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Eradication of Time Dependency in Leaching Data

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0892--6875(97)00063-0

Minerals Engineering, Vol. 10, No. 8, pp. 859--870, 1997

1997 Elsevier Science Ltd

Printed in Great Britain. All rights reserved

0892-6875/97 $17.00+0.00

BAT CH LEACHI NG DAT A ANALYSI S: ERADI CAT I ON OF

T I ME DEPENDENCY PRI OR T O ST AT I ST I CAL ANALYSI S

N. P O WE L L a n d M. A . J O R D A N

Camborne School of Mines (University of Exeter), Redruth,

Cornwall, TR15 3SE, UK. E-mail: M.Whitbread-Jordan@csm.ex.ac.uk

(Rece&ed 4 January 1997; accepted 22 April 1997)

ABSTRACT

The evaluation of batch experimental of data from laboratory and pilot testwork e.g. batch

leaching of metal fr om sulphide ores, may be utilised to determine the optimum process

conditions. Statistical analysis techniques shouM allow f or the time-dependent nature of

the data ,zs failure to recognise and correct f or such time dependency may lead to

incorrect interpretation of the data. This paper illustrates a corrective technique f or time-

dependent batch data. The technique is demonstrated using a typical data set fr om a batch

bioleach experiment. 1997 Elsevier Science Ltd

Keywords

Sulphide Ores, Leaching, Bioleaching

INTRODUCTION

Preliminary batch leaching tests such as the dissolution of copper from a low-grade (<1% Cu) are invariably

the starting point on which subsequent larger scale tests are based. These tests may vary in size but all will

provide valuable experimental data pertaining to key operating parameters such as reaction kinetics, strength

of lixiviants, metal recovery etc. Consequently accurate interpretation of experimental data is essential both

in terms of focusing: any on-going experimental work (optimisation of process conditions) as well as in the

final selection of process conditions. The fundamental problem with interpretation of batch leaching data

using conventional statistical techniques, is that the data is time-dependent i.e. metal concentration increases

with time (ordinarily) and excludes itself from much conventional statistical analysis. The time-dependent

nature of the raw data must therefore be compensated for. Jordan et al. [1] noted the problem of time

dependent leaching data and this paper is their response to this perceived gap within the currently available

literature commonly cited within the mining and minerals field. Napier-Munn [2] also considered similar

problems in analysing continuous plant data using the ANOVA technique.

MATERIALS AND METHODS

Oxidation of Sphalerite Mineral Sulphide Concentrate

A mixed mesophilk: culture (denoted by WJ in this paper) [3] was utilised at 30+2C for the oxidative

859

860 N. Powell and M. A. Jordall

dissolution of zinc from the mineral sulphide concentrate containing 53.3% Zn and 10.7% Fe. A 5%w/v

pulp density, in a nutrient salt solution, was prepared in a 250ml Erlenmeyer flask and autoclaved to sterilise

the flask contents. Each flask, except the control flasks which were inoculated with a 10%v/v solution of

thymol in methanol, were inoculated with a 10%v/v inoculum of the requisite culture. The nutrient salt

solution contained MgSO4.7H20 (0.4g/I), NH4SO 4 (0.4g/I), K2HPO4.3H20 (0.1g/l) and KCI (0. l g/1).

Each flask was sampled daily and the pH of the solution adjusted to predetermined level; pH ranges of

1.95-2.00, 1.55-1.60, 1.35-1.40 and 1.15-1.20 were used and adjustment was only attempted to the upper

limit i.e. if solution pH was below range then no pH adjustment was made.

Samples were stored at 4C prior to analysis by atomic absorption spectrophotometry (AAS).

EXPERI MENTAL RESULTS

Oxidation of the sphalerite concentrate with the mesophilic cultures, at variable starting solution pH values,

resulted in variable zinc leaching and recovery rates which are summarised in Table 1. Figures 1 and 2

show zinc concentration versus leaching time for each of the different starting solution pH values. The data

sets in Figure 1 have been interpreted using a set of French curves whilst the data sets in Figure 2 have

been fiited with a line derived using the mathematical technique of least squares regression.

TABLE 1 Summary of zinc leaching and recovery data from the sphalerite concentrate.

