L1050222 - In-Service Lubricants Analyzer User's Guide (001-049)

MOLECULAR SPECTROSCOPY
IN-SERVICE LUBRICANTS
FT-IR ANALYSIS PACK
User’s Guide
Release History
Part Number Release Publication Date
L1050222 D May 2013
Any comments about the documentation for this product should be addressed to:
User Assistance
PerkinElmer Ltd
Chalfont Road
Seer Green
Beaconsfield
BUCKS
HP9 2FX
United Kingdom
Or emailed to: info@perkinelmer.com
Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no
warranty of any kind with regard to this document, including, but not limited to, the
implied warranties of merchantability and fitness for a particular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in
connection with furnishing, performance or use of this material.
Copyright Information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this publication may be reproduced in any form whatsoever or
translated into any language without the prior, written permission of PerkinElmer, Inc.
Copyright © 2013 PerkinElmer, Inc.
Produced in the UK.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically marked as such,
are protected by law.
PerkinElmer is a registered trademark of PerkinElmer, Inc.

Spectrum Touch, Touch Apps, Spectrum, Spectrum Two, Frontier IR, Spectrum 400 and Spectrum 100
are trademarks of PerkinElmer, Inc.
Table of Contents
Introduction ............................................................................................... 5
About the In-Service Lubricants FT-IR Analysis Pack ........................................... 6
Conventions ...................................................................................................... 7
Conventions Used in this Manual ................................................................. 7
Notes, Warnings and Cautions ..................................................................... 7
Introduction to In-Service Lubricant Analysis by Infrared Spectroscopy ...............10
Infrared Absorption ...................................................................................10
Degradation Products ................................................................................11
Additive Depletion .....................................................................................11
Common Contaminants ..............................................................................12
Standard Methods for Lubricants Analysis by FT-IR ......................................13
References ................................................................................................14
Supplied Apps ..................................................................................................15
Warnings and Safety Information ........................................................... 17
Spectrometer Safety Summary ..........................................................................18
Use of Flammable Solvents and Samples ...........................................................19
Heptane ....................................................................................................20
Material Safety Data Sheets ..............................................................................21
Installing the In-Service Lubricants FT-IR Analysis Pack ....................... 23
Overview .........................................................................................................24
Unpacking the Kit .............................................................................................26
AVI Calibration .................................................................................................27
Installing the Flow Cell .....................................................................................30
Performing the Empty Flow Cell Check .................................................................32
Calibrating the Flow Cell Pathlength ..................................................................39
Using the In-Service Lubricants Analyzer ............................................... 47
System Validation Checks .................................................................................48
Flow Cell Contamination Check ...................................................................48
Control Samples ........................................................................................56
Instrument Performance Verification ...........................................................56
New Reference ................................................................................................57
Analyzing Samples ...........................................................................................64
Working with the Results ..................................................................................73
Advanced Configuration........................................................................... 75
Overview .........................................................................................................76
Modifying Touch Apps ......................................................................................77
Customizing Prompt Screens .............................................................................79
Setting Background Frequency ...................................................................80
Attaching an SOP.......................................................................................80
Changing Instrument Parameters ......................................................................82
Creating an Instrument Settings File ...........................................................83
Using your Instrument Settings File in the Touch App ..................................84
Configuring Reporting and Data Export ..............................................................86
Reports .....................................................................................................86
Spectral Export ..........................................................................................87
Results Export ...........................................................................................88
Implementing Alarm Limits ...............................................................................89
Incorporating Quantitative Measurements..........................................................90
Maintenance............................................................................................. 93
Maintenance of the Flow Cell ............................................................................94
Spares, Consumables and Upgrade Options .......................................................98
Spare Parts ...............................................................................................98
Flow Cell Refurbishment.............................................................................98
Index ..............................................................................................................99
Introduction
6 . In-Service Lubricants FT-IR Analysis Pack User's Guide
About the In-Service Lubricants FT-IR Analysis

Pack
The In-Service Lubricants FT-IR Analysis Pack (L1608009) is designed for use with Spectrum Two
spectrometers using Spectrum software and Spectrum Touch™ software. It can also be used
with Frontier IR, Spectrum 400 Series and Spectrum 100 Series spectrometers. The pack
contains everything you need to use your spectrometer for in-service lubricant condition
monitoring.
Figure 1 In-Service Lubricants FT-IR Analysis Pack

