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User Operation &

Maintenance Manual
Spectro-FTIR Oil Analyzer

160 Ayer Road Littleton, MA 01460 U.S.A. • Tel. 978.486.0123 • Fax 978.486.0030
email: service@spectroinc.com • web page: www.spectroinc.com

Manual Part No. FT2001


Spectro-FTIR User Operation & Maintenance Manual  |  i

Table Of Contents

1.0 INSTALLATION............................................................................................................. 1
1.1 SITE REQUIREMENTS................................................................................................. 1
1.2 SPECTRO-FTIR HARDWARE DESCRIPTION........................................................... 2
1.2.2 Internal Components of the Spectro-FTIR ...................................................................... 6
1.3 SPECTRO-FTIR HARDWARE INSTALLATION.......................................................... 7
1.3.1 Installing the Spectro-FTIR and the Base Cabinet............................................................ 7
1.3.2 Connecting the Spectro-FTIR to a Computer................................................................... 9
1.3.2.1 Stand-alone Configuration................................................................................................ 9
1.3.2.2 Spectro-FTIR and PC on a Network............................................................................... 10
1.3.2.3 Spectro-FTIR on a Network Computer.......................................................................... 10
1.4 SPECTRO-FTIR PLUMBING INSTALLATION......................................................... 11
1.4.1 Flow-Through Cell Plumbing......................................................................................... 12
1.4.2 Wedge Cell Plumbing..................................................................................................... 13
1.4.3 Manual Operation.......................................................................................................... 14
1.4.4 Automatic Operation...................................................................................................... 15

2.0 INITIAL SOFTWARE SETUP...................................................................................... 17


2.1 SETUP OF NETWORK CARD.................................................................................... 17
2.2 DISABLE VIRUS AND FIREWALL SOFTWARE......................................................... 19
2.2.1 Excluding Spectro-FTIR Software Program Directory from Virus Checking................... 19
2.2.1.1 Symantec Norton AntiVirus Corporate Edition.............................................................. 19
2.2.1.2 Symantec Norton AntiVirus Consumer Edition.............................................................. 19
2.2.1.3 McAfee VirusScan........................................................................................................... 20
2.2.2 Disabling Firewall Software............................................................................................ 20
2.2.2.1 Disable Internet Connection Firewall in Windows XP or Windows XP SP1................... 20
2.2.2.2 Disable Windows Firewall in Windows XP SP2.............................................................. 20
2.2.2.3 Norton Internet Security................................................................................................ 20
2.2.2.4 Norton Personal Firewall................................................................................................ 21
2.2.2.5 McAfee Internet Security................................................................................................ 21
2.2.2.6 McAfee Firewall.............................................................................................................. 21
2.3 OPUS SOFTWARE INSTALLATION AND CUSTOMIZATION............................... 21
2.3.1 Installing OPUS Software............................................................................................... 21
2.3.2 Registering OPUS.......................................................................................................... 23
2.3.3 Unlock Required Features............................................................................................... 25
2.3.4 Customize Measure Drop-Down Menu.......................................................................... 26
2.3.5 Disable FDA Compliance............................................................................................... 27
2.4 INSTALL SPECTRO-FTIR OIL ANALYSIS SOFTWARE........................................... 28
2.5 CONFIGURE OPUS WITH THE OIL ANALYSIS WORKSPACE FILE (Oil.xpm).... 29
2.6 SETUP OPUS VALIDATION PROGRAM FOR PQ AND OQ TESTS...................... 33

3.0 ROUTINE SAMPLE ANALYSIS................................................................................... 37


3.1 INTRODUCTION....................................................................................................... 37
3.2 DAILY DIAGNOSTIC TESTS...................................................................................... 38
3.2.1 Validate the Spectrometer, PQ Test................................................................................. 38
3.2.2 Calibrate Cell (New Cell Only - Does not Apply to Wedge Cells)................................... 39

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ii  |  Table of Content

3.2.3 Background Test............................................................................................................. 40


3.3 MANUAL SAMPLE MEASUREMENT........................................................................ 41
3.4 AUTOMATIC OPERATION........................................................................................ 44
3.4.1 Automatic Sample Analysis............................................................................................. 44
3.5 REPROCESS SPECTRA................................................................................................ 47
3.6 CREATING REPORTS................................................................................................. 48
3.7 PROGRAM OPTIONS................................................................................................. 49
3.7.1 Options Tab 1................................................................................................................ 49
3.7.2 Options Tab 2................................................................................................................ 51
3.7.3 Options Tab 3................................................................................................................ 52
3.7.4 Options Tab 4................................................................................................................ 53
3.8 ENGINE OIL PROPERTY CALIBRATION PROCEDURE........................................ 56
3.8.1 Introduction................................................................................................................... 56
3.8.2 Basic IR Subtraction Theory........................................................................................... 56
3.8.3 Step-by-Step Calibration Procedure................................................................................ 57
3.9 INTERPRETING SPECTRO-FTIR OIL ANALYSIS DATa......................................... 58
3.9.1 Introduction................................................................................................................... 58
3.9.2 Water Contamination..................................................................................................... 59
3.9.2.1 Water in Extreme Pressure (EP) Additive Fluids.............................................................. 59
3.9.2.1 Water in Synthetic Turbine Lubricants........................................................................... 59
3.9.3 Soot Contamination....................................................................................................... 59
3.9.4 Glycol Contamination.................................................................................................... 60
3.9.5 Fuel Contamination........................................................................................................ 60
3.9.5.1 Diesel Fuel Contamination............................................................................................. 60
3.9.5.2 Gasoline Fuel Contamination......................................................................................... 60
3.9.6 Degradation based on Nitration..................................................................................... 60
3.9.7 Degradation based on Oxidation.................................................................................... 61
3.9.8 Degradation based on Sulfation...................................................................................... 61
3.9.9 Lubricant Breakdown..................................................................................................... 62
3.9.9.1 Breakdown I Synthetic Lubricants.................................................................................. 62
3.9.9.2 Breakdown II Synthetic and Water in Petroleum Lubricants........................................... 62
3.9.10 Antiwear Reading (ZDDP) Additives ............................................................................ 62
3.10 SOLVENT REQUIREMENTS FOR THE SPECTRO-FTIR ....................................... 62

4.0 USER MAINTENANCE............................................................................................... 65


4.1 TROUBLESHOOTING................................................................................................ 65
4.1.1 All Power Supply LEDs are Off....................................................................................... 65
4.1.2 One Power Supply LED is Off........................................................................................ 67
4.1.3 No Data Transfer between Spectro-FTIR and the Computer.......................................... 67
4.1.3.1 The Green RX LED Does Not Light............................................................................... 67
4.1.3.2 The Green RX LED Lights but the Yellow TX Does Not................................................ 67
4.1.3.3 The SR LED Stays ON................................................................................................... 67
4.1.4 No Interferogram in the Check Signal Dialog................................................................. 68
4.1.5 Signal-to-Noise Ratio is Too Low................................................................................... 68
4.1.6 Insufficient Energy at the End of the Spectrum (High Wavenumbers)............................ 69
4.1.7 H2O Band Absorption is Too High................................................................................. 69
4.1.8 Spectral Resolution is not Reached................................................................................. 69

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Spectro-FTIR User Operation & Maintenance Manual  |  iii

4.1.9 Incorrect Abscissa (cm-1) Calibration............................................................................. 69


4.2 REPLACING AND REGENERATING THE DESICCANT IN A CARTRIDGE........ 70
4.2.1 Replacing the Detector Compartment Desiccant............................................................ 70
4.2.2 Replacing the Interferometer Compartment Desiccant................................................... 71
4.2.3 Desiccant Cartridge Regeneration Procedure.................................................................. 71
4.3 REPLACING THE IR SOURCE................................................................................... 71
4.4 REPLACING THE WINDOWS................................................................................... 72
4.5 REPLACING FUSES..................................................................................................... 74
4.6 FILTER REPLACEMENT AND CLEANING.............................................................. 74

WARNING!!!
High Voltages are Present During the Operation of the
Spectro-FTIR !

Observe all Safety Precautions!

Turn OFF the Main Power Switch and unplug the


Spectro-FTIR before any work is performed.

Definitions

The following definitions apply to specific instructions throughout this manual.

WARNING!!!
An operating procedure or practice that may cause injury if not carefully observed or
followed.

CAUTION!!!
An operating procedure or practice that may cause damage to the Spectro-FTIR if not
carefully observed or followed

NOTE!!!
An operating procedure or practice that is essential to emphasize

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iv  |  Table of Content

Revision History

Original v.1.0 21 November 2008, First Issue


Change 1 v.1.1 Review and technical edit. Added automatic operation plumbing and additional software
features.
Change 2 v.1.2 Added wedge cell option.

Total Number of pages in this manual is 82 consisting of the following:

Description Page # of Pages


Covers 2
Table of Contents i-iv 4
Chapter 1 1-16 16
Chapter 2 17-36 19
Chapter 3 37-64 27
Chapter 4 65-76 11

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Spectro-FTIR User Operation & Maintenance Manual  |  1

Chapter 1 1.0 INSTALLATION

The Spectro FT-IR Oil Analyzer, Figure 1.0-1, is


specifically designed for the molecular analysis of
lubricating oil to determine oil degradation and
contamination. It was developed and optimized

Installation for predictive maintenance programs according


to JOAP, ASTM E2412 and DIN standards for
the rapid determination of oxidation, nitration,
sulfation, water, coolant, fuel dilution, soot, wear
additive depletion and synthetic lubricant break-
down in used lubricating oils.

When coupled with an optional AutoSampler, the


Spectro FT-IR Oil Analyzer is ideal for condition
monitoring laboratories with large sample loads.
The system is easy to use and requires little train-
ing for operation since it is optimized for one ap-
plication: used oil analysis. It features continuous
online diagnosis of all spectrometer components
and automatic control of selected measurement
parameters.

The Spectro-FTIR is a bench-top instrument that


requires little counter space for operation. This
chapter details the installation and operational
requirements for routine sample analysis. It also
describes the major components and assemblies
to familiarize the operator with the instrument.

1.1 SITE REQUIREMENTS

The site where the Spectro-FTIR is setup for op-


eration must be properly planned and prepared to
optimize the analysis of oil samples. To save time
during installation, the site can be prepared prior

Figure 1.0-1, Spectro-FTIR Oil Analyzer

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2  |  Chapter 1 Installation

to the arrival of the Spectro-FTIR, or it can be Disk, (2) RJ-45 Ethernet ports. With an
performed at the same time. English operating system of either; Windows
XP or Windows 2000.
The Spectro-FTIR is a bench-top instrument and • Recommended Solvent: Pentane, see Section
can be placed on a laboratory counter or a sepa- 3.10.
rate table. The comfort of the operator must also • Waste Container (for oil & solvent): The
be considered if samples are to be analyzed for waste container must be corrosive resistant,
long periods of time. The physical requirements non-pressurized and located below the FTIR.
for the laboratory are as follows: • Purged Gas Option (available for humid
environments): Dried compressed air or
• Location: The Spectro-FTIR must be placed nitrogen regulated at 6-9 Psi.
on a level surface.
• It is always good practice to place instruments Important Consideration:
away from windows or doors where direct To provide for good data quality and a long spec-
sunlight or drafts could cause temperature trometer service life, ensure that the following site
fluctuations. requirements are met:
• General Space Requirements: Dimensions
are: 66.5 x 43.4 x 28.1 cm (26 x 17 x 11 • Do not install the spectrometer near sources
inches at a weight of 37kg (82 lbs.). of potential inductive electrical interference
• Operating Temperature: Minimum to (e.g. pumps, switching motors, microwave
maximum 18-35˚C (64-95˚F). Temperature ovens etc.), sources of high energy pulses, and
fluctuations of more than 1 ˚C shift during a sources that might cause magnetic or radio
sample measurement and 2˚C shift between frequency interference.
background measurements are not recom- • Do not place devices such as large electric
mended for optimum accuracy and repeat- motors, heaters, welding equipment, radio
ability. transmitting equipment, units emitting
• Humidity: For optimum performance life the pulsed NMRs, or high powered lasers in close
operational relative (non-condensing) humid- vicinity to the spectrometer. These devices
ity should be ≤ 80%. An optional purge kit can interfere with the spectrometer and cause
is available for high humidity environments. spectrometer malfunction. Ensure that these
types of devices are not connected to the
IMPORTANT NOTE: The Spectro-FTIR must same electrical circuit as the spectrometer.
be placed as far away as possible from any sources • If there are any problems concerning main
of vibration within the confines of the laboratory. power supply (e.g. brownouts, power surges,
Due to the sensitive nature of the instrument, the frequent thunderstorms), take precautions to
unit should isolated from any source of vibration ensure an uninterruptible power supply.
during analysis (Spectroil M, ventilation hoods,
motors elevators, air conditioners, etc. 1.2 SPECTRO-FTIR HARDWARE
DESCRIPTION
The resources and facilities external to the Spec-
tro-FTIR that are required for operation are: This chapter identifies the main components of
Minimal Electrical Requirements: 100-240 VAC the Spectro-FTIR. The user should become fa-
±10%, 50-60 Hz. miliar with the terminology in order to make it
easier to understand the operational and mainte-
• Computer (when not supplied by Spectro nance functions of the instrument as described in
Inc): Minimum requirements are Pentium this manual.
2 @800 MHz, 128MB RAM, 10GB Hard

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Spectro-FTIR User Operation & Maintenance Manual  |  3

Source/Laser
Compartment
Electronic Interferometer
Compartment Compartment

Detector AutoSampler
Compartment

Sample
Compartment

Figure 1.2-1, Main Components of Spectro-FTIR


The main compartments of the Spectro-FTIR are The entire cover is lifted from its bottom edge to
shown in Figure 1.2-1. The external and internal open the whole sample compartment. The cov-
components are described in the next two sec- er must be in the up position during routine oil
tions of this chapter. sample analysis. To extend spectrometer life re-
move the cell and keep the cover closed to protect
1.2.1 External Components of the Spectro- the optics when the instrument is not in use.
FTIR
This section of the manual has a brief description Status Indicator Display
of each of the Spectro-FTIR’s main components. The Spectro-FTIR status indicator display is lo-
cated in the rear right corner of the spectrometer,
Sample Compartment Figure 1.2-3. The display provides the user with a
The sample compartment has two access doors; general indication of the humidity level inside the
one from the top and the other from the front of spectrometer, the operating status of the laser, and
the spectrometer, Figure 1.2-2. The handle can the general spectrometer status.
be used to open the top lid of the sample com-
partment. This lid is intended for installing high Humidity Indicator – Detector Compartment
accessories into the sample compartment or ex-
changing the sample for applications other than This indicator lamp lights up red if the humidity
oil analysis. level inside the detector compartment is too high
and the desiccant cartridge needs to be replaced.
Compartment Cover Top Lid

Figure 1.2-2, Sample Compartment Doors Figure 1.2-3, Status Indicator Display

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4  |  Chapter 1 Installation

Otherwise, this indicator is normally OFF. Spectro-FTIR Rear Side


The rear of the Spectro-FTIR has two panels, the
Humidity Indicator – Interferometer electronics panel and the power supply panel,
Compartment Figure 1.2-4. As the names imply, the electron-
This indicator lamp lights up red if the humid- ics panel contains cable connections for commu-
ity level inside the interferometer compartment nications and instrument status and diagnostic
is too high and the desiccant cartridge needs to LEDs. The power supply panel contains LEDs to
be replaced. Otherwise, this indicator is normally indicate power supply status, fuses and the main
OFF. power connection and switch. The primary com-
ponents of the panels are described below:
Laser Indicator
The laser indicator lamp lights up yellow when Electronics Panel
the laser is in operation. ERR LED - The red ERR LED indicates an in-
terferometer error (e.g. a missing laser signal). As
long as this LED lights, data acquisition is not
Status Indicator
possible. The LED must be out for proper opera-
A green STATUS indicator lamp indicates that
tion.
the Spectro-FTIR is in proper operating condi-
tion. It lights up red if the spectrometer malfunc-
FWD LED - The yellow FWD LED indicates the
tions or is still in the initialization phase.
current interferometer mirror movement. As long
as the interferometer mirror moves forward this
IR Beam Outlet Port
yellow LED lights. During the backward move-
The IR beam outlet port is located on the right
ment the LED does not light. Thus, the LED
hand side of the Spectro-FTIR, Figures 1.2-2 and
flashes in the rhythm of the interferometer mirror
1.2-3. It provides a means to attache external
forward and backward movement. This rhythm
accessories. This port is not used in routine oil
depends on the chosen measurement parameters
analysis applications.
(e.g. resolution and velocity). (The abbreviation
FWD stands for ’forward’.)
COM 1 PORT LPT 1 PORT

ERR LED POWER


SUPPLY
FWD LED LEDs
+5 V
+12 V
TKD LED -12 V

MPE 1 PORT
CAN BUS
CONNECTOR
SR LED W
and
MAIN POWER
SG LED
SWITCH
RES BUTTON
FUSE BLOCK
TX LED
and
RX LED

PRIMARY POWER
ETEHRNET PORT
RECEPTACLE
Figure 1.2-4, Spectro-FTIR REar View

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Spectro-FTIR User Operation & Maintenance Manual  |  5

that a data packet is transmitted on the Ethernet.


TKD LED - The green TKD LED indicates that This does not necessarily mean that the data packet is
the interferometer mirror is within the data ac- destined for the spectrometer! The yellow TX LED
quisition range. Typically, it flashes with twice lights if the spectrometer transmits a data packet.
the frequency and synchronous to the FWD This indicates that the spectrometer is accessed by
LED. During data acquisition the light intensity a computer.
changes to bright green. (The abbreviation TKD
stands for ’take data’.) NOTE: Use these LEDs to test the operational
reliability of the Ethernet connection.
MPE 1 PORT - The MPE 1 is a versatile port
to connect external optical modules and detec- ETHERNET PORT - The ETH port is primar-
tors. It includes a complete CAN bus, transmits ily used to connect the spectrometer to a com-
all required remote trigger signals and establishes puter on which the Spectro Oil Analysis applica-
a complete connection to DDC (Digital Detector tion software is installed. The spectrometer can
Connection) compatible detectors. An identical be connected either to a 10Base-T intranet or
connection can be found on every optical module directly to the computer using a cross-over cable
port in front or on top of the instrument. (stand-alone configuration).