Starting

Solution pH

Maxi mum Rate of Zinc

Solubilisation (mg/l/hr)

French

Curve

Regression

Analysis

Control 0.8 0.5

1.0 7.7 5.4

1.2 9.5 6.9

Zinc

Recovery

(%)

8.0

21.8

25.5

1.4 28.2 18.0 56.7

1.6 37.1 18.0 50.4

During oxidation of the concentrate the solution pH in all flasks was noted to decrease i.e. solution acidity

increased, with the result that on termination of the experiment the solution pH in all flasks was < I. 1. Table

1 illustrates that for the experimental conditions investigated a starting solution pH value of 1.4 yielded

superior zinc recovery although the maximum rate of zinc leaching was lower than that of a starting solution

pH of 1.6. However, it should be noted that after 500 hours leaching the rate of zinc dissolution decreased

from 27.85 mgl/hr to 10.01 mg/1/hr resulting in a lower zinc recovery to solution. Based on these results

we would suggest that leaching the concentrate at a starting solution pH of 1.4 should maximise zinc

recovery from the concentrate. Optimisation of process parameters was not attempted.

ST AT ~ CALMET HODOLOGY

The statistical methodology on which the time-dependent nature of batch leaching data can be eradicated

is based on Ergun' s test[4] which assesses the equality of slopes. In the case presented the leaching data

for each test condition was fitted by a regression line and the gradients of each of these lines compared to

determine whether the gradients could be considered equal.

Had the data set presented simply consisted of independent columns of figures then to test for significant

Ba t c h l e a c hi ng da t a a ~ a l y s i s 861

differences betwe,~n them the appropriate statistical technique would be One-way Analysis of Variance

(ANOVA), which is j ust an extension of the t-test for means. However, the batch-leaching data presented

here is time-depe~'dent and thus violates a fundamental assumption of ANOVA (or of the non-parametric

alternatives). Time is effectively a third associated variable and it would appear that ' correction' of the

original data in some form is necessitated prior to conventional statistical testing.

16

Zi nc Concent rat i on (g/l)

12

I0

x

X

x

4

0

F

I I I I I I I I

50 150 250 350 450 550 650 750

Ti me ( Hours)

Ct l ( 1. 0 ) x WJ ( 1. 0 ) * WJ ( 1. 2 ) WJ ( 1. 4) x WJ ( 1. 6 )

Fig. 1 Zinc solubilisation from a sphalerite concentration using a mixed mesophilic culture.

To eradicate the time-dependency an obvious approach is to consider the rates of zinc extraction and to test

for differences between these for the varying solution pH values. The question then arises as to the time

period(s) over which the rates for the different pH values are to be compared. If ' small' time periods were

chosen (see Figure 3), for example, some form of numerical differentiation could be used to estimate the

rates but this might be considered unnecessarily involved.

On the other hand, file largest possible time period which can be chosen for calculation of a rate is of course

the range (in time) of the original data itself. The rate of metal dissolution for a particular solution pH (or

the control) then equates to the gradient or the slope of the linear regression line for that pH (The linear

regression line, in it.,; own fight, provides important information for interpolation and estimation purposes).

The appropriate tes! would then be an ' ANOVA for slopes' provided the linear correlation coefficients

862 N. Powell and M. A. Jordan

for the different pH' s were all deemed significant. Conveniently, although little-known, such a test does

exist, and is cited (as an exercise problem) in Draper and Smith [5]; the test appears to have been originally

proposed in Ergun [4]. The mathematical methodology is outlined below whereby the equality of the slopes

of a set of regression lines are tested;

16

14

12

10

Zi nc Conc e nt r a t i on ( g/ l )

X

X

!

Xx x

X x

X

X

-1

I I I I I I I I

50 150 250 350 450 550 650 750

Ti me ( Hou r s )

-'-- Ct l ( 1. 0) --x- WJ( 1.0) + WJ( 1. 2) ~ WJ( 1. 4) --x- WJ( 1. 6)

Fig.2 Regression lines for sphalerite leaching data.

Ergun' s test assesses (as a Null Hypothesis) the equality of the slopes 13 i of say, m lines, represented by

the models

= - + ( 1)

F or i = 1, 2 , . . mandj = 1,2 ..... n i.

It is supposed that n i bi-variate pairs (Til, Yil), (Ti2, Yi2)"..(Tini, Yin) are available for estimation of the

slopes of the i th line and further that the error or residual terms 8ij follow a N(O,o 2) distribution

Batch leaching data analysis 863

independently (The m variables T i will in the specific case-study here all be represented by a common

independent time-variate T).

Zinc Concentration ( g/ l )

7

6 -

4

0 I ' 1 I ! I I I I I

0 2 4 6 8 10 12 14 16 18 20

Time (Hours)

[ - - Metal Cone. (g/l) I

Fig.3 Illustration of rate determination concept for comparison of rates of metal leaching between data sets.