Introduction . 7
Conventions
Conventions Used in this Manual
Normal text is used to provide information and instructions.
Bold text refers to text that is displayed on the screen.
UPPERCASE text refers to keys on the PC keyboard. ‘+’ is used to show that you have to
press two keys at the same time, for example, ALT+F.
All eight-digit numbers are PerkinElmer part numbers unless stated otherwise.
Notes, Warnings and Cautions

Three terms, in the following standard formats, are also used to highlight special
circumstances and warnings.
NOTE: A note indicates additional, significant information that is provided with some
procedures.
We use the term WARNING to inform you about situations that could result
in personal injury to yourself or other persons. Details about these
circumstances are in a box like this one.
WARNING
Warning (Warnung)
Bedeutet, daß es bei Nichtbeachten der genannten Anweisung zu einer
Verletzung des Benutzers kommen kann.
Warning (Advarsel)
Betyder, at brugeren kan blive kvæstet, hvis anvisningen ikke overholdes.
Warning (Peligro)
Utilizamos el término WARNING (PELIGRO) para informarle sobre
situaciones que pueden provocar daños personales a usted o a otras
personas. En los recuadros como éste se proporciona información sobre este
tipo de circunstancias.
Warning (Danger)
Nous utilisons la formule WARNING (DANGER) pour avertir des situations
pouvant occasionner des dommages corporels à l'utilisateur ou à d'autres
personnes. Les détails sur ces circonstances sont données dans un encadré
semblable à celui-ci.
Warning (Pericolo)
Con il termine WARNING (PERICOLO) vengono segnalate situazioni che
potrebbero provocare incidenti alle persone. Troverete informazioni su tali
circostanze in un riquadro come questo.
Warning (Waarschuwing)
Betekent dat, wanneer de genoemde aanwijzing niet in acht wordt genomen,
dit kan leiden tot verwondingen van de gebruiker.
Warning (Aviso)
Significa que a não observância da instrução referida poderá causar um
ferimento ao usuário.
Warning (警告)
我们使用“警告”这一术语来通知您有关可能会对您自己或他人造成人
身伤害的情况。
有关这些情况的详细信息可在此类方框中找到。
Introduction . 9
We use the term CAUTION to inform you about situations that could
CAUTION result in serious damage to the instrument or other equipment. Details
about these circumstances are in a box like this one.
Caution (Achtung)
Bedeutet, daß die genannte Anleitung genau befolgt werden muß, um
einen Geräteschaden zu vermeiden.
Caution (Bemærk)
Dette betyder, at den nævnte vejledning skal overholdes nøje for at
undgå en beskadigelse af apparatet.
Caution (Advertencia)
Utilizamos el término CAUTION (ADVERTENCIA) para advertir sobre
situaciones que pueden provocar averías graves en este equipo o en
otros. En los recuadros como éste se proporciona información sobre
este tipo de circunstancias.
Caution (Attention)
Nous utilisons le terme CAUTION (ATTENTION) pour signaler les
situations susceptibles de provoquer de graves détériorations de
l'instrument ou d'autre matériel. Les détails sur ces circonstances
figurent dans un encadré semblable à celui-ci.
Caution (Attenzione)
Con il termine CAUTION (ATTENZIONE) vengono segnalate situazioni
che potrebbero arrecare gravi danni allo strumento o ad altra
apparecchiatura. Troverete informazioni su tali circostanze in un
riquadro come questo.
Caution (Opgelet)
Betekent dat de genoemde handleiding nauwkeurig moet worden
opgevolgd, om beschadiging van het instrument te voorkomen.
Caution (Atenção)
Significa que a instrução referida tem de ser respeitada para evitar a
danificação do aparelho.
Caution (小心)
我们使用“小心”这一术语来通知您有关可能会对本仪器或其它
设备造成严重损害的情况。
有关这些情况的详细信息可在此类方框中找到。
Introduction to In-Service Lubricant Analysis