COM1 PORT - The COM1 port is technical- Power Supply Panel


ly similar to a conventional, PC-compatible se-
rial port, however, it does not have the complete POWER SUPPLY LEDS ( + 5 V , +12V, - 12V)
functionality like serial port of a PC. It is only - These LEDs indicate the state of the secondary
used for special applications. voltages of the electronics unit.
Note: A dark power supply LED indicates a major
LPT1 PORT - This port is reserved for diagnostic electronics problem.
purposes. Do not connect any devices to this port!
(The abbreviation LPT stands for ’Line Printer’.) CAN BUS CONNECTOR - The CAN bus con-
SR LED AND SG LED - These two LEDs (red nector is primarily used to connect external au-
SR LED and green SG LED, indicate the internal tomated units (e.g. sample changer, moving mir-
operating state of the spectrometer communica- ror unit, etc.) to the spectrometer. The CAN bus
tion processor. (The abbreviation SR stands for also provides power to these units. Thus, most
’Status Red’ and SG for ’Status Green’.) external units can be operated without connect-
ing them to the power supply. Furthermore, the
RES BUTTON - The spectrometer is equipped CAN bus can be used as a communication link
with a reset button similar to the one you know to control these external units via the spectrom-
from a PC. Pressing this button longer than 1 eter. (The abbreviation CAN stands for Control-
second resets the spectrometer without the need ler Area Network.)
to turn it off. The effect is identical to switching
the spectrometer off and on again. MAIN POWER SWITCH - The main power
switch is used to switch the spectrometer ON and
TX LED AND RX LED - These LEDs indicate OFF. This switch interrupts the primary voltage
the data transfer between the spectrometer and supply.
the data system via the Ethernet connection. In
case of the stand-alone configuration, the green CAUTION: After switching the spectrometer
RX LED signals that the spectrometer receives off, wait at least 30 seconds before switching the
data. In case the spectrometer is connected to an spectrometer on again. This measure avoids peaks
Ethernet network, the green RX LED indicates in the initial current which could lead to fuse

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6  |  Chapter 1 Installation

blowing and/or damaging the power switch.


Detector - The standard spectrometer configura-
FUSE BLOCK - The fuse block contains two tion is equipped with a DigiTect™ DLATGS de-
fuses. See Section 4.7 for the fuse replacement tector with integrated preamplifier. This detector
procedure. package contains an analog-to-digital converter
that converts the analog signal from the detector
PRIMARY POWER RECEPTACLE - Connect directly into a digital signal. This digital signal
the supplied power cord to the primary power re- is transmitted to the data processing electronics
ceptacle at the spectrometer rear side as well as to unit of the spectrometer. The standard detector is
the mains socket outlet. a DLaTGS detector which covers a spectral range
from 12,000 to 370cm-1 and operates at room
1.2.2 Internal Components of the Spectro- temperature. The detector is mounted on a dove-
FTIR tail guide which allow an easy interchange.
This section identifies and briefly describes the in-
ternal components of the Spectro-FTIR as shown Beam Splitter – The beam splitter is made of
in Figure 1.2-5. potassium bromide (KBr). It is installed at the
factory and if defective, it must be replaced by a
IR Source - The MIR source is a globar (i.e. an U- qulified Spectro Inc. service technician.
shaped silicon carbide piece) that emits middle-
infrared light. Laser – The Spectro-FTIR is equipped with
a HeNe laser. This laser emits red light with a
NOTE: To gain access to the interferometer and wavelength of 633nm. The rated power output
detector compartments, a 6mm Allen wrench is 1mW. The laser controls the position of the
is provided with the instrument to remove the moving interferometer mirrors (also called ’scan-
covers. See Section 4.2 for the procedure to open ner’) and is used to determine the data sampling
these covers. positions. The monochromatic beam produced
by the HeNe laser is modulated by the interfer-
Laser Module
(Including Power Supply)

IR Source

Detector

Beam
Splitter

Desiccant Desiccant
Cartridge Cartridge
Figure 1.2-, Internal Components of the Spectro-FTIR

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Spectro-FTIR User Operation & Maintenance Manual  |  7

ometer to generate a sinusoidal signal. tion 1.4)


• Base Cabinet Assembly
Interferometer – The Spectro-FTIR is equipped • LNF Sipper and Mount (not required for
with a high stability interferometer with ROCK- automatic system)
SOLIDTM permanent alignment. The ROCK- • Vibration Strips
SOLIDTM interferometer incorporates dual • User Manual
retroreflecting cube corner mirrors in pendulum
arrangement. The high throughput design en- 1.3.1 Installing the Spectro-FTIR and the
sures the highest possible signal-to-noise ratio. Base Cabinet
1. Befor proceding, verify that the environ-
Desiccant Cartridge – The Spectro-FTIR is mental and utilities Site Requirements detailed
equipped with two desiccant cartridges; one in in Section 1.1 have been met.
the detector compartment and the other in the in-
terferometer compartment. The purpose of these 2. The Spectro-FTIR System consists of the
desiccant cartridges is to keep the air humidity Spectro-FTIR and the Base Cabinet Assembly.
level inside the interferometer compartment and Place the Base Cabinet Assembly on the bench
the detector compartment low. (Note that a high where the instrument will be operated.
air humidity level inside the spectrometer causes
damage to the spectrometer optics). 3. Vibration strips are installed between the
Base Cabinet and the Spectro-FTIR as shown
1.3 SPECTRO-FTIR HARDWARE in Figure 1.3-1. Note that the holes on the
INSTALLATION side strips must be aligned as shown at the top
of the figure.
Your local Spectro Inc. representative usually
carries out unpacking and installation of your 4. Install the left and right vibration strips so
Spectro-FTIR. The process is, however straight they align with the rear holes.
forward providing a qualified technician follows
the steps listed in this section. The steps refer to 5. Place the rear vibration strip onto the top
a Spectro-FTIR for manual operation, however, rear of the Base Cabinet between the side
notes are provided where the procedure differs for strips.
a Spectro-FTIR with an AutoSampler. 6. Carefully set the Spectro-FTIR onto the
Base Cabinet Assembly into the four holes on
The standard components delivered with the the two side vibration strips
Spectro-FTIR are:
CAUTION: The weight of the Spectro-FTIR is
• Spectro-FTIR approximately 37 kg (82 lbs). Due to its weight,
• Power cord two personnel should lift it onto the Base Cabinet
• Peristaltic Pump (additional pump or auto- Assembly.
matic system)
• Easy Load Pump Head for Peristaltic Pump 7. Before connecting the power cord, make
• Computer Sytem sure the Spectro-FTIR is switched “OFF” at
• Data cable (10Base-T cross-over cable) the main power switch at the rear of the instru-
• OPUSTM Software ment. Connect the supplied power cord to
• FT-IR Oil Analysis Software the primary power receptacle at the rear of the
• Basic Hand Tools instrument and the other end to main power
• System Spares Kit outlet.
• Sample Introduction Plumbing Kit (see Sec-

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8  |  Chapter 1 Installation

Figure 1.3-1, Installation of the Vibration Strips


CAUTION: The power cord cannot exceed 3 10. For manual systems, attach the sipper tube
meters (9 feet) in length. assembly to the front right side of the Base
Cabinet with the two provided screws, Figure
8. Attache the Easy Load Pump Head to the 1.3-3. This assembly is not required for auto-
Peristaltic Pump with the two provided screws. matic operation; however, it is good practice to
install it at this time in case a decision is made
9. Place the Peristaltic pump on the top front to revert to manual operation.
right corner of the Spectro-FTIR as shown in
Figure 1.3-2. Make sure the pump is switched 11. If the optional purge gas kit has been or-
“OFF” at its main power switch and connect dered with the Spectro-FTIR, attach the purge
the power cord to a power. gas hose, Figure 1.3-4 to the dried compressed
air or nitrogen supply. Set the flow rate to 6-8

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Spectro-FTIR User Operation & Maintenance Manual  |  9

Figure 1.3-4, Optional Purge Hose Attachment


liters per hour. High air humidity levels inside
the Spectro-FTIR compartments will damage
the optics. It is therefore highly recommended
that the purged gas remain on even when the
instrument is not in operation.

12. This completes the hardware installation


procedure of the Spectro-FTIR.

1.3.2 Connecting the Spectro-FTIR to a


Computer
The Spectro-FTIR is connected to a computer
(PC) through an Ethernet cable. There are three
connection topologies to choose from depending
on your laboratories’ requirements.
Figure 1.3-2, Recommended Location for
Peristaltic Pump a. Stand-alone Configuration (Standard)
b. Spectro-FTIR and its PC connected to a
network
c. Spectro-FTIR connected to a network com-
puter

The Ethernet cable used to connect the Spectro-


FTIR to a PC depends on the selected topology.
A cross-over cable is required for the stand-lone
configuration and a standard cable for all others.
The difference in Ethernet cables is shown in Fig-
ure 1.3-5.

Attach with Two 1.3.2.1 Stand-alone Configuration


Provided Screws This is the standard configuration where the Spec-
tro-FTIR is connected to a PC, i.e. neither the
Figure 1.3-3, Sipper Tube for Manual Sample Spectro-FTIR or the PC are part of a network.
Analysis This configuration requires a cross-over cable to
connect the Spectro-FTIR to the PC as shown in

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10  |  Chapter 1 Installation

1 1 1 1
2 2 2 2
3 3 3 3
4 4 4 4
5 5 5 5
6 6 6 6

Standard Ethernet Cable Cross-over Ethernet Cable


Figure 1.3-5, Ethernet Cables Used in Spectro-FTIR Copmuter Topologies

Figure 1.3-6. The cable is connected to the Ether- Ethernet Hub

net connector on the Spectro-FTIR and the other Standard


end to the network card Ethernet RJ-45 connec- Ethernet Cables

tor on the PC.

The stand-alone configuration has the following


advantages and disadvantages:
Personal Personal Spectro-FTIR
Computer 1 Computer 2
Advantages:
• Easy to install Figure 1.3-7, Spectro-FTIR & PC on a Network
• Full bandwidth available for the data transfer
The stand-alone configuration has the following
between Spectro-FTIR and PC.
advantages and disadvantages:
• No access conflicts with other PCs that may
try to access Spectro-FTIR as well.
Advantages:
• No data transfer rate problems.
• Remote access to Spectro-FTIR via internet
or the intranet is possible.
Disadvantages:
• The PC can access to all network resources
• No remote access to Spectro-FTIR from
(provided you have the corresponding access
other PCs on which OPUS is installed.
rights).
• No computer network connection
• A local printer is required to print out the
Disadvantages:
measurement results.
• Your network administrator must be involved
in configuring the connection.
1.3.2.2 Spectro-FTIR and PC on a Network
• Only a fraction of the bandwidth is available
In this configuration, both the Spectro-FTIR and
for the data transfer between Spectro-FTIR
its PC are connected directly to a network. Stan-
and PC. Due to data transmission delays, the
dard Ethernet cables are used in this configura-
measurement time may increases.
tion to connect both systems to a network hub,
• Access conflicts caused by other PCs that try
Figure 1.3-7.
to access Spectro-FTIR as well.

Cross-over 1.3.2.3 Spectro-FTIR on a Network Computer


Ethernet Cable
This configuration combines the advantages of
the other two configurations, however, it requires
Personal Computer Spectro-FTIR additional hardware and is the most difficult to
10.10.0.100 10.10.0.1 install. The configuration is shown in Figure 1.3-
Figure 1.3-6, Stand-alone Configuration 8.

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  11

Ethernet Hub cells differs slightly and the installation of both


alternatives are described in this section.
Standard
Ethernet Cable
1.4.1 Flow-Through Cell Plumbing
Locate the parts listed below to assemble and in-
stall the flow-through cell sample introduction
Cross-over
Ethernet Cable
system.
Spectro-FTIR
Personal Computer

Figure 1.3-8, Spectro-FTIR & PC on a Network • P/N FT2030 Flow-Through Cell


• P/N FT2037 Valve 25 PSI Flow Cell Assem-
bly (Pressure Relief Valve)
The stand-alone configuration has the following
• P/N FT2032 Input Tubing Assembly
advantages and disadvantages:
• P/N FT2033 Drain Tubing Assembly
• P/N ASP118 Carboy Assembly (Waste Con-
Advantages:
tainer)
• Full bandwidth available for the data transfer
• For automatic operation, additional tubing
between Spectro-FTIR and PC.
and a second peristaltic pump are supplied.
• Remote access to Spectro-FTIR via internet
or intranet is possible (provided you have the
A completed sample introduction system for the
corresponding access rights).
flow-through cell is shown in Figure 1.4-1a. Fol-
• The PC can access to all network resources
low the steps below to assemble the sample this
(provided you have the corresponding access
introduction system.
rights).
• Different data transfer rates for the data
1. Locate the Flow-Through Cell, P/N
exchange between Spectro-FTIR (10Base-T)
FT2030 and install it by sliding it into the
and the network (no restriction) are possible.
right hand side of standard 2x3 inch cell
holder. The cell should easily slide in from the
Disadvantages:
top.
• Your network administrator must be involved
in configuring the connection.
NOTE: It may be easier to install the tubing
• A second network interface card (supplied
with the cell holder removed. To remove the cell
with the instrument) is required for the PC
holder, push the lever on the floor of the compart-
controlling the spectrometer.
ment away from you and lift out the holder.
1.4 SPECTRO-FTIR PLUMBING
2. Locate and unpack the Flow -Through Cell
INSTALLATION
Assembly (Pressure Relief Valve) Assembly P/N
FT2037.
When the Spectro-FTIR is first setup as described
3. Connect the Drain Tubing Assembly P/N
in Section 1.3, sample introduction plumbing
FT2033 to the output connection of the Valve
must be installed and connected to carry the oil
Assembly using the ½ turn Leuer-Lock con-
from its sample bottle to the Spectro-FTIR for
nector.
analysis.
WARNING: Avoid over torquing the fittings to
There are two different sample cells for the Spec-
avoid strpping them.
tro-FTIR. Older instruments tend to have the
standard flow-through cell, and more recently,
4. Connect the Input Tubing Assembly P/N
Spectro has made available a wedge cell that re-
FT2032 to the input connection of the Valve
quires no fringe correction. The plumbing for the

1 May, 2009 / v.1.2


12  |  Chapter 1 Installation

Figure 1.4-1a, Spectro-FTIR Flow-Through Cell Sample Introduction System


Assembly using the ½ turn Leuer-Lock con- nector.
nector. 7. Place the peristaltic pump on the top right
5. Install the first stage of the Valve Assembly front right corner of the Spectro-FTIR. In-
P/N FT2037 to the Flow Cell input using the stall the pump head with the two provided
½ turn Leuer-Lock connector. screws. Open the peristaltic pump by moving
6. Connect the tubing from the second stage its handle from the left side to the right hand
of the Valve Assembly to the Flow Cell output side. Place the peristaltic pump tubing (black
connection using the ½ turn Leuer-Lock con- section) into the peristaltic pump. Close the

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  13

peristaltic pump by moving its handle from the 1.4.2 Wedge Cell Plumbing
left side to the right hand side when you are Locate the parts listed below to assemble and in-
ready to analyze samples. stall the wedge cell sample introduction system.

NOTE: It is good practice to open the pump to • P/N FT2042 Wedge Cell
take pressure off the tubing when the Spectro-FT- • P/N FT2046 Valve 25 PSI Wedge Cell As-
IR is not in use. This extends the life of the tube sembly (Pressure Relief Valve)
and avoids tube deformation. • P/N FT2032 Input Tubing Assembly
• P/N FT2033 Drain Tubing Assembly
8. Plug the pump power connector into the • P/N ASP118 Carboy Assembly (Waste Con-
appropriate power outlet (110 or 220 VAC). tainer)
9. Connect and RS 232 cable from the RS • For automatic operation, additional tubing
232 Input connector on the back of the sample and a second peristaltic pump are supplied.
introduction pump, Figure 1.4-7, to the
COM 1 port on the PC. A completed sample introduction system for the
flow-through cell is shown in Figure 1.4-1b. Fol-
For manual operation and sample analysis, pro- low the steps below to assemble the sample this
ceed with Section 1.4.3 introduction system.

For automatic operation with an AutoSampler 1. Locate the Wedge Cell, P/N FT2042 and
proceed with Section 1.4.4. install it by sliding it into the right hand side
of standard 2x3 inch cell holder. The cell
should easily slide in from the top.

Wedge Cell
FT2042

Cell Input Tubing


Cell Output Tubing (Part of Wedge Cell)
(Part of Wedge Cell)

Drain Tubing Assembly


FT2033

Pressure Relief Valve


FT2046
Input Tubing Assembly
FT2032

Figure 1.4-1b, Spectro-FTIR Wedge Cell Sample Introduction System

1 May, 2009 / v.1.2


14  |  Chapter 1 Installation

NOTE: It may be easier to install the tubing 232 Input connector on the back of the sample
with the cell holder removed. To remove the cell introduction pump, Figure 1.4-7, to the
holder, push the lever on the floor of the compart- COM 1 port on the PC.
ment away from you and lift out the holder.
For manual operation and sample analysis, pro-
2. Locate and unpack the Wedge Cell As- ceed with Section 1.4.3
sembly (Pressure Relief Valve) Assembly P/N
FT2046. Install it by pressing it into the clip For automatic operation with an AutoSampler
on the floor of the sampling compartment. proceed with Section 1.4.4.
3. Connect the Drain Tubing Assembly P/N
FT2033 to the output connection of the Valve 1.4.3 Manual Operation
Assembly using the ½ turn Leuer-Lock con- 1. Connect the free end of the Input Tubing
nector. Assembly to the Sipper Tube Assembly, Figure
1.4-2.
WARNING: Avoid over torquing the fittings to 2. Connect the free end of the Drain Tubing
avoid strpping them. Assembly to the Waste Container ASP118.
Additional tubing may be required depending
4. Connect the Input Tubing Assembly P/N on the proximity of the Waste Container to the
FT2032 to the input connection of the Valve Spectro-FTIR.
Assembly using the ½ turn Leuer-Lock con-
nector. NOTE: The ideal location for the waste con-
5. Connect the wedge cell input tubing to the tainer is on the floor below the Spectro-FTIR. In
first stage of the Valve Assembly P/N FT2046 all instances, it must be located lower than the
input using the ½ turn Leuer-Lock connector.
6. Connect the wedge cell output tubing to
the second stage of the Valve Assembly P/N
FT2046 input using the ½ turn Leuer-Lock
connector.
7. Place the peristaltic pump on the top right
front right corner of the Spectro-FTIR. In-
stall the pump head with the two provided
screws. Open the peristaltic pump by moving
its handle from the left side to the right hand
side. Place the peristaltic pump tubing (black
section) into the peristaltic pump. Close the
peristaltic pump by moving its handle from the
left side to the right hand side when you are
ready to analyze samples.

NOTE: It is good practice to open the pump to


take pressure off the tubing when the Spectro-FT-
Sipper Tube
IR is not in use. This extends the life of the tube Assembly
and avoids tube deformation.