This method would involve the calculation of gradients between all data points on individual lines e.g.

gradients for the lines AB, BC, CD etc. The method proposed determines the gradient of the

regression line fitted to the whole data set and uses this as a basis for comparison between data sets.

The least-squares estimate of [~ is

n i

b . - j=l ( 2)

I n l

E (r

j=l

with sum of square.,; (1 degree of freedom)

n i

j=l

(3)

and Residual Sum of Squares (n i - 2 degrees of freedom)

864 N. Powell and M. A. Jordan

n i

RSS(bi ) = E (Y .i -Y i )2-SS(bi ) = si, say (4)

.j=!

If the Null Hypothesis that ~i = 6, say, for all i, is assumed true, then the least-squares estimate of I~ is

m n i

E E <; - ~)<,- ~)

b = i=l j=, (5)

m n i

E E <,-E)~

i=1 .j=l

with Sum of Squares (1 degree of freedom)

m " , t

ss{b) = b'~fE E <~i,-g) ~

i=1 j = l

I. J

and Residual Sum of Squares m

(~_, n i -2m degrees of f r eedom)

i=1

(6)

m ni

RSS<b) = E E <r,,-~y-ss<b)

i=1 j= l

= S, say.

(7)

Following calculation of these sum of squares an Analysis of Variance (ANOVA) table can be formed as

follows (see Tables 2 and 3).

T A BL E 2 Ge n e r a l A N O V A t a b l e f o r E r g u n ' s t e s t .

Source Degrees of

Freedom

Sum of Squares Mean Square F

b 1 SS(b) M,

" ( 7 )

AU bigiven b m-I ~, SS( b, ) - SSO ) M2 F~= M2

i=l

m

Residual ~ n~ - 2m by subtraction s 2

2

m ~ll 1 | 1

Total (TSS) n, - m ~"~ E (gl - g )

i = l i - | , l - I

Batch l e a c h i n g data analysis 865

The Null Hypothesis Ho: 13i= [3 is tested by comparing the statistic F 2 with an appropriate percentage point

F ,m-I

(tabulated) of the ~ n,-2m distribution. If H o is not rejected then b (Eq.5) is used as the common slope

of the lines.

TABLE 3 Case Study Data.

i T YI Y2 Y 3 Y 4 Y s

time C~l(1.0) WJ(1) WJ(1.2) WJ(1.4) WJ(1.6)

1 66 1.659 1.499 1.059 1.611 1.573

2 67 1.686 1.661 1.385 1.888 1.472

3 90 1.724 2.260 1.690 2.406 1.981

4 114 1.705 2.118 1.846 2.477 2.115

5 136.5 1.736 2.411 1.990 2.848 2.176

6 160.5 1.923 2.553 2.076 3.059 2.423

10

11

12

232.75

256.25

280.25

304.25

401

424

1.926

1.853

1.779

1.821

1.842

1.770

2.840

3.044

3.577

3.532

4.003

4.262

2.392

2.414

2.797

2.899

3.463

3.937

4.204

4.221

4.716

5.121

8.357

8.769

3.572

3.740

4.319

4.963

8.085

9.1'70

13 448 1.756 3.978 4.078 8.682 8.928

14 472 1.764 3.785 3.887 8.670 9.746

15 496 1.789 4.225 9.406 10.528 3.936

4.864 16 592 1.921 5.061 11.177 10.808

17 616 1.895 4.391 5.222 10.943 10.896

18 664 2.063 5.452 5.836 13.514 13.038

19 691 2.131 5.180 5.389 11.261 11.816

20 736 2.124 5.575 5.289 11.767 12.416

21 785 2.135 5.819 6.792 15.117 13.421

From the data

( T - T ) ( Y : - ~ ( I) = 555.884,

(T-T)(Y3-Z~;3) = 7625. 449,

(T-T)(Y2-'Fg2) = 5947. 159

( T- T) ( Y4- ' : ' 4) = 19450.483

: ~ ( T - T ) ( Y s - 3 : 5) = 20077.193,

5 21

E E (T-T)(Yij -~fi) = 53656. 168

ill j=l

Also see Table 4.

Now from the definition of sample variance,

866 N. Powell and M. A. Jordan

21

(Ti)-Ti) 2

j=l

20

= ( 235. 4937) 2 f or all i.

also since T = TI = T 2 = T 3 = T 4 = T 5 giving

21

E (Tij - Ti )

j=l

= 1109145. 655 f or all i

and taking the 'cross-product' sums given under the case study data (see Table 3) and Using Eq.2

555. 884

b I = = 0. 000501

1109145. 655

5947. 159

b 2 = = 0. 005362

1109145. 655

7625. 449

b 3 = = 0. 006875

1109145. 655

19450. 483

b 4 = = 0. 017536

1109145. 655

20077. 193

b~ = = 0. 018101

" 1109145. 655

Also

5 21

i=l j=l

= 5( 1109145. 655) = 55455728. 275

(8)

so using Eq 5.