by Infrared Spectroscopy
The In-Service Lubricants FT-IR Analysis Pack provides the tools necessary to use Fourier
transform infrared (FT-IR) spectroscopy to monitor additive depletion, contaminant build-up
and base-stock degradation of in-service lubricants and hydraulic fluids.
Infrared Absorption
The chemical bonds within organic molecules are in a state of continual vibration, with bonds
stretching and contracting as well as bending relative to each other. When an infrared beam
falls on a molecule, waves of specific frequencies are absorbed from the beam by the
molecule. The actual frequencies absorbed depend on the types of bonds present in the
molecular structure. Chemical bonds within a molecule are said to exhibit “characteristic
infrared absorptions”.
A record of the frequencies at which absorption takes place for an organic compound is
called its infrared spectrum. An infrared spectrum of a compound will reveal information
about its molecular structure, as the existence of specific groups of atoms may be confirmed
from the presence of their characteristic absorptions. The spectrum of a mixture of
compounds contains contributions from all of the compounds.
As a lubricant wears, its composition changes as additives are depleted and contaminants
and breakdown products accumulate. As each of these compounds has a distinct infrared
spectrum, the spectrum of the lubricant will change and these changes can be used to assess
the condition of the lubricant.
An example of the changes seen as a lubricant wears is shown in Figure 2.
1.5
1.4
1.3 Phosphate
1.2 Nitration antiwear
1.1
1.0 Oxidation
0.9 Water
A
0.8
0.7 Soot
0.6
0.5 Used oil
0.4
0.3
0.2 New oil
0.1
4000 3500 3000 2500 2000 1500 1000 550
cm-1
Figure 2 Spectra of unused and used diesel engine oil
Introduction . 11
Degradation Products
Oxidation
Oil exposed to oxygen at elevated temperature will oxidize to a variety of compounds, the
majority of which are carbonyl compounds, including carboxylic acids. Carboxylic acids
contribute to the acidity of the oil, depleting the basic additives present and contributing to
corrosion. Oxidation can also increase the viscosity of the oil. The degree of oxidation is a
good indicator of oil degradation. A rapid increase in oxidation may indicate an engine
overheating or a depletion of the anti-oxidant additive due to an over-extended oil change
period.
Oxidative degradation also occurs with petroleum gear and hydraulic fluids.
Nitration
Nitrogen oxides, produced from the oxidation of atmospheric nitrogen during the combustion
process, react with the oil. Nitration increases the viscosity of the oil and is the major cause
of the build-up of varnish or lacquer.
A high nitration value, also known as NOx or nitro-oxidation, indicates an incorrect fuel/air
ratio, incorrect spark timing, excessive loads, low operating temperature or piston-ring
blow-by.
Sulfate
Sulfur oxides are produced by the combustion of sulfur compounds present in the fuel. These
oxides react with water, also produced by the combustion process, to form sulfuric acid. The
sulfuric acid is neutralized by the oil’s basic additives, forming inorganic sulfates. A rapid
increase in the sulfate value may indicate the use of a high sulfur content fuel, poor
combustion, over-cooling or the rapid depletion of anti-wear additive.
Ester breakdown
Synthetic lubrication oils usually contain a high proportion of synthetic polyol esters. These
esters are susceptible to breakdown in the presence of water and acids (hydrolysis). Ester
breakdown contributes to the acidity of the oil and can result in the formation of crystals of
the base polyol, leading to clogging of filters. Ester breakdown may indicate the presence of
water from condensation caused by low operation temperatures or from a coolant leak.
Additive Depletion
Numerous compounds are added to oils to confer desirable properties. These additives can
be depleted during use, and so monitoring this depletion can provide a warning of impending
lubricant failure.
Anti-wear
Anti-wear additives, such as di-alkyl or di-aryl dithiophosphates (ZDDPs) prevent direct

metal-to-metal contact by forming a coating on metal surfaces activated by frictional heat.
These can be depleted by hydrolysis or oxidation, resulting in increased wear rates. A rapid
loss of anti-wear additive may indicate excess loads or contamination by water from a
coolant leak.
Antioxidant
Phenolic antioxidant compounds are often used in turbine lubricants. Depletion of antioxidant
is followed by a rapid increase in the rate of oxidation.
Common Contaminants
Soot
Soot particles result from the incomplete combustion of fuel and, since they are too small to
be removed by the filter, remain suspended in the oil. Soot builds up continuously until it
reaches an unacceptable level; that level depends on the type of engine and lubricant. Diesel
oils tolerate higher soot levels than gasoline oils. The rate of soot build-up depends on
engine design, type of fuel and operating conditions. A high soot value may indicate poor
combustion due to an incorrect fuel/air ratio, a clogged air filter or an over-extended oil
change period.
Water and glycol
The presence of water and glycol in crankcase oil indicate a leak from the cooling system. It
is essential to detect such a problem early to avoid a serious failure. The presence of water
alone does not necessarily indicate a coolant problem, but may result from condensation due
to a low operating temperature.
Water contamination can also occur in hydraulic systems through leakage or condensation in
reservoirs.
Unburned fuel
The presence of fuel in the oil indicates poor combustion due to an incorrect fuel/air ratio, a
clogged air filter or an ignition problem. It may also indicate an over-extended oil change
period.
NOTE: The fuel measurement depends not only on the level of contamination, but also on
the aromatic hydrocarbon content of the fuel. The aromatic content of fuels varies
with location and season, so it may be appropriate to perform a calibration with the
fuel being used.
Introduction . 13
Standard Methods for Lubricants Analysis by FT-IR