8. Plug the pump power connector into the


appropriate power outlet (110 or 220 VAC).
9. Connect and RS 232 cable from the RS Figure 1.4-2, Sipper Tube Assembly for Manual
Operation

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  15

Spectro-FTIR so that waste oil sample and sol- Tubing will have to be cut to length depending
vent flow to the Waste Container due to gravity. on the location of the components. Additional
pieces of tubing will be required to connect to
3. This completes the manual sample plumb- the Waste Container, one-way valve and to the
ing setup of the Spectro-FTIR. solvent reservoir on the AutoSampler.
3. Connect a piece of tubing between the “T”
1.4.4 Automatic Operation connector and the waste container.
1. A filter is installed between the sample 4. Cut tubing to size and install the one-way
introduction peristaltic pump and the AutoS- valve into the tubing going to the AutoSampler
ampler sipper tube, Figure 1.4-3. Connect a solvent reservoir. Note that the fluid flow is in
short piece of tubing to the input side of the the direction as shown on Figure 1.4-4. This
filter and a longer piece between the output keeps the oil sample from flowing into the
of the filter and the AutoSampler sipper tube. solvent reservoir on the AutoSampler.
2. Connect the free end of the Drain Tubing 5. Connect the other end of the tubing from
Assembly to the ‘T” connector, Figure 1.4-4. the one-way valve to the top connection on the
solvent reservoir, Figure 1.4-5.
6. Place the second peristaltic pump used for
pumping solvent to the AutoSampler beneath
the first pump as shown in Figure 1.4-6.
7. Open the solvent peristaltic pump by mov-
ing its handle from the left side to the right
hand side. Place the peristaltic pump tub-
ing (black section) into the peristaltic pump.
Close the peristaltic pump by moving its
Solvent Reservoir Waste Output Connection

Figure 1.4-3, Sipper Tube Assembly for


Automatic Operation

To Solvent Reservoir
on AutoSampler

Solvent Flow

One-Way Valve

Drain Tubing
from Sample
‘T” Connector
Compartment

To Waste Container Solvent Input Connection

Figure 1.4-4, ‘T” Connection and One-Way Figure 1.4-5, Waste Tubing Connection to the
Valve Solvent Reservoir

1 May, 2009 / v.1.2


16  |  Chapter 1 Installation

the solvent pump to “Remote”.


12. The only recommended solvent is pen-
tane. Initially set the solvent pump speed to
130 (1 on the outer dial and 30 on the inner
dial). The setting may have to be adjusted up
or down depending on the rinse cycle perfor-
mance,
13. This completes the automatic operation
sample and solvent plumbing setup.

Figure 1.4-6, Location of Solvent Pump and


Tubing Connections
handle from the left side to the right hand side
when you are ready to analyze samples.
8. Connect the left-hand side of the black
pump tubing to the solvent supply and the
right-hand side to the AutoSampler solvent
input connector, Figure 1.4-5.
9. Plug the pump power connector into the
appropriate power outlet (110 or 220 VAC).
10. The solvent pump is slaved to the sample
pump. Connect the RS 232 Interface cable
from the back of the solvent pump to the ter-
minal strip on the back of the sample pump as
shown in Figure 1.4-7.
11. Set the Remote/Local switch on the back of

RS-232 Cable to Solvent Main Power


Cable to PC Peristaltic Pump Connection
“Interface”
Connector”
Figure 1.4-7, Connections at the Rear of the
Sample Pump

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  17

Chapter 2 2.0 INITIAL SOFTWARE SETUP

For operation, the Spectro-FTIR must have two


software programs installed on its personal com-
puter (PC) along with some specific settings for
proper communication between the spectrometer

Initial Software and the computer. The software and settings will
be pre-installed at Spectro Inc. when the comput-
er is supplied along with the Spectro-FTIR. The

Setup instructions in this chapter must be followed in


sequence when the customer supplies their own
computer, or if the original computer needs to be
replaced.

This chapter details the installation and setup in-


structions for the OPUS Software, the Spectro
FTIR Software, and software configuration re-
quiremets.

2.1 SETUP OF NETWORK CARD

The Spectro-FTIR can be used in two operating


modes, either as a standalone system operated by
its (PC), or as an integral part of a laboratory in-
formation system (LIMS) such as LabTrak.

When the Spectro-FTIR is used as a standalone


system, the network card supplied with the com-
puter can be used to communicate with the spec-
trometer. The network card in the PC is connect-
ed to the Spectro-FTIR with a crossover Ethernet
cable. Proceed with Step 1 to configure the net-
work card.

When the Spectro-FTIR and its PC is used in a


network, an additional network card (supplied
with the system) must be installed. Install the
card in the PC with the instructions provided
with the card or the PC. The installed network
card in the PC is connected to the Spectro-FTIR
with a standard Ethernet cable. Proceed with step
1 to configure the network card.

1. To configure the network card, open the


Windows XP Control Panel and right click on
“Network Connections”.

1 May, 2009 / v.1.2


18  |  Chapter 2 Initial Software Setup

2. Right click on the network card (Local


Area Connection) that you plan to use to
communicate with the Spectro-FTIR. Select
“Properties” from the drop-down menu, Fig-
ure 2.1-1.

NOTE: As long as the network port is used with


the Spectro-FTIR, it does not matter which net-
work card you select if there are more than one.
Figure 2.1-3, Internet Protocol Properties
3. Make sure the “General” tab is selected and Screen
scroll down to “Internet Protocol (TCP/IP)”, 6. Enter the IP address of “10.10.0.100” and
Figure 2.1-2. Sub Mask address of “255.0.0.0” as shown in
Figure 2.1-4. The Subnet mask address can
4. Select “Internet Protocol (TCP/IP)” by also be entered automatically by pressing the
double-clicking on it or by selecting “Proper- “Tab” key after the IP address is entered. Click
ties” and clicking on it. The screen shown in on “OK” to save the configuration and “Close”
Figure 2.1-3 will appear. to close the screen.

5. On the “Internet Properties (TCP/IP)” 7. After completion of the configuration


screen, select the radio button for “Use the fol- process, if the Spectro-FTIR is connected, the
lowing IP address:” by clicking on it. Local Area Connection just configured will be

Figure 2.1-1, Network Connections screen

Figure 2.1-4, IP ans Sub Mask Addresses


Entered

Figure 2.1-5, Configure Network Connection


Figure 2.1-2, General Tab and Internet Protocol Screen

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  19

enabled and will show as “connected” on the software files.


Network Connection screen Figure 2.1-5.
2.2.1.1 Symantec Norton AntiVirus Corporate
8. This completes the network card setup. Edition

2.2 DISABLE VIRUS AND FIREWALL Use the following procedure for configuring Sy-
SOFTWARE mantec Norton AntiVirus Corporate Edition on
a workstation to exclude the WIBUKEY, WIBU-
There have been reports of virus checking software SYSTEMS, and OPUS program directories from
adversely affecting performance and sometimes continuous virus scanning:
even causing errors in the Spectro-FTIR software.
It has been established that virus checking soft- 1. Select Start | Programs | Symantec Client
ware can slow down performance in certain situ- Security | Symantec AntiVirus Client.
ations. We recommend that virus checking soft- 2. Select Configure | File System Realtime
ware be configured in such a way as to minimize Protection.
the effects of virus scanner interference. 3. In the Options section, select the Exclude
selected files and folders check box.
Some virus checking software systems have the 4. Click Exclusions.
ability to virus scan continuously in the back- 5. Select the Check file for exclusion before
ground. This type of configuration can slow scanning check box.
down the performance of software, particularly in 6. Click Files/Folders.
a network environment.  7. Browse to the WIBUKEY software pro-
gram directory (for example, C:\Program Files\
The Spectro-FTIR software is data processing soft- WIBUKEY) and select the corresponding
ware that is very disk I/O intensive. The software check box.
is constantly opening files, writing to them and 8. Browse to the WIBU-SYSTEMS software
closing them. The software also makes frequent program directory (for example, C:\Program
use of temporary files. For these reasons, the po- Files\ WIBU-SYSTEMS) and select the corre-
tential performance decrease caused by continu- sponding check box.
ous virus scanning may be more apparent in our 9. Browse to the OPUS software program
software than in some other types of applications. directory (for example, C:\Program Files\
OPUS) and select the corresponding check
The Spectro-FTIR software uses a network in- box.
terface for communication. This communication 10. Click OK three times to save your changes.
cannot be run through a firewall protection sys- 11. Click Exit to exit Symantec AntiVirus Cor-
tem. The delays caused by the firewall can severe- porate Edition.
ly interrupt the analysis process and cause system
errors. The network adapter that communicates NOTE:  Additional instructions regarding how
with the FTIR should be disabled in any firewall to exclude files and directories can be found on
software and in Windows XP Firewall. Symantec’s Knowledge Base on the Internet.

2.2.1 Excluding Spectro-FTIR Software 2.2.1.2 Symantec Norton AntiVirus Consumer


Program Directory from Continuous Edition
Virus Checking Use the following procedure for configuring Sy-
This section details the step-by-step procedures mantec Norton AntiVirus Consumer Edition on
to disable virus checking software from different a workstation to exclude the WIBUKEY, WIBU-
manufacturers to exclude specific Spectro-FTIR SYSTEMS, and OPUS program directory from

1 May, 2009 / v.1.2


20  |  Chapter 2 Initial Software Setup

continuous virus scanning:


For more information on file exclusions in
1. Open Norton and click Options. McAfee software, see the user’s guide provided
2. Select Autoprotect | then Exclusions. with the McAfee software, or see McAfee’s Web
3. Click New and type in the path of the site at http://www.McAfee.com.
WIBUKEY directory (for example C:\Program
Files\WIBUKEY), make sure to include sub- 2.2.2 Disabling Firewall Software
folders. This section details the step-by-step procedures to
4. Click New and type in the path of the disable firewall software from different manufac-
WIBU-SYSTEMS directory (for example C:\ turers to exclude the Spectro-FTIR.
Program Files\ WIBU-SYSTEMS), make sure
to include subfolders. 2.2.2.1 Disable Internet Connection Firewall in
5. Click New and type in the path of the Windows XP or Windows XP SP1
OPUS directory (for example C:\Program A firewall is designed to help protect your com-
Files\ OPUS), make sure to include subfolders. puter from attack by malicious users or by mali-
6. Click OK and then Exit. cious software. Malicious software includes virus-
es that use unsolicited incoming network traffic
NOTE:  Additional instructions regarding how to attack your computer. Before you disable your
to exclude files and directories for your specific firewall, you must disconnect your computer
version of the consumer edition can be found on from all networks, including the Internet. To do
Symantec’s Knowledge Base on the Internet at: this, follow these steps:
http://service1.symantec.com/SUPPORT/nav.nsf/
pfdocs/199829164436 1. In Control Panel, double-click Network-
ing and Internet Connections, and then click
2.2.1.3 McAfee VirusScan Network Connections.
Use the following procedure for configuring 2. Right-click the connection on which you
McAfee VirusScan Enterprise to exclude the WI- want to disable ICF, and then click Properties.
BUKEY, WIBU-SYSTEMS, and OPUS program 3. On the Advanced tab, click to clear the
directory from continuous virus scanning: Protect my computer or network check box.

1. Open the On-Access Scan Properties dia- 2.2.2.2 Disable Windows Firewall in Windows
log box, then select one of the following icons XP SP2
in the left-hand pane: A firewall is designed to help protect your com-
• Default Processes puter from attack by malicious users or by mali-
• Low-Risk Processes cious software. Malicious software includes virus-
• High-Risk Processes es that use unsolicited incoming network traffic
2. On the Detection tab, click Exclusions in to attack your computer. Before you disable your
the What Not to Scan area. This will open the firewall, you must disconnect your computer
3. Set Exclusions dialog box. from all networks, including the Internet. To do
The Set Exclusions dialog box lets you add this, follow these steps:
or edit files, folders, or drives. Windows File
Protection is listed by default. 1. Click Start, click Run, type Firewall.cpl,
• To add an item to the list of exclusions, open and then click OK.
the Add Exclusion Items dialog box by click- 2. On the General tab, click Off (not recom-
ing Add. mended), and then click OK.
• To edit an item in the list, you can double-
click it or select it and then click Edit.

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  21

2.2.2.3 Norton Internet Security 2.3 OPUS SOFTWARE INSTALLATION


1. Log on using an account with Adult or AND CUSTOMIZATION
Supervisor rights. Open Norton Internet Secu-
rity. The OPUS software is supplied with your Spectro-
2. On the left side of the window, click Inter- FTIR on a CD-ROM. If the PC was purchased
net Status and then click Current Status. with the Spectro-FTIR the OPUS software will
3. In the Current Status window, click Dis- be pre-installed by Spectro Inc.
able.
2.3.1 Installing OPUS Software
2.2.2.4 Norton Personal Firewall The following is the procedure to install the
1. Open Norton Personal Fireall. OPUS software when the customer supplies the
2. On the left side of the window, click Inter- PC, or if it needs to be re-installed for mainte-
net Status and then click Current Status. nance purposes or onto a new computer.
3. In the Current Status window, click Dis-
able. 1. Locate the OPUS CD-ROM that is sup-
plied in the plastic box supplied with the
You can also disable Norton Personal Firewall by Spectro-FTIR, Figure 2.3-1. Open the box
right-clicking on the Norton Personal Firewall and install the CD-ROM into the PC.
icon in the notification area of the taskbar and
selecting disable. 2. The OPUS InstallShield Wizard opens
in auto-start and the first screens asks you to
2.2.2.5 McAfee Internet Security select your language preference. Select a lan-
1. Right-click the McAfee icon. guage from the drop-down menu and click on
2. Point to Personal Firewall and then click “OK”.
Options.
3. Click the Security tab.
4. Set the Security Level by moving the slider
to the desired level.
5. Set Access to Low.
6. Click OK to save changes.

2.2.2.6 McAfee Firewall


1. Click Stop McAfee Firewall to disable the
software.
2. From the Welcome to McAfee Firewall
screen, go to the Network Control Settings
and select Allow All Traffic.

Figure 2.3-1, OPUS CD-ROM Software Box

1 May, 2009 / v.1.2


22  |  Chapter 2 Initial Software Setup

3. The next screen does not apply to the


Spectro-FTIR, Figure 2.3-2. Click on the
“Skip this step” check box to select. Click on
the “Next” button.
4. On the License Agreement screen, Figure
2.3-3, select the radio button for “I accept the
terms of the license agreement”. Click on the
“Next” button.
5. The next screen requires that the “User
Name” and “Company” name be entered,
Figure 2.3-4. The information entered is up to
the user. Select whether the application is to
be installed for any user of the PC, or just an Figure 2.3-4, User Name and Company Screen
individual. Click on the “Next” button.
6. Select the “Custom” setup type, Figure 2.3-
5. Click on the “Next” button.
7. The next screen allows you to select the
destination on your computer where you wish
to install the OPUS files, Figure 2.3-6. The
default is the Program Files folder. Click on

Figure 2.3-5, Custom Setup Type Screen

Figure 2.3-6, Install Destination Screen

the “Next” button to select the default loca-


tion, or select the “Browse” button to change
the location.
8. The features (files) that need to be installed
are listed on the next screen, Figure 2.3-7. The
scroll bar on the right hand side needs to be
Figure 2.3-3, License Agreement Screen
used to view all the selections. If not already

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  23

10. The next screen, Figure 2.3-9 allows you


to import instrument configurations if OPUS
was previously installed on this PC. On new
installations, select the radio button for “No,
skip this step” and click on the “Next” button.

11. The final screen in the sequence, Figure


2.3-10 allows you to go back to review or
change any of the installations settings, or if
you are ready, click on “Install” to begin the
installation process.

Figure 2.3-7, Availabe Features Selection 12. When the installation is complete, the
Screen installation protocol can be printed by select-
selected, click the boxes to select the following ing “Print”, or by selecting “Accept”. A link to
files: the OPUS software will be placed on the PC’s
OPUS desktop
Basic Features
OPUS Lab 2.3.2 Registering OPUS
Standard
Documentation
OnLine Help
Extended Demodata
QUANT
QUANT Tutorial
TENSOR
TENSOR 27
VERTEX
VERTEX 80
Click on the “Next” button when the above
selections have been made.
9. On the next screen, Figure 2.3-8, select
“Tensor 27” from the window and click on Figure 2.3-9, Import from Previous Installation
“Next”. Screen

Figure 2.3-8, Instrument Model Selection


Figure 2.3-10, Ready to Install OPUS Screen
Screen

1 May, 2009 / v.1.2


24  |  Chapter 2 Initial Software Setup

The OPUS software must be registered in order


to receive information on updates and warranty
support. The software can be registered right after
it is installed or at anytime thereafter. To regis-
ter after the OPUS software is installed start with
Step 1, or at anytime thereafter start with Step 2.

1. When the OPUS software installation pro-


cedure of Section 2.3.1 is complete, the screen
shown in Figure 2.3-11 appears. Select the
check box for “I want to start OPUS” and click
on “Finish”.
Figure 2.3-13, Register OPUS Drop-down Menu
2. When the OPUS software opens, the 4. The About OPUS screen appears, Figure
OPUS Login screen appears, Figure 2.3-12, 2.3-14 Click on the “OK” button and the
and a password must be entered. The User ID screen will disappear.
is “Default” and the Password is “OPUS” (all
capital letters, no quotation marks). Click on 5. The Registration Dialog screen, Figure 2.3-
“Login” to start the software.

3. From the OPUS Operator Default screen,


Figure 2.3-13, click on the “Setup” menu bar
drop-down menu and select “Register OPUS”
from the available options.

Figure 2.3-14, About OPUS Screen

Figure 2.3-11, OPUS Registration Wizard

Figure 2.3-12, OPUS Login Screen Figure 2.3-15, Registration Dialog Screen

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  25

15, is used to enter Name, Company, Instru-


ment serial number, OPUS serial number, and
the Key.

6. The information that must be entered into


these fields can be found on the inside cover
of the OPUS software CD-ROM plastic box, Figure 2.3-17, Measure Drop-down Menu
Figure 2.3-16. Enter the information exactly
as printed on the box (it is case sensitive).

7. Click on “Check Registration Data” but-


ton. If the data was entered correctly, “IR”
should appear in the “Available software pack-
ages and libraries” field. If not, the data was
entered incorrectly.

8. Click on “OK” when data is entered cor-


rectly and “IR” appears in the “Available soft-
ware packages and libraries” field.

9. This completes the OPUS software registra-


tion procedure.
Figure 2.3-18, Select Vertex 80 From Drop-
down Menu
2.3.3 Unlock Required Features.
must be entered. The User ID is “Default” and
There are some features required for oil analysis
the Password is “OPUS” (all capital letters, no
that are not part of the standard Spectro-FTIR
quotation marks). Click on “Login” to start
OPUS Tensor 27 software. These features will
the software.
be imported from a different model instrument’s
3. From the OPUS Operator Default screen
software, the Vertex 80.
click on the “Measure” menu bar drop-down
menu, and select “Optic Setup and Service”,
1. If not already open, load the OPUS soft-
Figure 2.3-17
ware, by double clicking on its desktop icon.
4. The “Optic Setup and Service” window
2. When the OPUS software opens, the
appears. From the “Configuration” drop-down
OPUS Login screen appears and a password
menu select “Vertex80”, Figure 2.3-18 and
click on “Save Settings”.
5. Click on “Save and Close” to force the
software to accept the Vertex80 selection.
6. The “Optic Setup and Service” window re-
appears. From the “Configuration” drop-down

Figure 2.3-19, Select Tensor 27 From Drop-


Figure 2.3-16, Unique OPUS Registration Data down Menu

1 May, 2009 / v.1.2


26  |  Chapter 2 Initial Software Setup

menu select “Tensor27”, Figure 2.3-19 and


click on “Save Settings”.
7. This completes the procedure and the addi-
tional features are now unlocked and included
in the operating software.