53656. 168

b =

5545728. 275

= 0. 0096752248

(9)

TABLE 4 Means and Standard Deviations of Variables.

Variable

T

Yt

Mean Sample Standard Deviation

235.4937 3 8 2 . 5 0

1 . 8 5 7 2 0.14888 st

Y2 3.6541 1.29172

Y3 3.5122 1.63893

Y4 7.1530 4.19448

Y5 7.0089 4.33868

$2

$3

s4

S5

Batch leaching data analysis

Now considering the calculations necessary to form the ANOVA table (see Table 2) in turn;

From Eq.6

5 21

SS(b) = b 2 E E (T/j-T/)2 = ( 0"0096752248) 2( 5545728"27)

i=1 j= l

8 6 7

Then

5 21

iffil j= l

5

= 2o( s : )

i=1

= 20( 0. 148882+ .... 4. 338682) = 815. 578 f r om Tabl e 4

Next (see Table 5) using Eq.3

SS(bi) = 20bi 2( 235. 4937) 2

TABLE 5 Tabl e o f Sums of Square Values.

i

1

2

3

4

5

b, S$ (b~)

0.000501 0.278

0.005362 31.889

0.006875 52.424

0.017536 52.424

0.018101 341.075

Y. 7 8 9 . 0 7 3

So from Table 2, the ANOVA table for this Case study may be drawn up as in Table 6.

TABLE 6 ANOVA val ues f or Case Study Data.

Source Degrees of Sum of squares Mean Square F

Freedom

b 1 519.135 519.135 1860.7

All b~ given b 4 269.938 67.485 241.88

Residual 95 26.505 0.279

Total 100 815.578

In order to test the Null hypothesis: ~i = ~ for all i, the statistic F2=241.88. Consulting tables of the F-

distribution this is very highly significant (even at the 0.1% level) and therefore the Null Hypothesis must

clearly be rejected. (The statistic F 2 = 1860.70 would have been used to test whether ~ = 0 bad the

Hypothesis above been accepted).

The next stage is to calculate the equation of the (five) regression lines, using Equation 1 with the slopes

given by their respective estimates given in Eq.8. This is illustrated in Table 7 (means from Table 2).

HI K I 0: 1 - [

868 N. Powell and M. A. Jordan

TABLE

r i

0.749 (control) 1

0.978 2

0.988 3

0.984 4

0.983 5

7 Cal cul ated values of regression lines for Case Study Data.

Model using Eq. 8 Re-arranged Regression Equation

Y- 1.8572 = 0.00050 I(t - 382_5) Y = 1.6655675 + 0.00050It

Y- 3.6543 = 0.005362(t - 382_5) Y = 1.6.3335 + 0.005362t

Y- 3.5122 = 0.006875(t - 382_5 Y = 0.8825125 + 0.006875t

Y- 7.1530 = 0.017536(t - 382_5) Y = 0.44548 + 0.017536t

Y - 7.0089 = 0.018 ! 0 l(t - 382-5) Y = 0.0852675 + 0.01810 It

Note all non-control values of r (the correlation co-efficient) are highly significant even at the 0.1% level.

For purposes of reporting the calculated regression lines listed in Table 7, and determining the rate of zinc

solubilisation (see Table 1), these equations have been quoted to 2 significant figures (see Table 8).

The gradient and intercept values of each of the equations in Table 8 are ' small' . Hence the number of

decimal places quoted and used in the calculation of these are required to obtain the requisite degree of

accuracy. It should be evident that rounding of intermediate numerical values would have resulted in an

appreciable variation in the final equation.

TABLE 8 Fi nal reported val ues for cal cul ated regressi on equati ons

1

2

3

4

5

Report ed Regressi on

Equations

Y = 1.7 + 0.00050t

Y = 1.6 + 0.0054t

Y = 0.9 + 0.0069t

Y = 0.5-i- 0.018t

Y = 0.09 + 0.018t

DI SCUSSI ON

Ergun' s test has been applied to all the batch-leaching data with the initial null hypothesis that the slopes

of the (five) regression lines are equal. Since one of the regression lines will be fitted to the control data

the hope is obviously that this hypothesis will be rejected. I f this is the case then subsequent tests could be

carried out for differences between the rates for varying solution pH values if required. I f not then the

conclusion is that there is no difference between the control and test conditions (no further analysis

required). Figure 2 illustrates the regression lines for the case study data.