Spectral-subtraction and direct-trending methods
Because of the wide variety of lubricating oils available, it is essential to consider the oil type
when interpreting the spectrum. The changes due to wear may be quite subtle compared to
the differences between different oils. One approach to this problem is to measure the
spectrum of the unused oil (if this is available) and subtract this from the used oil. Figure 3
shows the example data of Figure 2 in this differential form. The heights of the peaks due to
breakdown products, contaminants and additive depletion can be measured.
0.7
0.6 Phosphate
Nitration antiwear
0.5
0.4
Oxidation
Water
Phenolic
A
0.3 Soot
antiwear
0.2
0.1
0.0
-0.1
4000 3500 3000 2500 2000 1500 1000 550
cm-1
Figure 3 Used-oil spectrum after unused-oil spectrum subtraction
The spectral-subtraction method works very well if the unused oil is available, but this is
often not the case, and using an incorrect reference spectrum can give misleading results.
Additionally, if the machinery has been topped up with a different oil, an appropriate
reference spectrum may not be available.
The alternative approach is to measure the peak heights directly in the used-oil spectrum. In
this case, the baseline (unused-oil) values for the measured parameters will depend on the
oil type, and the results should be trended through several measurements over the lifetime
of the oil or compared to alarm limits derived from statistical analysis of data for the
appropriate machine and lubricant type.
Standard practices and test methods
ASTM International publishes several documents discussing lubricants analysis by FT-IR,

including both direct-trending and spectral-subtraction methods. This Analysis Pack supports
all ASTM methods current at time of release1–4; a complete list is given in Supplied Apps on
page 15.
A collection of direct-trending FT-IR oil analysis methods for several oil types was developed
as part of the US Army, Navy and Air Force Joint Oil Analysis Program (JOAP). These
methods are widely used and are supported by the Analysis Pack; a complete list is given in
Supplied Apps on page 15.
Alarm limits
As the methods described above involve trends in absorbance values rather than direct
quantitative measurements, alarm limits should be derived from statistical analysis of oil
analysis and failure data from many machines. These limits are dependent on machinery
type and oil formulation, and a full discussion is beyond the scope of this guide. For more
information, refer to ASTM E2412-101.
Quantitative calibrations and additional analytes
It is possible to develop quantitative calibrations for certain analytes, although their validity
may be limited to the type of oil used to develop the calibration. As an example, soot may be
determined directly as a percentage of the oil mass. In some cases, particularly for marine
oils with high concentrations of basic additives, it is possible to measure total base number
(TBN), provided an appropriate calibration is developed5. If the appropriate software package
is purchased (see Spares, Consumables and Upgrade Options on page 98) and calibrations
developed, your Analyzer can be configured to perform these analyses.
References
1. ASTM E2412-10 “Standard Practice for Condition Monitoring of Used Lubricants by
Trend Analysis Using Fourier Transform Infrared (FT-IR) Spectrometry”, ASTM
International, 2010. http://www.astm.org/Standards/E2412.htm
2. ASTM D7412-09 “Standard Test Method for Condition Monitoring of Phosphate Antiwear
Additives in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis
Using Fourier Transform Infrared (FT-IR) Spectrometry”, ASTM International, 2009.
http://www.astm.org/Standards/D7412.htm
3. ASTM D7414-09 “Standard Test Method for Condition Monitoring of Oxidation in In-
Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using Fourier
Transform Infrared (FT-IR) Spectrometry”, ASTM International, 2009.
4. ASTM D7415-09 “Standard Test Method for Condition Monitoring of Sulfate By-Products
in In-Service Petroleum and Hydrocarbon Based Lubricants by Trend Analysis Using
Fourier Transform Infrared (FT-IR) Spectrometry”, ASTM International, 2009.
5. David Wooton, Stuart Barry, Samuel White and Robert Thomas, “Using Infrared
Spectroscopy in Used Engine Oils: Estimating Base Number”, Practicing Oil Analysis,
November–December 2005.
6. ASTM D7418-07 “Standard Practice for Set-UP and Operation of Fourier Transform
infrared (FT-IR) Spectrometers for In-Service Oil Condition Monitoring”, ASTM
International, 2007. http://www.astm.org/Standards/D7418.htm
Introduction . 15
Supplied Apps
The In-Service Lubricants FT-IR Touch Apps Software Kit (LX108938) supplied in the pack
provides the following in-service lubricants Touch Apps.
Table 1 Touch Apps Supplied with the In-Service Lubricants FT-IR Analysis Pack
Touch App Type Summary
Lubricants ASTM E2412: Spectral- See ASTM E2412–101.