2.3.4 Customize Measure Drop-Down Menu


Depending on the version of the OPUS software,
the Measure drop-down menu may already be
configured as necessary with the commands for
use with the Spectro-FTIR Oil Analysis Software.
This procedure will show the user the commands
that are required and if they are not present, how Figure 2.3-21, Select Toolbars Command
to install them.

1. If not already open, load the OPUS soft-


ware, by double clicking on its desktop icon.
2. When the OPUS software opens, the
OPUS Login screen appears and a password
must be entered. The User ID is “Default” and
the Password is “OPUS” (all capital letters, no
quotation marks). Click on “Login” to start
the software.
3. From the OPUS Operator Default screen
click on the “Measure” menu bar drop-down
menu, Figure 2.3-20. The two commands that
must be available and installed are “Advanced Figure 2.3-22, Customize Screen
Measurement” and “Optic Setup and Ser- menu, select the “View” drop-down menu and
vice”. Verify that the commands are installed, select the “Toolbars” command, Figure 2.3-21.
if they are, customization is not necessary, 5. The Customization screen appears, Figure
proceed with Step 8. If one or both of the 2.3-22. Make sure that the “Commands” tab
commands are not present, proceed with Step is selected. Select “Measure” in the Custom-
4. ization menu Categories column by clicking
4. To customize the Measure drop-down on it.

6. Locate “Advanced Measurement” in the


commands column and select it by clicking
and holding the mouse button, Figure 2.3-
23. While holding down the mouse button
drag the “Advanced Measurement” command
to the “Measure” drop-down menu. The
Measure drop-down menu will open and the
command can be dropped at any preferred
location in the drop-down sequence. Note
that a horizontal bar signifies where command
is being located in the sequence. Release the
Figure 2.3-20, Measure Drop-down Menu
mouse button to place the command into the

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  27

ure 2.3-25. Verify that “Enforce Predefined


Measurement Parameters” and “Automatic
Accessory Recognition” are not selected with
a “√” mark. If one or both are selected, de-
select them by clicking on the check box.
10. Click on the “Save Settings” button to
complete the Measure menu customization
procedure.

2.3.5 Disable FDA Compliance


Figure 2.3-23, Drag and Drop Commands to The Spectro-FTIR OPUS software defaults to
Menues Food and Drug Administration (FDA) specifica-
Measure drop down menu. tion 21 CFR 11 for pharmaceutical and biotech-
7. Repeat Step 6 but this time for the “Op- nology industries. This specification does not ap-
tic Setup and Service” command. Click on ply to oil analysis and it must be disabled in order
“Close” in the Customization menu to finish to analyze lubricants.
the Measure drop-down menu customization.
8. Click on the “Measure” drop-down menu 1. If not already open, load the OPUS soft-
and select “Optic Setup and Service” com- ware, by double clicking on its desktop icon.
mand, Figure 2.3-24. 2. When the OPUS software opens, the
9 The Optic Setup and Service menu ap- OPUS Login screen appears and a password
pears. Select the “Devices/Options” tab, Fig- must be entered. The User ID is “Default” and
the Password is “OPUS” (all capital letters, no
quotation marks). Click on “Login” to start
the software.
3. From the OPUS Operator Default screen
click on the “Setup” menu bar drop-down
menu and select “User Settings”, Figure 2.3-
26.
4. The window for User Settings shown in fig-
ure 2.3-27 appears. Click on the “CFR11” tab
Figure 2.3-24, Select Optic Setup and Service to select it. In the lower section, “Validation
options”, deselect “Work in GLP mode (Save
original data)” so that there is no check mark
to the left of it.
5. Click on “OK” to complete this procedure
to disable FDA data maintenance require-
ments.

Figure 2.3-25, Optic Setup and Service Screen Figure 2.3-26, Select User Settings

1 May, 2009 / v.1.2


28  |  Chapter 2 Initial Software Setup

Figure 2.3-27, Deselect Work in GLP Mode Figure 2.4-1, Spectro Oil Analysis Install Screen

2.4 INSTALL SPECTRO-FTIR OIL


ANALYSIS SOFTWARE

This section details the step-by-step procedure to


install the Spectro FTIR Oil Analysis Software.
The Spectro FTIR Oil Analysis Software is deliv-
ered with your instrument on a CD-ROM.
To install the software:

1. Locate the Spectro-FTIR Oil Analysis Soft-


ware CD-ROM and insert it into the PC.
2. Locate the CD-ROM on the PC by open- Figure 2.4-2, Read Me File
ing “My Computer”. The icon for the Spectro-
FTIR Oil Analysis Software CD-ROM will instructions. Click on “Next” to proceed.
be listed under the “Devices and Removable 6. The next screen allows you to select the
Storage” section. Double click on the Spec-
destination on your computer where you wish
tro-FTIR Oil Analysis Software icon to open to install the Spectro FTIR Oil Analysis Soft-
it. ware, Figure 2.4-3. The default is the Program
3. The Spectro-FTIR Oil Analysis Software Files folder. Click on the “Next” button to se-
CD-ROM contains three types of files, Acro- lect the default location, or select the “Browse”
bat Reader, Manuals in PDF format, and the
installation program. Double click on the
“Installation” icon.

NOTE: Acrobat Reader must be installed on


the computer in order print the PQ test report
which is created in the PDF format.

4. The screen shown in Figure 2.4-1 will


instruct you to close all open files. Click on
“Next” to proceed.
5. The next screen, Figure 2.4-2 has a Re-
adMe file. Read the file for any last minute Figure 2.4-3, Select Installation Destination

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  29

button to change the location.


7. The next screen, Figure 2.4-4, lists the files
to be installed. All three files, (Main Program
Files, Default Oil Database, Default Analysis
Methods) should already be selected. If not,
select them and click on “Next” to proceed.
8. The Start Installation screen, Figure 2.4-
5 provides an option to go back and make
changes, or to proceed with the installation.
Click “Next” to install the Spectro-FTIR Oil
Analysis Software.
9. When the software has been installed suc-
cessfully, the screen, Figure 2.4-6, appears to Figure 2.4--6, Software Successfully Installed
confirm the installation. Click on “Finish” to Screen
exit the Spectro-FTIR Oil Analysis Software
2.5 CONFIGURE OPUS WITH THE
installation.
OIL ANALYSIS WORKSPACE FILE
10. This completes the Spectro-FTIR Oil
(Oil.xpm)
Analysis Software Installation.
In order to analyze oil samples with the Spectro-
FTIR, a file with all the instrument parameters
must be loaded into the OPUS software. This file
is called “Oil.xpm” and was installed on the com-
puter along with the installation of the Spectro
FTIR Oil Analysis Software. This procedure will
provide a path for the OPUS software to locate
this file so that it can be used for the analysis of
routine oil samples.

1. Open the OPUS software by double click-


ing on its icon. When the software opens, the
OPUS Login screen appears and a password
Figure 2.4-4, Files to be Installed must be entered. The User ID is “Default” and
the Password is “OPUS” (all capital letters, no
quotation marks). Click on “Login” to start
the software.
2. Prior to loading the Oil.xpm file, verify
that the Optic Setup and Services are config-
ured correctly. This should have been per-
formed during the OPUS installation, Section
2.3.2 Steps 8 to 10, however, it will be repeat-
ed here for convenience.
3. On the OPUS default screen select “Mea-
sure” and from the drop-down menu select
“Optic Setup and Service”.
Figure 2.4-5, Start Installation Screen 4. Click on the “Save Settings” button to
complete the Measure menu customization
procedure.

1 May, 2009 / v.1.2


30  |  Chapter 2 Initial Software Setup

5. On the OPUS default screen select “Mea-


sure” and from the drop-down menu select
“Advanced Measurment”, Figure 2.5-1.
6. The “Measurement options” window ap-
pears, Figure 2.5-2. Select the “Basic” tab if
not already open. Click on the “Load” button
to the right of the “Experiment” field.
7. The “Select Measurement Parameters” win-
dow appears, Figure 2.5-3.

NOTE: It is good practice to make a copy of the


OIL.xpm file for future use in case it accidentally
gets corrupted. That way this procedure to load Figure 2.5-3, Select Measurment Parameter
the file can be repeated instead of performing a Screen
complete installation of the Spectro-FTIR Oil 9. The instrument parameters for routine oil
Analysis Software. analysis have now been loaded into the operat-
ing software and the procedure is complete.
8. Click on the drop-down menu next to the 10. The instrument parameters that have been
“Look In” field and the file structure similar loaded for routine oil analysis can be viewed in
to Figure 2.4.4 will appear. Navigate through the “Measurement” window by selecting the
the Program Files/Spectro Oil Analysis/XPM tabs for “Advanced”, “Optic”, “Acquisition”,
folders and select the “Oil.xpm” file and double “FT”, or “Check Signal”. The correct settings
click to load it. The “Measurements” options for these tabs are shown in the next five figures
window re-appears. (Figures 2.5-5 to 2.5-9)

Figure 2.5-1, Select Advanced Measurment


from the Measure Menu

Figure 2.5-4, Select Oil.xpm Measurment


Parameter

Figure 2.5-2, Basic Tab Screen

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Spectro-FTIR User Operation & Maintenance Manual  |  31

Figure 2.5-5, Advanced Tab

Figure 2.5-6, Optic Tab

1 May, 2009 / v.1.2


32  |  Chapter 2 Initial Software Setup

Figure 2.5-7 Acquisition Tab

Figure 2.5-8, FT Tab

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  33

Figure 2.5-9, Check Signal Tab

2.6 SETUP OPUS VALIDATION


PROGRAM FOR PQ AND OQ The Validation Program as described below
TESTS should be performed when the instrument is first
installed and whenever an optical component
The PQ and OQ tests are performance verifica- such as the laser, source, windows or detector has
tion tests that are run periodically to check the been replaced.
status of the Spectro-FTIR. This section describes
how these tests are validated (setup) during the NOTE: The cell and cell holder must be removed
initial installation of your Spectro-FTIR so that when this test is performed. See Section 1.4 for
they can be used as a reference to which future the procedure to remove the cell and cell holder.
tests are compared.
1. Open the OPUS software by double click-
The recommended frequency of the OQ test is to ing on its icon. When the software opens, the
perform it on a daily basis before routine samples OPUS Login screen appears and a password
are analyzed. The OQ test on the other hand is must be entered. The User ID is “Default” and
performed on an annual basis. The PQ test con- the Password is “OPUS” (all capital letters, no
firms the Spectro-FTIR’s accuracy and stability quotation marks). Click on “Login” to start
as compared to when the PQ reference measure- the software.
ment was stored. A failure of the OQ test by itself 2. On the OPUS default screen select the
does not necessarily mean that the performance of “Validation” menu, Figure 2.6-1, and from
the Spectro-FTIR has been compromised, it may the drop-down menu select “Setup OVP”.
only verify that some of the components have
degraded since installation (this is a normal oc- 3. The screen shown in Figure 2.6-2 will
curence). appear. Enter “Default” in the “Title for new

1 May, 2009 / v.1.2


34  |  Chapter 2 Initial Software Setup

Figure 2.6-3, Select Sample Compartment RT-


DLaTGTS

Figure 2.6-1, Validation Drop-down Menu

Figure 2.6-4, Select “Blanck Field” in


Accessory Drop-down Menu
Figure 2.6-2, Setup OVP Screen
configuration” field. Click on the “Add new
configuration” button to save the entry.

4. The Instrument Configuration and Ac-


cessory information can now be entered from
drop-down menus. From the Instrument
Configuration drop down menu, select “Sam-
ple Compartment RT-DLaTGTS”, Figure 2.6-3.
This corresponds to selecting the Spectro-FTIR
sample compartment and the detector.
Figure 2.6-5, “Default” Selected in test Channel
5. From the Accessory drop-down menu se- Field
lect the “blank” entry at the bottom of the pull 10 minutes to complete.
down selections, Figure 2.6-3. Click on “Save
and Exit” to save the selections.
7. When the LWN measurement has been
successfully completed, a dialog box with No
6. The screen shown in Figure 2.6-4 ap- change required along with some reference
pears. Note that the title for the configuration value will appear, Figure 2.6-6. Click on “OK”
(Default) entered in Step 3 now appears in to proceed. A green “√” mark will now appear
the Current Test Channel field. The software to signify that the LWN measurement was suc-
and Spectro-FTIR are now ready to begin the cessful..
measure the Laser Wave Number test. Click 8. The Spectro-FTIR is now ready to setup
on “Measure LWN” to begin the test as shown the PQ and OQ tests. Click on the “OVP
in Figure 2.6-5. This test can take about 5 to

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  35

Figure 2.6-6, LWN Calibration Reference Values Figure 2.6-8, PQ Test Protocol
Test Setup” tab and the OVP Test Setup can take about 5 to 10 minutes to complete.
main screen shown in figure 2.6-7 will appear. When the reference spectra have been gath-
Confirm that the Run PQ and Run OQ check ered, a green “√” mark appears on the Measure
boxes are selected. The PQ test should be Reference Spectra button to signify the process
default to “12” and “Hours” while the OQ test has been completed, Figure 2.6-9. Click on
should default to “12” “Months”. Click on the the “OK” button to proceed.
“Setup” button to the right of the PQ test to
proceed. 11. The OVP Test Setup main screen reappears
with a green “√” mark to the right of the PQ
9. The screen shown in Figure 2.6-8 will test to signify that it has been setup successful-
appear for the PQ Test Protocol. The default ly Figure 2.6-10. The red caution sign on the
configuration will already have all the op- OQ Setup button signifies that this second test
tion boxes selected, if not select them. Click needs to be performed. Click on the “Setup”
on “Measure Reference Spectra” button to button to the right of the OQ test to proceed.
proceed. Note that the Caution symbol on
the button signifies that user intervention is 12. The screen shown in Figure 2.6-11 will
required. appear for the OQ Test Protocol. The default
configuration will already have all the option
10. The Spectro-FTIR is now gathering the boxes selected, if not select them. Click on
reference spectra for the PQ test. This test “OK” button to proceed.

Figure 2.6-7, OVP Test Setup Main Screen Figure 2.6-9, Successful Completion of
reference Spectra Test

1 May, 2009 / v.1.2


36  |  Chapter 2 Initial Software Setup

Figure 2.6-10, Successful Completion of PQ Figure 2.6-12, Successful Completion of OQ


Test Setup Test Setup

Figure 2.6-11, OQ Test Protocol Figure 2.6-13, OPUS Default Screen

13. When the test is complete, the OVP Test


Setup main screen reappears with a green “√”
mark to the right of the OP test to signify that
it has been setup successfully Figure 2.6-12.
Click on the “Save and Exit” button to com-
plete the PQ and OQ Test Setup procedure..

14. The software will return to the OPUS de-


fault screen. Note the icon in the lower right
hand corner turned from red to yellow Fig-
ure 2.6-13. This signifies that the OVP tests
have been setup but have not been performed
during routine operation. The icon will turn
to green when the tests have been performed,
Section 3.1.1.

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  37

Chapter 3 3.0 ROUTINE SAMPLE ANALYSIS

This chapter describes the routine operating pro-


cedures for the Spectro-FTIR in the analysis of in
service oil samples. The Spectro-FTIR is delivered
with multiple analysis programs, and it can also

Routine Sample be used to trend lubricant degradation and con-


tamination based on ASTM Standard Practice E
2412. One copy is supplied with your Spectro-

Analysis FTIR.

NOTE: Additional copies of ASTM E 2412


Standard Practice for Condition Monitoring of
Used Lubricants by Trend Analysis Using Fourier
Transform Infrared (FT-IR) Spectrometry are
available from ASTM International at: http://
www.astm.org.

3.1 INTRODUCTION

The Spectro-FTIR Oil Analysis program is used


to measure and analyze oil degradation and con-
tamination. Routine sample analysis consists of
Daily Diagnostic Tests and Sample Analysis, ei-
ther manually or automatically with an AutoSam-
pler.

The Spectro-FTIR user interface is simple and


easy to operate. In manual operation mode, the
operator selects the type of oil to analyze from a
list and presses a single on-screen button to be-
gin analysis. An on-screen wizard walks the op-
erator through the task of filling and cleaning the
cell. An automatic cleanliness check is performed
on the sample cell prior to any measurement to
ensure there is no contamination present from
previous measurements. The results of each mea-
surement are displayed to the user, and optionally
saved to a file for further analysis and study. An
optional computer controlled AutoSampler and
pump can be used to automatically sample and
analyze an entire rack of samples.

This chapter assumes that several on-time proce-


dures have already been performed, they are:

• The OPUS software has been installed and

1 May, 2009 / v.1.2


38  |  Chapter 3 Routine Sample Analysis

tested, Section 2.3.


• The Spectro-FTIR Oil Analysis program has
been installed, Section 2.4.
• Measurement analysis operating options have
been setup, Section 3.7.
• The probe and sample flow configuration
has been setup, either manual or automatic,
Chapter 1.4 and 1.5.

CAUTION: This section assumes that the opera-


tor is familiar with the solvent requirements
for the Spectro-FTIR and how solvents should
be stored, handled and disposed of. If not, read
Figure 3.2-1, Main Spectro Oil Analysis Screen
Section 3.10 to become familiar with the solvent
requirements for the Spectro-FTIR.