Using the procedure outlined there are statistically significant differences between the rates of zinc

extraction for the columns of data (although at this stage it may not be possible to say specifically where

the differences lie). It is evident when examining the regression equations that there is a difference between

the control data and the rest i.e. the sterile acid leach and the bio-catalysed leach (the latter having a positive

effect on metal leaching rate). I f this were the only question of interest a simplification might be to deal

with j ust two columns of data as before, one the control data as before, and the second containing the me.ans

of the' solution pH' columns at the chosen times i.e. Ergun' s test with i = 2.

Ergun' s test thus enables practioners to deal with similar time-dependent batch data; this is obviously useful

since the data will often be of this type. I f it is required to specifically test further the non-control columns

for difference in the rate of metal extraction from one solution pH, as it is in the case presented here where

we require to identify which solution pH value results in the maximum rate of metal solubilisation, then an

Batch leaching data analysis 869

extension to the procedure needs to be adopted.

The basis of analy,;is of data from a subsequent test or tests between regression lines representing different

solution pH value,,; may be dependent upon factors external to that of the data set. For example the co-

precipitation of zinc at solution pH values in excess of 1.5 has been noted[6] hence even though the rate

of zinc solubilisation may be maximised at a solution pH 1.6 operating constraints negate such conditions.

For the case study if we assume that co-precipitation of metals is not problematic, and the null hypothesis

states that the slop,~ of the regression lines to be tested are equal, then the next test would be to determine

whether or not this hypothesis holds for the control line and solution pH 1.6 line. If the hypothesis is

rejected then this would indicate that there is a significant difference between the rate of zinc extraction

when operating at a solution pH 1.6 and the control (note that the control in each case was the same

solution pH under biologically sterile conditions). A similar test could be carried out for each of the other

solution pH lines (versus the control) to prove that there was a beneficial effect following the introduction

of a Thiobacillus culture in to the leach solution.

More importantly is the scenario where there visually appears to be very little difference between two sets

of data e.g. the solution pH lines 1.2 and 1.4 in Figure 2. In such a case Ergun' s test would be applied to

these two data sets alone (excluding the control data from which both of these lines had previously been

proven to be signiticantly different) to assess whether to accept the null hypothesis that these lines were

equal. A result indicating that the null hypothesis was true would indicate no significant difference between

these two data sets For the two lines indicated Ergun' s test indicated that there was no difference.

The methodology o~atlined may be tailored to suit individual case studies where time-dependent data requires

analysis. Interpretation of the results from Ergun' s test can be based both on the data to be analysed and

other factors both raetallurgical and economic.

.

.

CONCLUSIONS

Eradication of time dependency from batch leaching data is a requirement prior to the application

of certain ~;tandard statistical techniques e.g. ANOVA.

Regression of batch data followed by ANOVA on the gradients of these regressed lines has been

shown/proven to differentiate between data sets for the case study presented. This technique should

be directly applicable to other instances where analysis of batch data is required.

.

2.

3.

.

5.

6.

REFERENCES

Jordan, M.A., Powell, N., Chin, C.K. & Phillips, C.V., Experimental Data Analysis: A Guide To

The Selection Of Simple Statistical Tests, Minerals Engineering, 10, No.3, 275-286 (1997).

Napier-Munn, T., Detecting Performance Improvements In Trials With Time-Varying Mineral

Processes - - Three Case Studies, Minerals Engineering, 8 No.8, 843-858 (1995).

Jordan, M.A., Barr, D.W. & Phillips, C.V., Iron and Sulphur Speciation and Cell Surface

Hydrophobicity during Bacterial Oxidation of a Complex Copper Concentrate, Minerals

Engineering, 6, Nos 8-10, 1001-1011 (1993).

Ergun, S., Application of the principle of least squares to families of straight lines, Industrial and

Engineering Chemistry, 48, 2063-2068 (Nov. 1956).

Draper, N. & Smith, H., Applied Regression Analysis (Second Edition), John Wiley & Sons Inc,

(New York), ISBN 0-471-02995-5, (1981).

Personal Communication, F.Pooley, Department of Materials Engineering., University of Wales,

College of Cardiff, (1995).

870 N. Powell and M. A. Jordan

ACKNOWLEDGEMENTS

The authors would like to thank The Institution of Mining & Metallurgy for financial assistance (1995

Stanley Elmore Fellowship Award to Dr M.A. Whitbread-Jordan).

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