Petroleum Crankcase subtraction
Lubricants ASTM E2412: Direct- See ASTM E2412–101. These methods are also
Petroleum EP trending compatible with the analyses specified by Standard
Test Methods D7412, D7414, and D7415.
Lubricants ASTM E2412: Direct-
Petroleum Lubricant trending
Lubricants ASTM E2412: Direct-

Polyol Ester trending
Lubricants JOAP: Direct- The JOAP Apps provide the analyses specified by the
Run All Tests trending US Army, Navy and Air Force Joint Oil Analysis
Petroleum Ground Program.
Petroleum Hydraulic Run All Tests calculates parameters for all oil types;
Synthetic Ground
the other Apps are sub-sets of these calculations
Synthetic Turbine appropriate for specific oil types.
Synthetic Hydraulic
Lubricants Other: Other Estimates the aromatic, napthenic and paraffinic

Brandes fractions of a mineral oil.
See UK Ministry of Defence, Defence Standard
05-50, Methods for Testing Fuels, Lubricants and
Associated Products, Part 65: Determination of
Hydrocarbon Types in Mineral Oils by Infrared
Spectroscopy, 14 July 1995.
Lubricants Other: Direct- Contains additional calculations for turbine fluids,

Turbine Fluids trending including: phenolic antioxidant, oxidation, and
unsaturated esters.
Lubricants Other: Direct- Measures analytes relevant to synthetic turbine

Turbine Synthetic trending lubricants, including: water, ester breakdown, oxidation,
and antiwear depletion.
Lubricants Tools: Other Checks the fringe-suppression performance of the

Empty Flow Cell Check flow cell and collects a corrected empty-cell spectrum
for use with direct-trending methods.
Lubricants Tools: Other Checks for the presence of contamination build-up on

Flow Cell Contamination the flow cell windows.
Check
Lubricants Tools: Other Collects a reference oil spectrum for use with
New Reference spectral-subtraction methods.
Warnings and Safety
Information
Spectrometer Safety Summary

For safety information concerning your spectrometer, refer to the Warning and Safety
Information section of the User’s Guide supplied with your instrument.
Warnings and Safety Information . 19
Use of Flammable Solvents and Samples
Flammable solvents or samples should not be stored on or near the

instrument. Handling of such materials during preparation should be
performed in a safe area away from the instrument such as a fume
cabinet.
WARNING
Do not operate the instrument with the sample compartment lid closed to
prevent build-up of flammable vapor.
WARNING
Some chemicals used with this instrument may be hazardous or may

become hazardous after completion of an analysis. The responsible body
(for example, the Laboratory Manager) must take the necessary
precautions to make sure that the surrounding workplace is safe and that
WARNING
the instrument operators are not exposed to hazardous levels of toxic
substances (chemical or biological) as defined in the applicable MSDS
(Material Safety Data Sheets) or OSHA (Occupational Safety and Health
Administration [United States]), ACGIH (American Conference of
Governmental Industrial Hygienists [United States]), or COSHH (Control
Of Substances Hazardous to Health [United Kingdom]) documents.
Venting for fumes and disposal of waste must be in accordance with all
national, state and local health and safety regulations and laws.
We recommend that you use heptane as the rinse solvent. This highly
flammable solvent presents no hazard during routine use, but:
• DO clean up leakages and spillages immediately and thoroughly.