3.2 DAILY DIAGNOSTIC TESTS

The daily diagnostic tests consist of:


• PQ Test, a short-term test to verify that the
Spectro-FTIR’s performance is suited for
daily operation.
• Cell Calibration, a procedure to determine
the cell’s path length that is only performed if
a new cell is installed.
• Background Test, to establish the background
signal used to correct spectra should be per- Figure 3.2-2, OPUS Main Default Screen
formed every few hours of operation. each day, the icon color may still be green. Pro-
ceed with the test so that the test is performed on
3.2.1 Validate the Spectrometer, PQ Test a daily basis.
1. Start the Spectro Oil Analysis Software
by either double-clicking on the “Spectro 4. The Instrument Status screen will ap-
Oil Analysis” icon on the PC desktop, or by pear, Figure 3.2-3. The six diagnostic tests in
selecting it from the “Programs” section of the the top row of the Instrument Status screen
“START” menu. are performed automatically by the Spectro-
2. The Main Spectro Oil Analysis screen will FTIR each time OPUS is started. A green “√”
open. Select “Show OPUS” from the Help (check mark) signifies that the diagnostic test
drop-down menu, Figure 3.2-1. passed. The icon in the second row will have
3. The Main OPUS default screen opens, “Expired” at its bottom to signify that it needs
Figure 3.2-2. The icon in the lower right hand to be performed. Click on the “icon” to run
corner will be yellow if it has been 24 hours the test.
since the PQ test has been performed. Double
click on the “Yellow Icon”. 5. The screen shown in Figure 3.2-4 will
appear. If the PQ and OQ tests are due to
NOTE: The PQ test is a daily test. If it has been be run, there will be a check mark for each as
less than 24 hours since it was last performed, shown in the figure. On a routine operating
and is usually performed around the same time basis, only the PQ test will be performed be-

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  39

On standard cells, this procedure calibrates the


Spectro-FTIR’s cell by determining it’s path
length (thickness) and stores the information in
the software for use in the analytical results. The
procedure needs to be performed only when a cell
has been installed and can be skipped thereafter
during routine operations. Follow the procedure
below to calibrate a new cell.
1. Start the Spectro Oil Analysis Software
by either double-clicking on the “Spectro
Oil Analysis” icon on the PC desktop, or by
Figure 3.2-3, Instrument Ststus Screen selecting it from the “Programs” section of the
“START” menu.
2. From the Main Analysis screen, select
“Setup” and from the drop-down menu select
“Program Options”, Figure 3.2-5.
3. The “Program Setup” screen, Figure 3.2-6,
appears. The tab for “Option 1” should be the
default selection, if not, select it by clicking on
it.
4. Cell Fringe Correction must be disabled. If
it is ON, turn it OFF by deselecting the “En-
able Fringe Correction” button in the lower
third of the Options 1 tab, Section 3.7.1, item
C.
Figure 3.2-4, OVP Measurement Dialog
5. Close Options 1 tab by clicking on the
cause it is a daily test and the OQ is an annual “Exit Setup” button.
test. 6. Install the new cell to be calibrated. The
cell must be clean and dry.
NOTE: The report format is a PDF file, Adobe 7. Perform a “Background Test”, Section
PDF Reader must be installed before the test 3.2.3.
can be run. Verify that Adobe PDF Reader is 8. Return to the “Program Options”, step 2.
installed before the test is run. Click on “Run 9. Make sure the “Option 1” tab is selected
Tests” to perform the tests. and click on the “Calibrate Cell” button. The

6. When the tests are complete, the software


will return to the default OPUS screen and
the icon in the lower right hand corner will be
green.

3.2.2 Calibrate Cell (New Cell Only - Does


not Apply to Wedge Cells)
This procedure applies only to new standard cells,
it does not apply to wedge cells. For wedge cells,
make sure fringe correction is disabled (step 10)
and jump to step 12. Figure 3.2-5, Setup Drop-down Menu

1 May, 2009 / v.1.2


40  |  Chapter 3 Routine Sample Analysis

2. The Main Spectro-FTIR Oil Analysis


screen will open. To start the Background Test,
select the “Background” button by clicking on
it.
3. The measurement wizard will ask you to
clean and dry the sample cell, Figure 3.2-
7. If the cell is dirty, you must pump solvent
through the cell to clean it. (See Section 3.2
for recommended solvents) Next, pump air
through the cell to dry it. When the sample
cell is clean and dry select the “Next” button
by clicking on it.
4. If the Cell Cleanliness Check option has
been enabled in Program Options, tab 1 (Sec-
tion 3.7.2) then the wizard will perform a
cleanliness check of the cell Figure 3.2-8. If
the test fails you will be instructed to clean the
cell again. The test must pass before a back-
Figure 3.2-6, Program Setup Screen ground measurement can be performed.
cell path length will be computed and dis- 5. When the cleanliness test passes, the wizard
played in the Cell Path Length field. informs you it is ready to perform a back-
10. Enable Fringe Correction by selecting the ground measurement. Select the “Next” but-
“Enable Fringe Correction” button. ton by clicking on it to start the background
11. Close Options 1 tab by clicking on the measurement. The wizard informs you that
“Exit Setup” button. the background measurement is in progress,
12. Perform another “Background Test”, Sec- Figure 3.2-9.
tion 3.1.3 to establish the background with the
new cell installed and its path length calcu- CAUTION: Do not touch the instrument during
lated. the measurement or subject it to harsh vibrations.

3.2.3 Background Test


The background test should be performed at least
once per day when the Spectro-FTIR is used for
routine sample analysis. A more frequent sched-
ule is recommended when the laboratory’s envi-
ronment (temperature, humidity) changes a lot
throughout the day. The default frequency of the
background test is 24 hours but it can be changed
under “Program Setup” in tab 3, Section 3.7.4
The background test must be performed on a
clean and dry sample cell.

1.Start the Spectro Oil Analysis Software


by either double-clicking on the “Spectro
Oil Analysis” icon on the PC desktop, or by
selecting it from the “Programs” section of the
“START” menu. Figure 3.2-7, Please Clean Cell Screen

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  41

ment.
3.3 MANUAL SAMPLE MEASUREMENT

During a manual sample measurement, the oper-


ator must control all aspects of pumping sample,
solvent, and air through the sample cell. Only
a single sample can be measured and analyzed at
one time.

1. Start the Spectro Oil Analysis Software


by either double-clicking on the “Spectro
Oil Analysis” icon on the PC desktop, or by
selecting it from the “Programs” section of the
“START” menu.
2. The Main Spectro FTIR Oil Analysis
screen will open, Figure 3.3-1.
(arrows to sections)

Figure 3.1-8, Performing Cell Cleanliness The figure shows the main operator screen con-
Screen
figured for manual operation. The left side of
the screen contains a field that will display the
result of each analysis to the operator. When
the program is opened, the Analytical Results
field will be empty. The results are concatenat-
ed (consecutively linked) unless the “Clear Re-
sults List Before Each Measurement” Option
is selected in the Program Settings, Options 3
Tab, Section 3.7.4.

The right side of the screen contains all the


operator controls. At the top of the screen
are two text fields that must be completed to
perform a sample measurement.
Results of Analyses Analysis Methods

Figure 3.2-9, Performing Background


Measurement Screen

6. When the background measurement is


complete, the wizard screen will disappear and
the “Analyze” button on the Main Spectro-
FTIR Oil Analysis screen will become active.

You are now ready to perform a sample measure- Figure 3.3-1, Main Analysis Screen

1 May, 2009 / v.1.2


42  |  Chapter 3 Routine Sample Analysis

10. Select the “Analyze” button by clicking on


3. Perform a background test, Section 3.2.3. it to begin the sample measurement and analy-
unless it was performed recently. sis. You will be warned if a required parameter
4. On the main analysis screen enter the is missing. The Measurement Instructions
operator’s name or initials into the “User’s section will appear and the wizard will walk
Name” field. This will appear in all reports and you through the steps required for performing
databases. a manual sample measurement.
5. Enter the sample or identification number 11. The measurement wizard will now ask you
for this sample into the “Sample Number” to clean and dry the sample cell, Figure 3.3-
field. A new sample number is requested for 4. If the cell is dirty, you must pump solvent
each sample measured. The sample number through the cell to clean it and then pump
can be numeric, alphabetical or a combination air through the cell to dry it. If the sample is
thereof. already clean and dry or if it has been cleaned
6. Select one of the analysis methods in the and dried, select the “Next” button by clicking
list that corresponds to the type of oil being on it.
analyzed. The Spectro-FTIR software is deliv-
ered with the most common analysis methods
required for in-service oil analysis including
ASTM Standard Practice E 2412.
7. If the selected method requires a subtrac-
tion spectrum then the Subtraction Spectra
section becomes active and will no longer be
grayed out. If it does not become active, pro-
ceed with Step 9.
8. If the subtraction field is active. Use the
open folder button to the right of the field to
locate and select the subtraction spectrum.
This file must be measured and stored prior to Figure 3.3-3, Subtraction File Selected
the use of this analysis method. A sample file
of Subtraction Spectra is shown in Figure 3.3-
2.
9. Select the required Subtraction Spectra and
click on “Open” to activate it. The selected
spectra will now appear in the “Spectra for
Subtraction” field, Figure 3.3-3.

Figure 3.3-2, Subtraction Spectra Folder Figure 3.3-4, Please Clean Cell screen

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Spectro-FTIR User Operation & Maintenance Manual  |  43

12. If the “Cell Cleanliness Check” option If another analysis is performed at this time, the
has been enabled in Program Options, Op- results are concatenated (consecutively linked)
tions 1 tab, Section 3.7.2., then the wizard will unless the “Clear Results List Before Each Mea-
perform a cleanliness check of the cell, Figure surement” Option is selected in the Program Set-
3.3-5. If the test fails you will be instructed to tings, Option 3 Tab, Section 3.7.
clean the cell again. The test must pass before
a sample measurement can be performed. 16. Select the “Clear Results List” button to
13. The wizard will instruct you to pump oil
into the sample cell, Figure 3.3-6 when the cell
cleanliness test has passed or is skipped because
it is disabled.
14. Pump the oil into the sample cell, and
then press the “Next” button by clicking on it
to continue. The wizard informs you that a
sample measurement is in progress, Figure 3.3-
7.

CAUTION: Do not touch the instrument during


the measurement or subject it to harsh vibrations

15. When the measurement and analysis are


complete the results will be displayed in the
Analysis Results screen. A sample screen with
a typical analytical result is shown in Figure
3.3-8.
NOTE: Any warnings or errors are reported in
Figure 3.3-6, Pump Oil Into the Cell
the line following the procedure that produced
the warning or error.

Figure 3.3-5 Performing cleanliness Check Figure 3.3-7, Analysis in Process

1 May, 2009 / v.1.2


44  |  Chapter 3 Routine Sample Analysis

of each analysis to the operator. When the pro-


gram is opened, the Analytical Results field will
be empty. The results are concatenated (consecu-
tively linked) unless the “Clear Results List Be-
fore Each Measurement” Option is selected in the
Program Settings, Option 3 Tab, Section 3.7.4.
The right side of the screen contains all the opera-
tor controls. Follow the steps below to operate in
the Automatic Measurement Mode.

1. To complete the two text fields on the up-


per right side of the screen, enter the operator’s
Figure 3.3-8, Analytical Results in Main Screen name or initials. This will appear in all reports
manually clear the analytical results at any and databases.
time. Select the “Print” button to send the 2. Note that the right hand field that was
current text to a configured printer. called “Sample Number” in the manual opera-
tion is now designated as “Batch Number”. A
IMPORTANT NOTE: If you are not going to batch typically consists of multiple samples
perform any additional sample measurements consisting of an entire rack of samples or less.
you should pump the sample cell empty, then Enter the batch or identification number for
clean and dry the sample cell. this rack of samples. A new batch number is
requested for each rack measured. The batch
3.4 AUTOMATIC OPERATION number can be numeric, alphabetical or a
combination thereof.
The Spectro-FTIR can be operated in the auto- 3. Select a predefined rack setup from the
matic mode with an optional Auto Sampler. In “Autosampler Rack Definition” drop-down
this mode of operation the filling, emptying, and menu, Figure 3.4-2. This defines the layout
cleaning of the cell is performed automatically of the sample rack used to hold your sample
using a computer controlled AutoSampler and bottles. You can define new rack definitions if
external pump(s). A rack of samples is thus mea- an appropriate setup does not appear in the list
sured automatically according to the operators’ (Section 3.4.2).
settings.
After selecting a rack definition the graphic to the
3.4.1 Automatic Sample Analysis right of the drop-down menu will be updated to
In order to analyze samples in the Automatic Mea-
surement Mode, the mode must be enabled in the
Program Setup, Options 3 tab, Section 3.7.4. It
is also assumed that the sample flow plumbing for
the cell and AutoSampler is setup per Section 1.5,
Automatic Operation Plumbing Setup.
In the automatic mode, the main Spectro-FTIR
Oil Analysis screen is changed as shown in Figure
3.4-1.

The figure shows the main operator screen config-


ured for automatic operation. The left side of the
Figure 3.4.1, Main Spectro Oil Analysis Scren in
screen contains a field that will display the result
the Automatic Mode

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Spectro-FTIR User Operation & Maintenance Manual  |  45

Figure 3.4-2, AutoSampler Rach Definitions and


Rack Layout Details
graphically represent the layout of the selected
sample rack. In the example, the rack contains
24 sample bottles. In addition to updating the
graphical representation of the sample rack, the Figure 3.4-3, Methods Pull-down Menu to
Assign Method to a Sample
sample rack assignment grid is populated with the
appropriate number of positions for the selected position. This field is required.
sample rack. • Subtraction Spectra: If the selected analysis
method requires a subtraction spectrum then
4. To prepare the sample rack for automatic this field becomes active. Left-click on the
measurement, you need to assign data for each field to display a file selection dialog. Locate
position in the rack that will contain an oil and select the appropriate subtraction spec-
sample to be analyzed. The rack graphic and trum file.
rack assignment grid are interactive. Left-click
on any of the rows in the assignment grid and 5. When the data for the samples in the rack
it is highlighted in yellow. The correspond- has been entered, select the “Analyze” button
ing sample position on the rack graphic is also by clicking on it to begin sample measurement
highlighted in yellow. Alternately you can left- and analysis. You will be warned if a required
click on a sample position in the rack graphic parameter is missing. The status bar displays
and the corresponding row in the assignment information about each step in the measure-
grid is highlighted, Figure 3.4-3. ment cycle.

There are four columns in the assignment grid Each sample measurement consists of the steps
that must be filled in for each sample in the rack. below and summarized in Figure 3.4-4.

• Analyze: Check this field to instruct the • The sample cell is tested for the presence
program to measure the sample at this posi- of oil or solvent. If found, the cell is auto-
tion on the rack. The position number and matically cleaned and dried. (Only tested
sample cell color turn blue. if Cleanliness Check is enabled in Program
• Sample ID: This is a unique sample ID num- Options, Section 3.7.)
ber for the sample located at this position on • The probe is moved to the next enabled
the sample rack. This is a required field. sample position and inserted into the sample
• Analysis Method: Left-click on this field to bottle.
display a drop-down list of analysis methods. • Oil is pumped into the cell for the Pump
Select one of the methods to be applied to Time specified in Program Options, Section
the analysis of the sample located at this rack 3.7.

1 May, 2009 / v.1.2


46  |  Chapter 3 Routine Sample Analysis

Analyze Button

Cell is tested for


Failed
Presence of Oil or
Solvent

Passed

Probe is moved to the Next


Enabled Position & Inserted in the
Sample Bottle

Oil is Pumped into the Sample Cell

Sample Cell is Failed


Tested for Oil

Passed

Sample
Probe is Removed from Sample
Measurement &
Bottle & Allowed to Drip
Analysis

Probe is Moved to Rinse Station


Cell & Lines are Rinsed

Probe is Removed from Rinse Solvent


& Air is Pumped to Dry It.

Figure 3.4-4, Automatic Sample Measurement Analysis Flow

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Spectro-FTIR User Operation & Maintenance Manual  |  47

• The sample cell is tested for the presence of and saved in the designated database.
oil. If oil is not detected, the oil is pumped Any warnings or errors are reported in the line
and the cell is tested again. If after a few tries following the procedure that produced the warn-
the cell still does not contain oil the operator ing or error.
is queried to determine if pumping should
continue. The rack graphic displays different colors depend-
• The probe is removed from the sample bottle ing upon the state of a sample position.
and excess oil is allowed to drip.
• The sample measurement and analysis is
A white cell indicates an unused sample
performed.
position on the sample rack.
• The probe is moved to the rinse station of the
AutoSampler and a rinse cycle is performed.
Solvent is pumped through the line and A blue cell indicates a sample position that
sample cell. has been assigned a sample bottle.
• The probe is removed from the rinse solvent
and air is pumped through the sample cell.
• The sample cell is tested for the presence of A yellow cell indicates the currently se-
oil. If oil is detected, additional rinsing is lected sample position.
performed. If solvent is detected, additional
air pumping is performed. At the completion of the cell analysis, if all
procedures in the analysis method were within
As each sample position is measured, the results specifications, the cell position is displayed in
are displayed to the operator in the Analysis Re- green.
sults section, Figure 3.4-5.

When a database is selected in Program Setup, If an error occurred during the analysis,
Option 3 tab, Section 3.7.4, the results are stored the cell position is displayed in red.
(add blue)

6. When all the samples in the rack have been


successfully analyzed, remove the rack, insert a
new one and repeat this procedure.

3.5 REPROCESS SPECTRA

It is possible to take an existing spectra of a sam-


ple and view results by applying different methods
to it without the need to re-analyze the sample.
This option is only available when the program
is in manual operation mode. It is applied to the
file in the same manner as if the program had ac-
quired the spectra. When a spectra is reprocessed,
the results are displayed to the user in the results
screen, but reports and results are not saved to the
database or CSV file.

Figure 3.4-5, Analysis Results Field


To use this option:
1. Select the analysis method you wish to

1 May, 2009 / v.1.2


48  |  Chapter 3 Routine Sample Analysis

use to reprocess the sample from the list on


the main program screen. An example for the
hydraulic method is shown in Figure 3.5-1.
2. Select “Reprocess Spectra” from the
“Setup” drop-down menu, Figure 3.5-2.
3. The screen shown in Figure 3.5-3 appears.
Use the open folder button to locate and view
the OPUS spectra file you want to reprocess.
4. When the spectra file has been located and Figure 3.5-4, File to be Reprocessed
highlighted, click on the “OPEN” button to “Reprocess” button by clicking on it and the
select the file. spectra will be reprocessed with the selected
5. The file name will appear in the Select File analytical method. The results will appear in
to Reprocess field, Figure 3.5-4. Select the the Analytical Results screen.

3.6 CREATING REPORTS

The Spectro-FTIR Oil Analysis software has the


capability to create high quality reports that can
be printed based upon data stored in the results
database. In order to create reports, the “Store
Results in Database” button must be activated
in the Program Options, Option 2 tab, Section
Figure 3.5-1, Select Method for Reprocessed 3.7.3.
Sample
To create a report from a sample or batch:
1. Select “View Reports” from the “Main”
drop-down menu, Figure 3.6-1.
2. The report selection dialog appears, Figure
3.6-2. Each row in the list corresponds to a
saved report in the database. Select the report
you wish to create and double-click on its line.

3. A preview is created and displayed on the


screen, Figure 3.6-3. Use the controls on
the preview window to view and/or print the
Figure 3.5-2, Setup Drop-down Menu
report.
4. Close the report window when you are
finished viewing it.

Figure 3.5-3, Locate File to Reprocess Figure 3.6-1, Main Drop-down Menu

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Spectro-FTIR User Operation & Maintenance Manual  |  49

3.7 PROGRAM OPTIONS

The Program Options feature provides the user


with alternative ways to configure and setup the
Spectro-FTIR for the analysis of in-service oil
samples. There are four option tabs; each con-
tains program options and parameters that can
be configured according to the analytical needs of
the operator. The four available tabs and their op-
tions are described in this section.

Figure 3.6-2, Report Seletion Dialog To view the tabs, select “Program Options” from
the “Setup” menu, Figure 3.7-1.

3.7.1 Options Tab 1


The Program Options, Option 1tab is shown in
Figure 3.7-2. The available settings and corre-
sponding fields are explained in this section.

