jordache, 2000; Romagnoli and Sánchez,
2000) or maximum likelihood methods (Kreyszig, 1970; Seinfeld and Lapidus,
1974). For these methods, all information is used for all streams, elements
and nodes for which metallurgical accounting information is available.
Repeating these methods using a Monte Carlo simulation approach based on
known measurement uncertainty distributions allows one to generate the
distribution in recovery estimates and therefore to calculate the recovery
variance after reconciliation. Other possibilities are more elements assayed
and better feed mass measurement and sampling. In essence this would aid
the metallurgist to investigate various options to determine where the most
variance reduction can be obtained for the least investment.
• It should be noted that no assumption of the distributions of measurement
uncertainties were made. This does not influence analyses, except where
standard errors are converted into standard deviations, or visa-versa, where
an assumption of normality is made. The normality assumption influences the
95% confidence intervals. A skewed (non-symmetrical) distribution will lead to
non-symmetrical confidence limits around the expected value.
• The error propagation model is based on fundamental theorems in
mathematics and statistics and material balances and is not constrained to a-
priori knowledge of the error distributions. However, practical implementation
of the model requires a method to translate standard errors to standard
deviations, and the quantification of the error distribution through fitting the
histogram developed through well-planned sampling campaigns and / or the
continuous use of well calibrated sampling and measurement devices. In
short, we need a model of how measurement error itself behave at different
measurement values.
• Errors which lie outside the propagation of variance models presented above
may be caused by bias or by data which is simply in error for some other
reason such as mis-entry of data or mislabelling of samples.
• Large relative standard deviations or measurement variances may require a
more complex variance propagation formulation, as the first term of the Taylor
series approximation becomes inadequate to quantify the full effect of
measurement errors on the variance in the calculated variable (recovery in
this case).
Acknowledgements

This project was performed at the University of Stellenbosch as a subproject of the


AMIRA P754 program on Metallurgical Accounting and Reconciliation, done in
collaboration with the Julius Kruttschnitt Mineral Research Centre and the University
of Cape Town .

The AMIRA P754 program is aimed at delivering a Code, a set of Guidelines and a
set of Toolboxes for Metallurgical Accounting and Reconciliation with the aims of:

• improving transparency at the corporate governance level;

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• quantifying the causes and sources of “unaccounted losses” and bias;
• quantifying the uncertainty in measurements of masses, assays, stocks and
recoveries;
• quantifying the investment risk associated uncertainties in working capital
(inventories and stocks) and operating performance (recovery).
The authors would like to acknowledge the contributions of the AMIRA P754
sponsors and the contributions of the National Research Foundation through its
THRIP (Technology and Human Resources for Industry Program) initiative.

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References

Bartlett, H.E., Confidences in Metallurgical Balances Estimated from Errors in Mass


Measurement, Sampling, and Analytical Determinations, Exploration, Mine, Met and
Environmental Sampling 2005 (EMMES 2005), SAIMM, Johannesburg, 3-4
November, 2005

Eksteen J.J., Frank S.J., Reuter M.A., Distributed compositional and temperature
nature of melts in submerged and open arc furnaces in high carbon ferrochrome
production, Proceedings of the 10th International Ferroalloys Congress (INFACON X),
1-4 February, Cape Town, South Africa, pp. 83 -93, 2004

François-Bongarçon, D., The Philosophy of Statistical Bias Testing Revisited and


Applied to Automatic Samplers, Proceedings of the 2nd World Conference on
Sampling and Blending, 10-12 May, Sunshine Coast, Queensland, Australia, pp. 15-
17, 2005

Kreyszig, E., Introductory Mathematical Statistics: Principles and Methods, John


Wiley and Sons, New York, N.Y.Y., pp. 355-357, 1970.

Narasimhan, S., and Jordache, C. Data Reconciliation and Gross Error Detection: An
Intelligent use of Process Data, Gulf Publishing, Houston, Texas, 406 pp. 2000

Romagnoli, J.A., and Sánchez, M.C., Data Processing and Reconciliation for
Chemical Process Operations, Process Systems Engineering, Vol. 2, Academic
Press, San Diego, California, 270 pp., 2000

Seinfeld, J.H., and Lapidus, L., Mathematical Methods in Chemical Engineering, Vol.
3 (Process Modeling, Estimation and Identification), Prentice-Hall, Englewood Cliffs,
New Jersey, 545 pp, 1974.

Wills, B.A., Mineral Processing Technology, 7th Edition, Butterworth-Heineman, 2005

Xiao, Z., Vien, A., Limitations of variance analysis using propagation of variance,
Minerals Engineering, Vol. 16, pp. 455–462, 2003

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APPENDIX H – USEFUL WEB SITES
ANSI – www.ansi.org

AOAC – www.aoac.org

APLAC – www.ianz.govt.nz/aplac

ASME – www.store.asme.org

ASTM – www.astm.org

British Standards – www.bsonline.bsi-global.com

CITAC – www.citac.org

COMAR (Reference Material Data Base) – www.comar.bm.de

DIN – www.normas.com/DIN/indexes/

EURACHEM – www.eurachem.org

IEC – www.iec.org

ILAC – www.ilac.org

Institute of Measurement and Control – www.instmc.org.uk

ISA – www.isa.org

ISO – www.iso.ch

(ISO) REMCO – www.iso.org/remco

JIS – www.jis.org

NATA – www.nata.asn.au

NIST – www.nist.gov

OIML – www.oiml.org

SABS – www.stansa.co.za

SANAS – www.sanas.co.za

Standards Australia – www.standards.org.au

UKAS – www.ukas.com

VAM – www.vam.org.uk

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