WARNING
• DO always keep the lid on the solvent bottle and waste bottle.
Heptane
Safety information for heptane is summarized below. See the Materials Safety Data Sheet
(MSDS) for heptane, supplied by your local Safety Officer, for full details.
Physical data
Description Clear, colorless liquid with a faint gasoline-like odor
Boiling point 98°C
Specific gravity 0.6837
Solubility in water Insoluble
Vapor pressure 40 mmHg at 20°C
Vapor density 3.45
Fire and explosion hazard
Heptane is flammable (USA definition)/highly flammable (European definition)
Flash point −4 °C
Explosive limits 1.05–6.7%
Ignition temperature 223 °C
Firefighting measures Extinguish fire with foam, dry powder, carbon dioxide or
vaporizing liquid
Storage and handling
When storing heptane, observe local and national regulations. Keep containers tightly closed.
When handling heptane, wear safety goggles and protective gloves. Do not breathe the
vapor, and avoid contact with eyes, skin and clothing.
Warnings and Safety Information . 21
Material Safety Data Sheets

You can search for up-to-date copies of safety data sheets on materials, such as ZnSe, used
in PerkinElmer products that are known to have safety issues from the Technical Resources
section of the PerkinElmer website. The MSDS information is available in a range of
languages, and includes data items required in specific national, supra-national and state
jurisdictions.
To obtain a safety data sheet for a particular compound, follow the steps described below.
NOTE: To read MSDS *.pdf files you will need Adobe Reader 5.0 or later. An installation of
this software is available on the Software Utilities CD.
1. Launch your web browser and navigate to the PerkinElmer web site:
www.perkinelmer.com
If you are not redirected automatically you may have to select the home page
appropriate to your location.
2. Search for the term MSDS using the search box located at the top of the home page.
The Search for Material Safety Data Sheets (MSDS) page is displayed.
3. Enter the key words for the compound, in the Product name box, and then click Go.
A full list of all MSDS documents that refer to the compound is displayed.
4. Select the MSDS document you want to view.

Installing the In-Service
Lubricants FT-IR Analysis
Pack
Overview
This chapter details the steps that must be taken to install your analysis pack and verify that
it is operating correctly.
1. Install your application pack software from the In-Service Lubricants FT-IR Touch Apps
Software DVD (LX100934) as described in Installing your Touch App (L1050270).
2. If this kit was purchased with a spectrometer, install your spectrometer following the
instructions provided in the User’s Guide for your instrument.
3. Log in to Spectrum software.

Enter your User name and Password, if required, and then click OK.
The default user name and password are Administrator and administrator, respectively.
4. Ensure that your instrument is included in the list of available instruments.

Choose Select Instrument from the Setup menu to display the Instrument Connection
dialog, and then check the drop-down list of instruments.
If you did not add your instrument to those available in Spectrum software as part of
installing your instrument in Step 2, refer to the Spectrum Administrator’s Guide
(L1050095) for more information.
If the application pack installation updated your existing Spectrum software version, any
existing instruments will still be available.
5. Select your instrument from the list on the Instrument Connection dialog and then click
Connect.
6. When you have confirmed that you can connect to your instrument, exit Spectrum
software.
NOTE: You can log in and connect to your instrument using only one application at a time.
You must exit Spectrum before using Spectrum Touch, and vice versa.
7. Ensure that you have all the necessary items listed in Unpacking the Kit on page 26.
8. Perform the AVI Calibration as described in AVI Calibration on page 27.
9. Set up the flow cell, waste bottle and tubing as described in Installing the Flow Cell on
page 30.
10. Run the Empty Flow Cell Check App in Spectrum Touch as described in Performing the
Empty Flow Cell Check on page 32.
You can also access an SOP for the Empty Flow Cell Check App from within the Touch
App.
Installing the In-Service Lubricants FT-IR Analysis Pack . 25
11. Calibrate the pathlength of the flow cell using Spectrum software as described in
Calibrating the Flow Cell Pathlength on page 39.
If you are an administrator setting up the application for multiple users, then you will need to
set up new users in Spectrum. Refer to Setting up Users, Groups and Passwords in the
Spectrum on-screen Help.
Unpacking the Kit

The pack includes the following items:
Part Number Description Quantity
LX108938 In-Service Lubricants FT-IR Touch App™ Software Kit 1
L1272309 Used-Oil Flow Cell (with ZnSe windows) 1
L1608117 IR Flow Cell Waste Tubing with Luer Fitting 1
L1608118 Plastic Syringe 3 mL Luer Lock (pack of 100) 1
04821008 PTFE Stopper – Luer Fitting (pack of 6) 1
L9003631 Torque Driver (24 cNm) 1
L9003632 Hexagonal Bit (3.0 mm) 1
If any of these items are missing or damaged, contact your local PerkinElmer Customer Care
Representative.
Additional Materials Required