A. Last Diagnostic Message


The last error message received will be displayed
in this field if hardware diagnostics are enabled,
and a diagnostics error was reported

B. Cell Cleanliness Test


Figure 3.6-3, Sample Report This option performs a cell cleanliness test on the
sample cell prior to any background or sample
measurement. A sample spectrum is recorded
and integration is performed to determine the
level of the CH band in the absorbance spectrum.
By default the cell cleanliness test is enabled.
Click on the box to un-check this option if you
do not want to perform a cell cleanliness test prior

Figure 3.7-1, Setup Drop-down Menu

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50  |  Chapter 3 Routine Sample Analysis

A.

B.

C.

Figure 3.7-2, Options Tab 1

to each measurement. fault setting is to discard them after the test. In


order to save the spectra, click on the Save Cell
Warning: A dirty sample cell could contaminate Cleanliness Spectra box to enable this feature.
your oil sample and result in erroneous results.
C. Cell Fringe Correction
The next two fields are used to set values that de- Most sample cells, (other than wedge cells) exhib-
termine cell cleanliness. The Oil Limit value is it fringing characteristics in the sample spectrum
used during automatic sampling to determine if due to multiple reflections within the sample cell.
a cell requires additional solvent or air pumped This option eliminates most of the effect of fring-
through it to properly clean it. The Oil Limit is ing from the cell.
the prediction value above which oil is reported
in the cell. The Pass Limit is the prediction value By default, this option is disabled. To enable it
below which the cell is considered clean. Values you must first calibrate the cell to determine the
between these two levels are thus considered resi- cell path length. The procedure to calibrate the
due from the solvent. cell is detailed in Section 3.1.2.

The spectra generated during the cell cleanliness Upon completion of the cell calibration pro-
test can be saved and archived. However, the de- cedure, the program computes the Cell Path
Length, and the option to enable the Cell Fring-
1 May, 2009 / v.1.2
Spectro-FTIR User Operation & Maintenance Manual  |  51

ing Correction becomes available. reference (background) interferograms. Gener-


ally both should be selected, however on some
The Refractive Index of Sample value is used to sample cells the fringing is not noticeable on the
compute the fringing correction. This is the re- reference (background) interferogram. In that
fractive index of the material used to create the situation the Correct Reference Igram option can
sample cell. The default value corresponds to the be deselected.
sample cells currently used in the Spectro-FTIR.
The Apply Enhanced Fringe Correction optionis
The Window Size and Ramp Size options are used used to cancell out second order harmonics and
to determine how the correction algorithm is ap- only applies when samples that are extremely clear
plied to the interferogram. The default values of and clean are processed. If the instrument is giv-
70 and 100 are shown in the figure. An increase ing poor repeatability on clean samples, select this
in these values will cause a loss of information in option along with the 2. Sigram Offset.
the spectrum, or if they are set too low, the fring-
ing will become more evident. 3.7.2 Options Tab 2
The Program Options, Option 2 tab is shown in
The Correct Sample Igram and Correct Refer- Figure 3.7-3. The available settings and corre-
ence Igram options determine if the fringe cor- sponding fields are explained in this section.
rection will be performed on the sample and/or A. Program Files

A.

B.

Figure 3.7-3 Options Tab 2

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52  |  Chapter 3 Routine Sample Analysis

This section of the Options 2 tab defines the files shown in the figure.
and folders used by the Spectro Oil Analysis Soft-
ware. Default values are included. 3.7.3 Options Tab 3
The Program Options, Option 3 tab is shown in
Analysis Methods Database File: Figure 3.7-4. The available settings and corre-
This is the file containing the definitions for the sponding fields are explained in this section.
different oil analysis methods. If you move the
file to a different location you should select it us- A. Setup Password
ing the open folder button to the right of the field. Select this button to create/edit/delete a password
to protect the Setup menu options. When a pass-
Experiment Method File: word has been set, the user must enter the correct
This is the parameter file used by the OPUS pro- password before access is granted to any of the
gram to perform the sample and background options on the Setup menu.
measurements. Any experiment method file
(xpm) can be used as long as it is compatible with Click on “Set Password” and a dialog window
the analysis method(s) being used. One file will appears that allows you to edit or delete the pass-
be used for all measurements. word. Press the “Enter” key when changes have
been made.
Sample Spectra Root Path:
This is the root folder where all spectra measured B. Options
by the program will be stored. This section contains general program options
that did not fit into a particular category.
The Store Results in Database is disabled by de-
fault, however, it is good practice to activate it to By default the program is in manual operation
archive analytical results for future reference. It is mode and fuel pumping and cleaning must be
also not possible to review or print reports unless performed manually. Select the Automatic Mea-
the option is enabled. When enabled, all results surement Mode option to enable the use of the
from analyses are stored in a Microsoft Access da- AutoSampler and pump under computer control
tabase. The filename and path can be specified in to measure a rack of samples automatically. Refer
the field below the option. to Automatic Operation, Section 3.4, for more
information.
B. Analysis Results File
When selected, the Store Analysis Results in Enable Perform Hardware Diagnostics option to
CSV file option stores the results of each measure- perform hardware diagnostics on the spectrom-
ment in a comma-delimited text file. The results eter prior to each measurement cycle. The field
can then be imported into a spreadsheet or other to the right of the checkbox contains the URL
program such as the LabTrak Oil Analysis Infor- for the spectrometer. The default URL is entered,
mation Management System. however if you have changed your spectrometer
settings you need to update this field.
The field below the option checkbox specifies the
filename and path of the file. A new background measurement is required each
time the program is started. When selected, the
The remaining checkboxes are used to specify Force New Background option makes it manda-
what information is stored in the file. These are tory to perform a new background measurement
in the order (left to right, top to bottom) that after a specified period of program operation.
they will appear in the file. Typical selections are This is useful if the program is never shutdown
during day-to-day usage. The field to the right

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  53

A.

B.

Figure 3.7-4 Options Tab 3


of the checkbox specifies the time period between manually clears the list.
background measurements in hours. A minimum
setting of 24 hours is recommended, however, 3.7.4 Options Tab 4
more frequent measurements may be required if The Program Options, Option 4 tab is shown in
the laboratory experiences repeated environmen- Figure 3.7-5. This option is only relevant when
tal changes. the Spectro-FTIR is operated in the automatic
mode. It contains the controls to define the pa-
The Always Clean Cell Before a Background op- rameters and test the operation of the AutoSam-
tion forces the program to clean the sample cell pler and peristaltic pump. The available settings
prior to a background measurement in automatic and corresponding fields are explained in this sec-
measurement mode. tion.

The Clear Results List Before Each Measure- A. Auto Sampler Settings
ment option clears the main screen list of analy-
sis results between each measurement. When AutoSampler Driver:
disabled the results are appended until the user In order to use the AutoSampler option, driver
for the AutoSampler accessory must be selected.

1 May, 2009 / v.1.2


54  |  Chapter 3 Routine Sample Analysis

A.

B.

Figure 3.7-5 Options Tab 4


The default driver included with the software is connected to Serial 1 and “1” should be entered
for the Cetac ASX-520 AutoSampler. Select the into the field.
driver by clicking on the open folder button to
the right of the Auto Sampler Driver field. Select Rinse Time is the time the AutoSampler spends
the file “ASX520.dll”. If this is a legitimate driver, cleaning the probe and pumping solvent through
the name of the driver will appear in the text field. the sample line. At the end of this time period
(i.e. “ASX-520 AutoSampler”) a check of the sample cell is performed to deter-
mine if oil or solvent are still present in the cell.
AutoSampler Parameters: If oil is detected, the rinse cycle is repeated. A
There are three parameters for the AutoSampler, typical rinse time is 10 seconds, additional time
COM Port, Rinse Time and Probe Depth. De- may be necessary if the oil samples are exceedingly
fault values are provided. contaminated or heavily sooted.

The COM Port is the serial port number that the Probe Depth is the distance the probe tip will de-
cable from the AutoSampler is attached to the scend into the sample bottle to perform a sample
computer. A typical configuration when per- measurement, and to clean the probe tip. A typi-
formed at Spectro Inc. will have the AutoSampler cal setting for the probe depth is 130 to 135 mm.

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  55

The depth should be decreased if the samples tend


to have a lot of sediment at the bottom or if plen- The COM Port is the serial port number that
ty of sample is available. the cable from the pump is attached to the
computer. If you are connected to Serial 2,
The Manual Probe Position controls at the bot- then enter “2” in the field.
tom of the AutoSampler section are used to test
the operation of the AutoSampler accessory. Pump Speed is the velocity the pump should
use while pumping oil and solvent. The
RESET: Press this button to move the probe maximum speed for the MasterFlex pump is
back to its home position. This resets the 1000 and the default value is 200. During air
alignment of the probe if it has been acciden- pumping, the pump switches to its automatic
tally moved manually. speed automatically.

RINSE: Press this button to initiate a rinse Air Time is the amount of time the pump will
cycle. The probe is returned to the start spend pumping air after rinsing the line with
position and a rinse cycle is initiated. (Note: solvent. If solvent is still detected in the line,
This option does not use the “Use AUX1 for the air time is repeated.
Solvent Pump” option in the Sample Pump
Settings section.) Oil Pump Time is time after oil is detected in
the cell. If no oil is detected after this time pe-
PUMP ON: Pressingthis button engages the riod elapses, the pump will continue to pump
AutoSampler onboard peristaltic pump. oil until the system detects the presence of oil
in the sample cell.
PUMP OFF: Pressing this button disengages the
AutoSampler onboard peristaltic pump. After the sample measurement is complete, the
system will pump air to empty the tubing be-
MOVE: This button moves the probe to the fore solvent is pumped. The Hose Drain Time
X, Y, and Z coordinates given in millimeters field sets the amount of time the air will pump
in the three fields. Type values in the fields before solvent is pumped.
and press the “MOVE” button. If you enter
a value outside of the range of the probe, the The Use AUX1 for Solvent Pump option is
probe will not move. used if you are connecting another MasterFlex
pump (i.e. MasterFlex Model # 77521-40) to
B. Sample Pump Settings the AUX1 connection on the rear of the pump.
In order to use the sample pump with the AutoS- This will be used to power the manual pump as
ampler, the correct Pump Driver must be selected. the solvent pump in lieu of using the onboard
The default driver included with the software is AutoSampler pump.
for the MasterFlex 7550 Computerized Pump.
Select the open folder button to the right of the The remaining controls in this section are used to
Pump Driver field by clicking on it to open a file test the operation of the pump.
dialog. Select the file “Masterflex.dll”. If this is
a legitimate driver the name of the driver will ap- INITIALIZE: Communications with the Mas-
pear in the text field. (i.e. “MasterFlex L/S Pump”) terFlex pump have to be initialized prior to
sending the pump commands. The LED
AutoSampler Parameters: display on the pump will display “P01” when
There are five parameters for the Sample Pump. the pump has been initialized. After selecting
Default values are provided. this button, a dialog will appear informing you

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56  |  Chapter 3 Routine Sample Analysis

of the status of the pump. passed through the cell using the normal peristal-
tic pump in the manual mode or automatically
PUMP STATUS: Press this button to view a dia- with the auto sampler.
log that shows the current status of the pump.
3.8.2 Basic IR Subtraction Theory
PUMP ON: This button turns on the pump FTIR subtraction enables oil properties to be re-
using the speed value set in the “Pump Speed” ported in quantifiable units such as % concentra-
field. tion, this makes diagnosis easier to understand,
and end-users and customers often like to know
PUMP OFF: This button turns off the pump. results in units they can comprehend. In IR
subtraction, a generic calibration curve for each
CONTROL: These controls toggle the pump property is performed and stored in the oil analy-
between Local (manual) and Remote (com- sis software. It is assumed that the absorbance
puter) control. response for each property will be the same when
present in different oil types. However, different
3.8 ENGINE OIL PROPERTY oil types will often have a different zero baseline
CALIBRATION PROCEDURE response for each individual property. Subtract-
ing the fresh oil from the used oil of the same
3.8.1 Introduction base, can eliminate this zero offset. The resulting
This procedure outlines how to calibrate the Spec- subtracted absorbance is equal to the amount of
tro-FTIR spectrometer using spectral subtraction the property itself and it can then be referenced to
so that Fuel, Glycol, and Water can be reported in just the slope of the calibration curve.
quantifiable units.
Important Fact!
It is assumed that the operator has setup the Spec- IR subtraction is a very useful way to have a quan-
trometer for oil analysis and is familiar with run- titative calibration that can serve a host of differ-
ning samples using the Spectro Oil Analysis soft- ent oil types, but it does have one big disadvan-
ware. The relevant fringing corrections need to tage - you must have the same oil matrix in both
have been applied so clean “fringe free” spectrums the used sample and the subtracted fresh oil. If
can be gathered and that the cell path length has not, you will create an artificial offset based on
been calculated Sections 3.1.2 and 3.7.1. the absorbance response in the blank oil which
will cause gross inaccuracies in the final result.
NOTE: More accurate limits of detection can When an oil sample is received for analysis with
be achieved if an optional wedged cell is used to an FTIR spectrometer and the results are required
perform these calibrations. The wedged cell will in % concentration, it’s imperative that the user
eliminate much of the noise at zero levels caused know exactly what the matrix of the fresh oil sam-
by fringing. ple is, and also that a replicated scan of the base
oil is stored on your FTIR. Unfortunately, over
The calibrations for water and glycol contamina- time, used oil in an engine is frequently topped
tion must be undertaken immediately after the off by a mechanic with a multitude of different
standards are shaken so that the water remains in a brands, or even worse, a new and different brand
homogenized state. It is therefore recommended was used without the knowledge of the laboratory
that all oil property calibrations be done manually and the FTIR operator. This will result in many
using lure lock syringes. The oil can be flushed false positives, or even worse a false negative. The
from the cell using a pump on the exit port and response for fuel and glycol is very susceptible to
pentane solvent on the input side. If lure lock sy- these kinds of problems because the response of
ringes are not available, then the standards can be the property is so small in relation to the peak

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  57

already present in the fresh oil itself. the sample and add the contaminant until
the weight gathered from the spreadsheet is
3.8.3 Step-by-Step Calibration Procedure reached to within 0.01 grams.
In order to create IR subtraction calibrations, a. Fuel – 0, 2, 5, 8, 10 %
fresh oil types that you plan to analyze will be b. Water – 0, 0.1 , 0.25 , 0.5, 0.75%
required along with quantities of fuel, water and c. Glycol - 0, 0.1 , 0.2 , 0.3 , 0.5 %
glycol which will be mixed in exact amounts with
the fresh oils. The procedure also requires the use Note: It is very important that the diesel fuel be
of a spreadsheet called “ftir_subtraction_tools.xls” weathered to simulate the fuel contaminate in a
and a copy of Microsoft Excel. The “ftir_subtrac- crankcase. Heat the fuel to 107 degrees C then
tion_tools.xls” spreadsheet can be downloaded hold it at this temperature for 30 minutes. This
from the Spectro Inc. web site by using the part- represents a loss of around 5% by weight.
ner Login feature and selecting “Documented
Procedures” after logging in. Note: Glycol standards should be made using
a 50:50 mixture of glycol based antifreeze and
NOTE: This procedure assumes that the user has water.
operating experience with the Spectro-FTIR and
a detailed knowledge of the Spectro-FTIR Oil 6. Make sure to thoroughly shake each of the
Analysis Software. Experience in mixing fluids samples to ensure that the contaminant prop-
to create standards by weight is also essential. If erty gets into complete suspension in the fluid.
you are unsure about any of this, contact some- Extra care needs to be taken with the water and
one in your organization who has knowledge in glycol standards because these properties are
this area or contact your local representative for difficult to homogenize. Placing these samples
assistance. in an ultrasonic bath will help homogenize the
water and the glycol.
Follow the step-by-step procedure below to create 7. Ensure that the cell is clean and collect a
the required calibration curves. fresh background.
8. Do the following calibrations in this order:
1. Gather all the fresh oil types from engine Water, Fuel, Glycol – start with zero and work
oils that you plan to run on the FTIR. up to the highest concentration. Ensure to
2. Store a scan of each fresh oil type on the shake the water and Glycol standards thor-
FTIR using the standard Direct Trending oughly before injecting.
Method. 9. Use the corresponding individual prop-
3. Rename the spectral files with the oil type erty methods (e.g. Spectral subtraction diesel
and put them in the computer’s subtraction_ calibration) on the Main Oil Analysis screen
spectra folder in the spectro oil analysis folder. to analyze each calibration set. Enter at least 4
ml of oil into the top of the cell using lurelock
CAUTION: Ensure that the .0001 extension is syringes if possible. Reconnect the hose and
not removed, (example: citgo_10w40.001). flush the cell and check for cleanliness before
entering the next sample. Make note of the re-
4. Open the ftir_subtraction.xls tools work sulting absorbance value in the Analytical Re-
sheet. sults screen and enter it in the corresponding
5. Create the following five standards by % box on the worksheet. As you enter more
weight for each property making sure to tare values a linear calibration curve will begin to
the scale with the empty bottle for each cali- form in the graph box.
bration standard. After adding the oil, and 10. After each property calibration set is com-
recording the weight on the spreadsheet, tare plete, flush out the oil thoroughly with pen-

1 May, 2009 / v.1.2


58  |  Chapter 3 Routine Sample Analysis

tane and dry the cell in preparation of the next


calibration set. Check the cell cleanliness and NOTE: Negative values that are close to zero are
take a fresh background for each oil property considered zero. If you get values that are very
set and repeat step 9 for each property. negative or are unrealistically positive, then the
11. If care was taken to homogenize each fresh oil probably does not match the used oil
standard, the calibration curves should be base and the offset between the two is causing a
very close to linear for each property. The R2 false result.
correlation coefficient dictates the fit of the
data points used in each calibration. The value Please contact support@spectroinc.com or appli-
should be at least 0.95 (95%). If the fit is less cations@spectroinc.com for further help.
than this value then it’s suggested to repeat the
calibration steps from step 6 exactly as they are 3.9 INTERPRETING SPECTRO-FTIR
stated with emphasis on thorough shaking of OIL ANALYSIS DATa
the samples.
12. Open the spectral subtraction crankcase 3.9.1 Introduction
E2412 method file so you can edit the proper- In recent years molecular spectrometric analysis
ties. by IR (infrared) has been applied to in-service oil
13. Note down the slope of each property analysis. Its value lies principally in the fact that
calibration curve in your worksheet. The slope it is a purely instrument-based test (meaning it
is the number that precedes the x (e.g. y=4x+2, does not need extensive sample preparation or
slope = 4). wet chemistry), it is relatively quick to perform
14. Enter the slope for each oil property into and is capable of simultaneously detecting mul-
the “use procedure formula“ box for each oil tiple parameters. Although often backed up with
property in the spectral subtraction crankcase standard ASTM methods when more precision
E2412 method file. If the slope is 4 you would is required, it is excellent for trending techniques
enter value*4. Important we DO NOT add where changes in data are indicative of lubricant
an offset into this formula because the new oil contamination and/ or degradation.
subtraction will eliminate this.
15. Repeat step 14 for each oil property. In-service oil analysis using the IR technique has
16. Save the method file and open it again to been widely accepted over the past few years, and
ensure that all changes made are still there. instrument manufacturers such as Spectro Inc.
17. You are now ready to run spectral subtrac- provide custom software with analytical methods
tion on a used oil sample. Clean the cell thor- for the typical physical property analysis. A one-
oughly with solvent and take a clean cell back- minute analysis provides information on oil con-
ground. Enter a sample number and select the taminants include water, blow-by products (soot),
spectral subtraction crankcase E2412 method coolant chemicals (ethylene glycol) and unburned
file from the list. The spectra for subtrac- fuel and degradation based on nitration, oxida-
tion box will now have become white so you tion, and sulfation. Chemometric techniques are
can browse to the fresh oil sample spectra that sometimes also applied to effectively analyze TAN
matches the makeup oil of the used sample you (total acid number) and TBN (total base number)
are going to analyze. with IR instruments.
18. Fuel, water and glycol results will now be
reported in % values. This section of the chapter provides basic guide-
lines for lubricant degradation and contamina-
NOTE: If you wish to report values in ppm, then tion analysis by FTIR spectroscopy. These limits
multiply the slope value by 10000 and update the provided should only be used as a GUIDELINE!
value in the use procedure formula box. The actual allowable limits specified by OEM’s

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  59

(Original Equipment Manufacturers) may vary oil lowers overall viscosity, but continuous water
somewhat from these values. Also, the ever- contamination eventually causes oxidation and
changing formulation of high performance addi- viscosity increase.
tive packages in the highly competitive lubricant
market may also have some effect on the values 3.9.2.1 Water in Extreme Pressure (EP)
stated in this guide. Guidelines are provided for: Additive Fluids
These limits apply to mineral / synthetic gear lu-
• Water Contamination, Section 3.9.2 bricants and hydraulics with EP additive pack-
• Soot Contamination, Section 3.9.3 ages.
• Glycol (antifreeze) Contamination, Section
3.9.4 Normal and Abnormal Limits
• Fuel Contamination, Section 3.9.5 • Synthetic Hydraulic Ground Equipment:
• Degradation based on Nitration, Section Normal <200 ppm, Alert at 1000ppm
3.9.6 • Synthetic Hydraulic Air Equipment: Normal
• Degradation based on Oxidation, Section <20ppm, Alert at 350ppm
3.9.7
• Degradation based on Sulfation, Section NOTE: This is only used for EP additive fluids,
3.9.8 it is not to be used for synthetic turbine oils or
• Lubricant Breakdown, Section 3.9.9 petroleum crankcase oils
• Antiwear Reading (ZDDP) Additive, Section
3.9.10 3.9.2.2 Water in Synthetic Turbine Lubricants
These limits apply to water measurement in Syn-
Reference ASTM E 2412 & JOAP thetic (polyol ester) lubricants used in high per-
formance jet engines. Common lubricants in this
3.9.2 Water Contamination class are Mil-PRF-7808 and Mil-PRF-23699.
The presence of water needs to be monitored be-
cause it can cause costly breakdowns due to inter- Normal and Abnormal Limits
nal corrosion and lubricant degradation. Through • Synthetic Turbine Lubes: Normal 0-30 abs
periodic oil analysis with instruments such as the units, Alert at 45 units (approx 1000ppm)
Spectro-FTIR, water can be detected giving the
user the opportunity to react accordingly and 3.9.3 Soot Contamination
make adjustments to rectify the problem before it Soot in used oil is an indication of the amount
gets out of hand. of insoluble carbon suspended in the lubricant.
Soot particles are extremely small, on the order of
Water contamination in lubricating oils or hy- 0.01 µm. They are carbon left over from incom-
draulic fluids comes from two primary sources, plete combustion of the hydrocarbon molecules
leaks in the system or condensation of moisture in diesel fuel. Dispersant additives are present in
in the air space. Large amounts of free water will diesel engine lubricants to prevent soot particles
separate and settle to the base of the lubricating from agglomerating and plugging oil filters that
system reservoir. Most lubricants and hydraulic are meant to capture hard, abrasive particles. Soot
fluids will dissolve small amounts of water, how- by itself is not harmful to diesel engine operation,
ever, the presence of water over approximately 1% but excessive levels of fuel soot in an oil sample are
is detrimental to the formation of an oil film and typically due to an incorrect air/fuel ration due to
thus promotes metal-to-metal contact of rotat- restricted airflow in a filter that results in an in-
ing equipment resulting in abnormal wear. The sufficient air supply to the combustion chamber.
presence of water accelerates oil oxidation and High levels of fuel soot when not corrected will
subsequent oil thickening. At first, water in the lead to oil thickening, the formation of deposits,

1 May, 2009 / v.1.2


60  |  Chapter 3 Routine Sample Analysis

and a reduction in the protective antiwear addi- applicable to synthetic lubricants.


tives in the lubricant.
3.9.5 Fuel Contamination
Infrared Spectroscopy is the preferred method to Fuel contamination in a used oil or hydraulic sys-
determine soot in a used oil sample. tem is a measure of the fuel present in the sample.
In diesel engines, fuel dilution is usually caused
These limits apply to monitoring soot loading in by excessive idling, defective injectors, or loose
diesel crankcase engine oils. connections. In aircraft turbines, the usual cause
for fuel dilution is leakage of an inter-cooler. In
Normal and Abnormal Limits all instances, excessive fuel in the lubricant or hy-
• Diesel Engines: Normal <20 abs units, draulic fluid reduces the oil film strength due to
Borderline 40 abs units, Alert at 50 abs units viscosity decrease, thus increasing metal-to metal
(50 units = ~ 3% soot) contact and wear. Excessive fuel also leads to pre-
mature oil oxidation.
NOTE: Non sooted fluids will show non-zero
(negative readings) which is due to the transmit- Through periodic oil analysis, with instruments
tance characteristics of the fluid. such as the Spectro FTIR, fuel dilution can be de-
tected giving the user the an opportunity to react
3.9.4 Glycol Contamination accordingly and make adjustments to rectify the
Coolant system leakage is one of the most serious problem before it gets out of hand.
hazards for any lubricating system. Glycol from
antifreeze breaks down at normal engine tempera- 3.9.5.1 Diesel Fuel Contamination
tures and forms sludge and deposits. Water in the These limits apply to monitoring used oil samples
coolant reduces lubricity and can cause corrosion for JP-5 or JP-8 fuel contamination in mineral
and premature wear. and synthetic lubricants.

An analysis for water by itself may not be reliable Normal and Abnormal Limits
enough since engine temperatures will vaporize • Diesel Engines: Normal 220-230 abs units
low levels of water. Infrared spectroscopy with (E2412 method using multiplier), Alert at
the Spectro-FTIR can also be applied to detect >255 abs units.
antifreeze contamination.
3.9.5.2 Gasoline Fuel Contamination
These limits apply to monitoring the presence of Limit guidelines for gasoline contamination are
Ethylene Glycol (Antifreeze) in crankcase lubri- not available due to the very small number of gas-
cants. oline engines enrolled in condition monitoring
programs, therefore, abnormal and normal values
Normal and Abnormal Limits have not been set. In most cases, using subtrac-
• Diesel Engines: Normal 0-1 abs units , Alert tion will produce a value of close to zero.
at >3 abs units
3.9.6 Degradation based on Nitration
NOTE: As ethylene glycol is approximately a Nitration is similar to oxidation. Nitration results
50:50 dilution with water, a valid glycol alarm from the reaction of oil components with nitro-
should also produce a high water reading for the gen oxides that are produced from the oxidation
mineral water band. A strong glycol reading with of atmospheric nitrogen during the combustion
a low water reading may indicate contamination process. In addition to causing oil thickening, ni-
of a water free silicone fluid. This reading is not tration products are the major cause of the build-
up of varnish or lacquer on engine parts.

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  61

ual classes of diesel engines as well as other gear


A test for lubricant degradation due to nitration boxes and hydraulic systems will be dependant
is commonly applied to four-cycle and natural gas upon the amount of oxidation typically produced
engines. Nitration byproducts are rarely found in such systems and how well the lubricant can
in diesel engines, and if so, a serious operational neutralize the by-products.
problem is probably its source.
Normal and Abnormal Limits
These limits apply to the monitoring of the • Diesel Engines: Normal: Between 6 – 12 abs
buildup of nitration products in mineral based units, Alert at > 18 abs units
lubricants. The limits have been based on a large
population of high speed diesel engines. Normal 3.9.8 Degradation based on Sulfation
and abnormal values for individual classes of die- As engine oils continue in service, combustion
sel engines as well as other gear boxes and hydrau- gases combine with the oil resulting in the for-
lic systems will be dependant upon the amount mation of acids that are corrosive to the surfaces
of oxidation typically produced in such systems with which they come in contact. Sulfur in fuel
and how well the lubricant can neutralize the by- may cause the formation of strong sulfuric acid.
products. Alkaline additives are used to neutralize this ef-
fect. The reserve alkalinity or the remaining abil-
Normal and Abnormal Limits ity of these basic compounds to neutralize acidic
• Diesel Engines: Normal <3-8 abs units, Alert compounds is measured by the total base number
at >14 abs units (TBN) of the oil. Sulfation correlates inversely
with TBN.
3.9.7 Degradation based on Oxidation
Oxidation is perhaps the most predominant Sulfation as determined with an infrared spec-
problem as a lubricant remains in service. It is trometer, such as the Spectro is a measure of the
a form of lubricant degradation responsible for decline of a lubricant’s ability to combat acidity.
numerous lubricant problems including viscos- It complies with ASTM E 2412. For specific oils
ity increase, varnish, sludge and sediment forma- in specific applications it is possible to use IR
tion, additive depletion, base oil breakdown, filter spectroscopy as a direct measure of TBN. This
plugging, loss of lubricity, loss in foam control, is done by using a partial least squares regression
acid number (AN) increase, rust formation and of the spectra of numerous samples in which the
corrosion. Oxidation occurs as lubricant mol- TBN has been determined by standard analytical
ecules are exposed to oxygen over long time pe- methods. This is sometimes also referred to as
riods and is accelerated by high operating tem- Chemometric calibration.
perature. Therefore, monitoring and controlling
oxidation is a priority of any machine condition These limits apply to monitoring oxidized sulfur
monitoring program. compounds in mineral based engine crankcases,
gearboxes and hydraulic systems. Such com-
Oxidation is determined analytically by the pounds come from sulfur compounds in the fuel
amount of infrared light absorbed by oxidation or lubricant additive compounds.
products.
Normal and Abnormal Limits
These limits apply to the monitoring of the build- • Diesel Engines: Normal <10-15 abs units,
up of oxidation products in mineral based lubri- Alert at 35 abs units
cants and hydraulic fluids. The limits have been • Mil-L-17331: Normal<13 abs units, Alert at
based on a large population of high speed diesel 20 abs units
engines. Normal and abnormal values for individ-

1 May, 2009 / v.1.2


62  |  Chapter 3 Routine Sample Analysis

NOTE: Sulfation measurement not applicable in 3.9.10 Antiwear Reading (ZDDP) Additives
synthetic based lubes. The most common additive in many different
classes of lubricants, from engine oils to antiwear
3.9.9 Lubricant Breakdown hydraulic fluids is ZDDP. The initial concentra-
Lubricant antioxidants are additives that enhance tion of ZDDP in any oil can be determined by
a lubricant’s thermal stability, improve perfor- measuring zinc and phosphorus levels using and
mance and reduce sludge formation, thus extend- elemental analysis technique such as atomic emis-
ing the useful life of lubricants in virtually any sion spectroscopy. However, emission spectros-
application. They reduce thickening and inhibit copy cannot not be used to monitor in-service
acid formation in a variety of applications, in- ZDDP additive depletion. In-service ZDDP
cluding engine oils, automatic transmission flu- depletion is best measured by molecular spectros-
ids, industrial oils, as well as compressor oil and copy such as FTIR.
gear and hydraulic oils. ASTM E 2412 refers to
two types of lubricant breakdown, Breakdown I These limits apply to monitoring Phosphate an-
and Breakdown II. tiwear compound levels in mineral and synthetic
lubricants.
3.9.9.1 Breakdown I Synthetic Lubricants
These limits apply monitoring the breakdown of Normal and Abnormal Limits
Synthetic (Polyol Ester) Jet Engine Turbine Lu- • Diesel Engines: Normal 8-12 abs units, Alert
bricants. at <5 abs units
• Synthetic Turbines: Normal 95-110 abs
Normal and Abnormal Limits units, Alert at <80 abs units
• Normal <30 for Synthetic turbine lubri-
cants, Alert at 45 Units (approx TAN 1.0 3.10 SOLVENT REQUIREMENTS FOR
mgKOH/g) THE SPECTRO-FTIR

NOTE: The limits and methods do not apply to There are several criteria for choosing a rinse sol-
mineral based oils, result may increase due to vent for the Spectro FT-IR Oil Analyzer. Among
increase in water levels. these are:
- The solvent must be a good oil solvent to dis-
3.9.9.2 Breakdown II Synthetic and Water in solve whatever oil is left in the cell and tubing
Petroleum Lubricants of the flow path.
These limits apply to additional monitoring of - The solvent needs to evaporate quickly so
degradation of polyol ester synthetic turbine oils that no solvent remains in the cell and tub-
and are used as the primary monitoring method ing. This is important both for collecting a
for water in high detergent/ dispersant mineral good clean cell background as described in
based lubricants, typically crankcase oils. It can Section 2.1 and for preventing samples from
also be used as secondary monitoring of water in becoming contaminated with rinse solvent
EP additive lubes. when they are pumped into the cell for analy-
sis.
Normal and Abnormal Limits - The solvent need not be very expensive.
• Mineral Crankcase Oils: Normal <30 abs Reagent grade (high purity) solvent is not
units, Alert at 45 abs units necessary.
• Synthetic polyol –Ester Turbine Oils: Normal - The solvent should conform to local regula-
< 20 abs units, Alert at 24 abs units tions regarding hazardous and toxic sub-
50 units = ~ 1000ppm stances.

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  63

The solvent needs to evaporate out of the cell and will not evaporate as quickly and it will take more
the tubing leading to the cell so that the FT-IR time to dry the cell for background collection and
can obtain a hydrocarbon free background dur- the chance of contaminating the oil sample with
ing background collection and when running solvent will be greater.
used oil samples. Also, during routine analysis,
hydrocarbons remaining from the solvent may
interfere with the spectra collected from the oil
sample.  The fuel measurement is especially sensi-
tive to any solvent remaining in the cell or tubing
because the spectral signature of the solvent may
be similar to that of the fuel.

Therefore, it is necessary to use a solvent that


evaporates as quickly as possible while still being
a good solvent for oil.  Pentane is the lowest boil-
ing point hydrocarbon that is still liquid at room
temperature.  Pentane has 5 carbon atoms in its
molecular structure.  If it had 4 hydrocarbons, it
would be butane and it would be a gas at room
temperature. Pentane is the best possible solvent
for this application, but it is not necessary to use
reagent grade pentane, nor is it absolutely neces-
sary to use a solvent containing only pentane.  The
solvent can be a mixture of light hydrocarbons,
those containing 5, 6 or 7 carbon atoms in the
molecular structure.  In English, such a mixture
of highly volatile liquid (at room temperature)
hydrocarbons is called “Petroleum Ether”.  A
mixture that has a somewhat higher boiling point
range is called “Naphtha”.  It is recommended
to find a technical grade (not the purest or most
expensive) pentane, hexane, petroleum ether or
naphtha.  At Spectro, in Massachusetts, we use
technical grade pentane in 5 gal (about 20 liters)
containers costing approximately $200.
Regarding terminology, sometimes pentane or
hexane are supplied as “pentanes” or “hexanes”.
This is due to the fact that pentane and hexane
have isomers, that is the carbon atoms may not be
in a straight chain, but may be branched. Isomers
have nearly identical physical properties. There-
fore using “pentanes” or “hexanes” is entirely ac-
ceptable.

Please note that the best solvent is pentane and


any solvent containing larger molecules (more
than 5 carbon atoms per hydrocarbon molecule)

1 May, 2009 / v.1.2


64  |  Chapter 3 Routine Sample Analysis

This Page is Intentionally Left Blank

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  65

Chapter 4 4.0 USER MAINTENANCE

This chapter describes the most common Spectro-


FTIR problems, their potential causes and recom-
mended solutions. The Spectro-FTIR is designed
in a way that the operator can identify and cor-

User rect many faults without requiring the support of


the Spectro Inc. Service Department. In case of
failure, it is strongly recommended that you first

Maintenance perform a diagnosis using the OQ and PQ tests.


This chapter provides troubleshooting hints and
step-by-step procedures to replace major compo-
nents.

CAUTION: Perform only the maintenance func-


tions that are described in this manual. Adhere
strictly to the described procedures and observe
the relevant safety precautions. Otherwise,
personal injury and/or spectrometer damage can
be the result. In this case, Spectro Inc. does not
assume any liability. Only Spectro Inc. Service
Personnel should perform maintenance work that
is not described in this manual.

4.1 TROUBLESHOOTING

This section deals with the following spectrometer


problems:

• 4.1.1 All power supply LEDs are off.


• 4.1.2 One power supply LED is off.
• 4.1.3 No Data Transfer between Spectro-
FTIR and the Computer.
• 4.1.4 No interferogram is observable in the
Check Signal Dialog
• 4.1.5 Signal-to-noise ratio is too low.
• 4.1.6 Insufficient energy at the end of the
spectrum (i.e. at high wavenumber).
• 4.1.7 H2O band absorption is too high
• 4.1.8 Spectral resolution is not reached
• 4.1.9 Incorrect abscissa (cm-1) calibration

4.1.1 All Power Supply LEDs are Off


The power supply LEDs, Figure 4.1-1 are at the
spectrometer rear side, labeled +5V, +12V and
-12V. These LEDs indicate the state of the sec-
ondary voltages of the electronics unit.

1 May, 2009 / v.1.2


66  |  Chapter 4 User Maintenence

+5 Volt

+12 Volt

-12Volt

Figure 4.1-1, Rear View, Power Supply LEDs

Probable Cause Solutions


Spectrometer is not turned on. Turn on the spectrometer using the main power switch.
Power cord not is connected. Connect the power cord to the power outlet as well as to the
appliance inlet connector.
No voltage is applied. Check whether the proper voltage is applied at the outlet to
which the spectrometer is connected.
Defective fuse. Replace the fuse. (See Section 4.2).
Short circuit in the power supply unit. Typically, a short circuit is accompanied by a “ticking” sound
in the power supply unit. Disconnect the power supply unit im-
mediately. If there are additional external circuitry connected
to the CAN bus or the MPE port, disconnect them and try it
again. If this measure solves the problem the external cir-
cuitry has caused the short circuit. Otherwise, it is an internal
problem of the spectrometer electronics. Contact your local
Spectro Inc. service representative.
Defective power supply unit. If the power supply LEDs do not light correctly, the power sup-
ply unit probably needs to be replaced. If they do not light at
all, contact your local Spectro Inc. service representative

Probable Cause Solutions


An external device shortens the power Disconnect all external devices from the CAN bus or the
supply unit. MPE port and try it again.
Temporary short circuit in the spectrom- Switch off the spectrometer, wait about 30 seconds and
eter. switch it on again. After the initialization cycle the power
supply LED will turn to green.
A defective LED. In this case there is no spectrometer malfunction and the
spectrometer operates properly. Only the defective LED
needs to be replaced.