The In-Service Lubricants FT-IR Analysis Pack includes most items that you need for your
analysis. However, you will require the following additional materials:
• Sample for pathlength determination

We recommend using >99% purity squalane (OilExpress 4 Pathlength Calibration Fluid,
part number N9308377) with the Pathlength - squalane.qmd Quant method.
Alternatively, you can use HPLC- or spectroscopic-grade heptane with the CELLPATH.md
Quant method.
Refer to Calibrating the Flow Cell Pathlength on page 39 for more information.
• Cleaning solvent
Heptane is recommended, but you may use any non-polar solvent suitable for your
application.
Hydrocarbon solvents such as pentane, petroleum ether or kerosene are suitable
cleaning solvents. Mineral diesel fuel is also acceptable, but the use of diesel containing
significant concentrations of fatty acid methyl esters (FAME; biodiesel) is not
recommended as any carry-over may increase the measured oxidation numbers.
• Waste bottle with a drilled cap.

The waste tubing has an outside diameter of 4 mm.
• Lens tissue or cotton buds

AVI Calibration
The Touch Apps supplied for with the In-Service Lubricants FT-IR Analysis Pack are
configured to use an AVI (Absolute Virtual Instrument) calibration. AVI in Spectrum software
is an instrument standardization algorithm used to ensure that equivalent results are
obtained when the same measurement is performed on multiple instruments. It uses a
methane cell inserted in the beam path as the reference material.
NOTE: You can modify the Instrument setup step to not use AVI. Refer to Changing
Instrument Parameters on page 82Error! Bookmark not defined. However, to
obtain the optimum performance from the system, we recommend that you use the
AVI feature.
Before running collecting data using the Spectrum Touch Apps, perform the AVI calibration in
Spectrum software:
1. If you have a Spectrum Two spectrometer, ensure that the 4 cm−1 J-stop card is
inserted in the left-hand side of the slide holder.
Frontier IR, Spectrum 400 Series and Spectrum 100 Series spectrometers have an
automated J-stop, and so no action is required.
2. Start Spectrum Software.

The Spectrum start-up splash-screen is displayed, followed by a dialog that may require
your login details.
3. Enter your User name and Password, if required, and then click OK.
4. Select Standardize from the Measurement menu.
NOTE: You can also access the AVI Calibration Wizard from the Adjustments Toolbox, via
the Setup Instrument Advanced tab.
The AVI Calibration dialog is displayed.
5. Ensure that the beam path is clear, and then click Continue.
The background spectrum is collected.

When the scan is complete, if your instrument does not have a methane cell in the
internal filterwheel, you are prompted to insert the methane cell.
OR
If your instrument does have a methane cell in the automated filterwheel, this will
automatically be inserted in the beam path. Continue at Step 7. Insert the methane cell
in the slide holder.
If you have a Spectrum Two spectrometer, it should be inserted in the right-hand side
of the slide holder.
6. Click Continue.
The spectrum of the methane cell is collected.
7. When the calibration is complete, click OK to exit the dialog.
NOTE: To use the AVI calibration from Spectrum, the AVI option must be selected on the
Setup Instrument Advanced tab. It is already enabled in the supplied Touch Apps.
You can change the instrument settings in your Touch App; refer to Changing
Instrument Parameters on page 82.
Installing the Flow Cell

1. Insert the flow cell into the slide holder in the sample compartment, so that the syringe
ports are facing outwards (Figure 4).
Figure 4 Flow cell installed in the Spectrum Two slide holder
2. Position the waste bottle (not supplied) on a level surface at, or below, the level of the
spectrometer sample compartment.
We recommend using a bottle with a drilled (not airtight) cap to reduce the evaporation
of volatile solvent waste.
NOTE: Do not place the waste bottle where it is likely to be knocked over.
3. Insert the Luer fitting on the supplied flexible waste tubing into the upper syringe port
on the flow cell (Figure 5).
Figure 5 Attaching tubing to the upper syringe port

4. Insert the other end of the tubing into the waste bottle, ensuring that the end of the
tubing is lower than the lower port of the flow cell (Figure 6).
If the tubing is too long, cut it to length.
Figure 6 Flow cell connected to waste bottle