1 May, 2009 / v.1.2


Spectro-FTIR User Operation & Maintenance Manual  |  67

4.1.2 One Power Supply LED is Off

4.1.3 No Data Transfer between Spectro-FTIR and the Computer

In this case the troubleshooting procedure depends on the connection topology. The default con-
nection (stand-alone configuration) is established using a cross-over cable between the PC and the
spectrometer, Section 1.3.2. Alternatively, the spectrometer can be connected directly to an Ethernet
network using the Ethernet port. The direction of the data transfer is indicated by the RX and TX
LEDs on the spectrometer’s rear. The TX LED lights when the spectrometer sends data and the RX
LED lights when the spectrometer receives data.

4.1.3.1 The Green RX LED Does Not Light


This fault indicates a problem with regard to the physical connection between the spectrometer and
the PC or the network.
Probable Cause Solutions
Wrong cable type is used. If the Spectro-FTIR is connected directly to a PC a cross-over
Ethernet cable must be used. If the Spectro-FTIR is con-
nected to a network, a regular Ethernet cable must be used.
Verify that this is the case.
Defective cable or unstable connection. Check the RJ-45 connection to the Ethernet port and at the
other end of the cable. Replace the cable, if necessary.
Spectrometer does not start up. Check the main power supply. All the power supply LEDs
+5V, +12V and -12V must light when the spectrometer is
switched on
4.1.3.2 The Green RX LED Lights but the Yellow TX Does Not
This indicates that there is no logic connection between the spectrometer and the network or the
computer.
Probable Cause Solutions
Wrong IP address has been assigned to Assign the correct IP address to the spectrometer. You find
the spectrometer. the correct IP address on a label on
the spectrometer rear side. The procedure is detailed in
Section 2.1.
TCP/IP settings mismatch between spec- Refer to Section 1.3.2.
trometer and computer/network.

4.1.3.3 The SR LED Stays ON


The SR LED indicates whether the instrument is busy and not available for communication.
Probable Cause Solutions
Spectrometer is still in the initialization After switching on the spectrometer wait about one minute
phase until the initialization procedure is completed.
Spectrometer controls hang up. Reset the spectrometer using the reset button at the spec-
trometer rear, Figure 1.2-5 and wait for initialization to ter-
minate. If this measure does not solve the problem, contact
your local Spectro Inc. Service Representative.

1 May, 2009 / v.1.2


68  |  Chapter 4 User Maintenence

4.1.4 No Interferogram in the Check Signal Dialog


This problem can have the following possible causes if the computer can access the spectrometer and
that there is an optical connection between the interferometer outlet and the detector inlet.
Probable Cause Solutions
Optical path is blocked. Check whether the accessory in the sample compartment
blocks the IR beam.
Defective or not correctly inserted IR Check whether the IR source is inserted properly or replace
source. In this case the error message the IR source, if it is defective. (See Section 4.3.)
Source is broken or not connected ap-
pears.
Detector is not installed or incorrectly Check whether the detector is inserted properly in the dove-
installed. In this case the error message tail guide.
Device not connected. No analog board
selected appears.
Beam splitter is not properly installed. Check whether the beam splitter is properly installed. If the
In this case the following error message beam splitter is damaged replace it and check the signal
appears: NOT SCANNING. Laser-A (Check Signal dialog window of the OPUS software).
modulation too small, Laser-B modula-
tion too small, Laser signal modulation is
to small. Beam splitter is damaged prob-
ably due to much moisture in the system.
The red ERR LED on the spectrom- In case of an optics misalignment, contact your local Spectro
eter rear side lights up, i.e. there is a Inc. Service Representative. I n case of a defective laser, a
spectrometer error, for example, strong warning will be displayed by the application software. Re-
mechanical shocks have caused a tem- place the laser unit. (See Section 4.5).
porary or permanent optics misalignment
or the HeNe laser is defective.
Defective power supply unit. Check the power supply LEDs on the spectrometer rear
side. If none of the LEDs lights, the power supply unit prob-
ably needs to be replaced. Contact your local Spectro Inc.
Service Representative.
Detector saturated or A/D converter Either reduce the light source intensity by using a smaller
overflow aperture or reduce the gain settings.

4.1.5 Signal-to-Noise Ratio is Too Low

Probable Cause Solutions


Energy throughput is too low. See Section 4.1.4, No Interferogram in the Check Signal
Dialog Window earlier in this chapter.
IR source is switched off. Switch on the IR source (using software).
Defective IR source. In this case the Replace IR Source, see Section 4.3.
error message Source is broke or not
connected appears.
Interferometer is out of alignment. Contact your Spectro Inc. Service Representative.

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Spectro-FTIR User Operation & Maintenance Manual  |  69

4.1.6 Insufficient Energy at the End of the Spectrum (High Wavenumbers)

Probable Cause Solutions


Defective IR source. In this case the Replace IR Source, see Section 4.3.
error message Source is broke or not
connected appears.
Interferometer is out of alignment. Contact your Spectro Inc. Service Representative.

4.1.7 H2O Band Absorption is Too High


Probable Cause Solutions
Desiccant cartridge requires regenera- Substitute the installed desiccant cartridges for a regener-
tion. ated or new one, see Section 4.2.
Air humidity level inside the sample com- Purge sample compartment with dry air or nitrogen gas. (If
partment is too high. option is installed).

4.1.8 Spectral Resolution is not Reached


Probable Cause Solutions
Wrong aperture is selected. Decrease aperture size.
Optical system is out of alignment Contact your Spectro Inc. Service Representative.

4.1.9 Incorrect Abscissa (cm-1) Calibration

Probable Cause Solutions


For measurements requiring maximum Perform a PQ test. Check the H2O peak positions and cor-
precision, an abscissa calibration has to rect any deviations from the exact value by adjusting the
be performed after changing a compo- laser wavenumber. To do this, select in the OPUS Measure
nent (e.g. laser module, b detector etc., menu the Optic Setup and Service function. Click on the
except desiccant cartridge). Interferometer/ AQP tab and enter the laser wavenumber in
the corresponding entry field. If you work according to GMP
standards do not forget to perform an instrument validation
after correcting the laser wavenumber.

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70  |  Chapter 4 User Maintenence

4.2 REPLACING AND REGENERATING latch that is opened with an Allen screw that is
THE DESICCANT IN A located at the left spectrometer side and covered
CARTRIDGE by a black cap.

The desiccant in cartridges must be replaced and 1. Remove this plug and loosen the Allen
regenerated in regular intervals to ensure opti- screw (approximately half a turn)
mum spectrometer performance in case the Spec- using an Allen wrench (6mm), Figure 4.2-2.
tro-FTIR is not purged. 2. Remove the detector compartment lid.
3. Pull the desiccant cartridge out of the
High air humidity level inside the spectrometer holder and inspect the cartrige.
impairs the measurement results. Therefore, a 4 . Insert a new or regenerated desiccant into
desiccant (molecular sieve) is used to reduce the the holder. Ensure that the cartridge top side
air humidity level inside the interferometer and (with the label ’TOP’) is up.
detector compartments. Although these com- 5. Re-install the detector compartment lid by
partments are sealed, the air humidity can reach a performing the above steps (1and 2) in reverse
high level, for example, if the covers are removed order.
because of a component change. The Spectro-
FTIR is equipped with two desiccant cartridges,
one is in the detector compartment and the other
in the interferometer compartment, Figure 4.2-1.
The desiccant cartridges should be regenerated or
replaced approximately every 6 months or at least
when the electronic HUMIDITY indicator (Sec-
tion 1.2.1) on the top of the spectrometer lights
up red.

4.2.1 Replacing the Detector Compartment


Desiccant
The detector compartment lid is secured with a
Figure 4.2-2 Location of Desiccant Cartriges

Detector Interferometer
Desiccant Desiccant
Cartridge Cartridge

Figure 4.2-1, Location of Desiccant Cartriges

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Spectro-FTIR User Operation & Maintenance Manual  |  71

4.2.2 Replacing the Interferometer 3. Place the spent molecular sieves in a oven
Compartment Desiccant for at least 24 hours at a temperature of 150
The interferometer compartment lid is secured °C.
with a latch that is opened with an Allen screw 4. Refill the desiccant cartridge with the hot,
that is located inside the source/laser compart- dried sieves and push the black cap on the
ment. white tube.
5. Store the regenerated cartridge in a dry en-
1. Open the source/laser compartment by vironment (e.g. exicator) until a spent cartridge
pressing down near the middle front of the lid needs to be replaced by regenerated one.
and lift it to its full open position.
2. Loosen the Allen screw shown in Figure 4.3 REPLACING THE IR SOURCE
4.2-3 by approximately half a turn using a
6mm Allen wrench to unlatch the interferom- The IR sources are pre-aligned and electrically
eter compartment lid. coded enabling the spectrometer firmware to
3. Take off the interferometer compartment auto-detect the source type. This information is
lid. passed on to the application software, which in
4. Pull the desiccant cartridge out of the turn selects the appropriate parameter set for the
holder and inspect the cartridge. measurement.
5 . Insert a new or regenerated desiccant into
the holder. Ensure that the cartridge top side WARNING: During the spectrometer operation
(with the label ’TOP’) is up. the light source becomes very hot. Avoid any skin
6. Re-install the lids of the interferometer contact. Risk of skin burn! Wait until the light
compartment and the source compartment by source has cooled down sufficiently before you
performing the above steps (1 and 3) in reverse remove it.
order.
To replace the IR source:
4.2.3 Desiccant Cartridge Regeneration 1. Switch OFF the Spectro-FTIR.
Procedure 2. Open the source/laser compartment by
1. Pull off the top black cap (with the label pressing down near the middle front of the lid
’Top’) from the white tube. and lift it to its full open position.
2. Empty the desiccant (molecular sieve) into
a container that can withstand a temperature CAUTION: Wait until the IR source has cooled
of 150 °C. down to room temperature.
Open Compartment with 6mm Allen Wrench
3. Loosen the knurled thumb screw of the IR
source release lever (approximately one turn),
Figure 4.3-1.
4. Press the IR source slightly downwards
while rotating the release lever aside.
5. Take the IR source carefully out of the
holder using the IR source handle.
6. Remove the new IR source from its box
and insert it into the operating position holder.
Ensure that the two pins of the holder engage
in the holes of the IR source.
7. Gently press the IR source downwards and
Figure 4.2-3, Latch for Source/Laser rotate the release lever over the source to secure
Compartment

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72  |  Chapter 4 User Maintenence

Thumb Screw & Release Lever


Figure 4.3-3, Measurement Options Screen
Figure 4.3-1, IR Source
it.
8. Tighten the knurled thumb screw of the
release lever (about one turn).
9. The height of the new IR source must be
adjusted for maximum signal. If not already
open, go to the OPUS software.
10. Switch ON the Spectro-FTIR.
11. Open the OPUS software by double click-
ing on its icon. When the software opens, the
OPUS Login screen appears and a password
must be entered. The User ID is “Default” and
the Password is “OPUS” (all capital letters, no Figure 4.3-4, Check Signal Screen
quotation marks). Click on “Login” to start
the software. source in and out until maximum signal is
12. On the OPUS default screen select “Mea- obtained.
sure” and from the drop-down menu select
14. When maximum signal has been obtained,
“Advanced Measurment”, Figure 4.3-2. close the source/laser compartment lid by
13. The “Measurement options” screen ap- pressing new the front middle of the lid.
pears, Figure 4.3-3. Select the “Check Signal”
tab. 4.4 REPLACING THE WINDOWS
14. Note the signal peak for the current IR
source height position, see example in Figure In the Spectro-FTIR, the sample compartment is
4.3-4. separated from the interferometer compartment
15. Adjust the thumb screw that holds the IR and the detector compartment by KBr windows,
Figure 4.4-1. In the course of time, fumes and
dust will deposit on the windows so that the
transparency (infrared transmittance) is seriously
reduced. When these windows become dull, they
must to be replaced. After they are replaced, they
must be rotated to maximize signal throughput.

The procedure to remove and replace a widow is


identical for both sample stand windows. A flange
Figure 4.3-2, Measure Drop-down Menu
removal tool is supplied with the Spectro-FTIR to

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Spectro-FTIR User Operation & Maintenance Manual  |  73

Sample Compartment Windows counterclockwise and remove the complete


window flange assembly from the sample com-
partment wall.

CAUTION: Handle the windows with great care


because they are made of fragile material that
cracks under influence of mechanical pressure.
Do not touch the window surface.

3. Place the window flange assembly on an


even surface with the retainer ring pointing
upwards.
4. Insert the corresponding pins of the flange
Figure 4.4-1, Sample Compartment Windows removal tool into the holes of the retainer ring
assist in the removal and replacement process. To and rotate the tool counterclockwise.
remove and replace a window: 5. Disassemble the window flange assembly.
6. If required, replace the window.
The windows are attached to sample compartment 7. Assemble the individual flange parts as
walls by means of a bayonet socket. The socket shown in Figure 4.4-2.
has 4 flanges and the lens assembly can thus be 8. Insert the corresponding pins of the flange
place in 4 different rotation positions. Replace- removal tool into the holes of the retainer ring
ment of windows is a two part process. First the and rotate the tool clockwise to lock the win-
window is physically removed and replaced and dow in flange assembly.
second, it is rotated to its maximum throughput 9. Insert the pins of the flange removal tool
position. into the corresponding holes of the window
flange assembly.
CAUTION: Wear gloves while performing the 10. Install the window flange assembly in
procedure as contact with bare hands may lead to the sample compartment wall and rotate the
irreversible contamination. window flange removal tool clockwise until the
assembly locks in place.
1. Insert the pins of the flange removal tool, 11. Repeat the process if necessary for the sec-
Figure 4.4-2, into the corresponding holes of ond window.
the window flange assembly.
2. Rotate the tool approximately ¼ turn The windows now must be rotated to their maxi-
mum throughput position. To determine maxi-
mum signal throughput:

1. Remove the flow cell assembly. Push the


lever on the floor of the compartment away
Flange from you and lift out the assembly.
Removal 2. Open the OPUS software by double click-
Tool ing on its icon. When the software opens, the
OPUS Login screen appears and a password
must be entered. The User ID is “Default” and
the Password is “OPUS” (all capital letters, no
quotation marks). Click on “Login” to start
Figure 4.4-2, Flange Removal Tool the software.

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74  |  Chapter 4 User Maintenence

3. On the OPUS default screen select “Mea- To replace a fuse:


sure” and from the drop-down menu select 1. Switch OFF the Spectro-FTIR by turning
“Advanced Measurment”, Figure 4.3-2. the main power switch to the “O” position and
4. The “Measurement options” screen ap- unplug the power cord.
pears, Figure 4.3-3. Select the “Check Signal” 2. Open the fuse block by inserting a small
tab. flat-ended screwdriver into the groove and
5. The Check Signal screen becomes active, gently prying out the fuse block. Turn the fuse
Figure 4.3-4. The signal throughput at the block downwards.
current lens position will be displayed. 3. The fuse block contains two fuses. Replace
6. Note the amplitude for this window posi- both fuses with 5x20 mm fuses
tion. with a rated current of 4A, slow blow (accord-
7. Using the flange removal tool, loosen the ing to IEC 60 127-2).
lens, rotate it 90 degrees clockwise and reinstall 4. Close the fuse block by turning the block
it again. upwards and pressing it against the housing
8. Note the amplitude for this window posi- until the spring clip engages.
tion. 5. Reconnect the power cord to the Spectro-
9. Repeat steps 7 and 8 for the remaining two FTIR.
positions for this window. 6. Switch ON the Spectro-FTIR.
10. Review the amplitude for the four positions
and place the lens into the position with the 4.6 FILTER REPLACEMENT AND
maximum signal throughput (amplitude). CLEANING
11. If both windows were replaced, repeat steps
6 through 10 for the other window. In manual and automatic operation of the Spec-
12. Reinstall the flow cell assembly. This com- tro-FTIR, the oil sample flows through a 100µm
plete the window replacement procedure. filter before it enters the flow cell. This filter
keeps large particles from entering the system and
4.5 REPLACING FUSES clogging the flow cell. If heavily contaminated
samples have been run on the unit, the filter and
If the voltage status LEDs at the spectrometer rear its gasket should be removed and cleaned thor-
side do not light when the Spectro-FTIR is ON, oughly with solvent to remove particles that are
a blown fuse of the spectrometer main power sup- obstructing the filter mesh. This section describes
ply can be the cause. The fuse block is the filter replacement procedure for both the
at the spectrometer rear side, below the main manual and the automatic configurations of the
power switch, Figure 4.5-1. Spectro-FTIR .

Manual Configurations
In manual configurations of the Spectro-FTIR,
the filter is on the top of the sipper tube assembly.
To clean or replace the filter disconnect the tubing
at the peristaltic pump to keep it from twisting.
Hold the sipper tube assembly with one hand and
twist the knurled knob on top of the assembly in
a counter clockwise direction, Figure 4.6-1. Re-
move the filter with tweezers or needle nose pli-
ers, Figure 4.6-2. The filter can be cleaned and
Fuse Block
reused unless it is completely clogged with sludge
Figure 4.5-1, Rear View, Locaton of Fuses
and wax, or if there is visual physical damage to

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Spectro-FTIR User Operation & Maintenance Manual  |  75

tighten the knurled knob to the sipper assembly


until slight resistance is felt due to the seal created
by a grommet. Continue to hand-tighten past the
grommet for one or two turns until the knurled
knob is completely seated in the assembly.

Automatic Configurations
In automatic configurations of the Spectro-FTIR
the filter is in line with the flow cell and the Au-
toSampler sipper tube, Figure 4.. To clean or re-
place the filter, remove the tubing from each end.
Unscrew the two sections of the filter holder. Re-
move the filter with tweezers or needle nose pli-
ers. The filter can be cleaned and reused unless it
is completely clogged with sludge and wax, or if
there is visual physical damage to it. The filter can
be cleaned with kerosene. For stubborn depos-
its on the filter, put the filter in a container with
kerosene. Then put the container in the ultra-
sonic bath for a few minutes, this will probably
break loose any deposits. Install a cleaned or re-
placement filter in reverse order of the procedure
Figure 4.6-1, Gaining Access to the Sipper Tube
described above.
Filter

In-Line Filter

Figure 4.6-2, Remove/Install Filter Figure 4.6-3, Automatic Configuration Filter


it. The filter can be cleaned with kerosene. For
stubborn deposits on the filter, put the filter in a
container with kerosene. Then put the container
in the ultra-sonic bath for a few minutes, this will
probably break loose any deposits.

Install a cleaned or replacement filter in reverse


order of the procedure described above. Hand-

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76  |  Chapter 4 User Maintenence

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1 May, 2009 / v.1.2

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