Performing the Empty Flow Cell Check

The Empty Flow Cell Check App checks the performance of the flow cell and stores a
reference spectrum of the empty cell. The cell must be absolutely clean and dry before
proceeding. It is recommended, therefore, that you perform this check only at installation
using a new cell, or after the cell has been dismantled for cleaning and then reassembled.
Refer to Maintenance of the Flow Cell on page 94.
When using direct-trending oil analysis methods, the spectrum of the empty cell measured
by the Touch App will be automatically subtracted from the sample spectrum. This gives
more accurate results and improves reproducibility between systems.
NOTE: Always use the supplied Touch App to measure the empty cell spectrum. Some
processing is carried out after measurement of the spectrum to account for the
difference in refractive index between air and oil.
NOTE: You can also access this SOP for the Empty Flow Cell Check App from within the Touch
App.
Before running the Empty Flow Cell Check Touch App, you should:
• Ensure that the 4 cm−1 J-stop card is inserted in the left-hand side of the Spectrum Two
spectrometer slide holder.
automated J-stop and do not require a card to be fitted.
• Perform an AVI calibration.

You only need to do this once at installation and then after instrument maintenance (for
example, source replacement). Refer to AVI Calibration on page 27.
To run the Touch App:
1. From the Start menu select All Programs; the PerkinElmer Applications group; the
Spectrum Touch sub-group and then the Spectrum Touch application.
The Spectrum Touch Log-in screen is displayed.
2. Press the appropriate user icon , and then enter your password.
The Main Menu screen is displayed.
3. Press Empty Flow Cell Check in the Lubricants Tools group.

The Empty Flow Cell Check screen is displayed.
4. When you are ready to continue, press Next .

The Sample Information screen is displayed.
Do not alter the Sample ID.

CAUTION
5. Press Next .
The Background Measurement screen is displayed.
6. Remove the cell from the sample slide and lay it on the bench.
Take care that the end of the waste tubing remains inside the waste container.
7. Ensure that the beam path is clear.
8. Press Next to measure the background spectrum.

When the background measurement is complete, the Sample Measurement screen is

displayed.
9.
Place the flow cell on the slide holder.
10. Press Next to scan the empty cell spectrum.

When the scan is complete, the result is displayed.

If the check passed, the Empty Flow Cell Fringe Check Passed screen is displayed.
OR
If the check failed, the appropriate Empty Flow Cell Fringe Check Failed screen is
displayed.
The screen lists potential causes for the failure, together with suggestions for repeating
the check. In the following example, the check has failed because the baseline level is
lower than expected:
11. Click Next .

The Detailed Results screen is displayed, which shows the calculated flow cell
interference Fringe Amplitude and the Baseline Level.
To view the spectrum, select Graph from the drop-down list.

Spectrum Touch automatically performs Quality Checks to test for common sampling
problems.
A summary of the results of the Quality Checks is shown above the results list. This
icon is amber if a problem has been identified that you may want to investigate to
improve the quality of the spectra you are collecting. It is red if a serious problem has
been identified that you should attempt to cure before collecting further spectra.
To view the results of each test, select Quality Checks from the drop-down list.
For more information on Quality Checks, refer to the Spectrum Touch on-screen Help
To print the current screen, press Print .
12. If the Empty Flow Cell Check passed, press Next to exit the Touch App and return
to the Main Menu.
The corrected empty-cell spectrum is saved to the reference spectra folder, which is
usually C:\pel_data\spectra\Lubricants Reference
OR
If Empty Flow Cell Check failed, press Next to exit the Touch App and return to
the Main Menu. Ensure that the cell is clean and dry, and then repeat the test. If it fails
a second time, contact your local PerkinElmer Customer Care Representative and
arrange to have the flow cell refurbished.
Calibrating the Flow Cell Pathlength

The Analyzer uses a flow cell with a nominal pathlength of 0.1 mm, but the real value of the
pathlength may vary between 0.09 and 0.125 mm. Before using the analyzer for the first
time, and after any maintenance of the flow cell, it is important to measure the precise
pathlength. The pathlength will be saved in the header of each collected spectrum and used
by the Touch App to normalize calculated properties.
The pathlength is determined by comparing the spectrum of a calibration sample with a

supplied reference model. This process is assisted by the Setup Pathlength tool in Spectrum
software.
The pathlength calculated is saved for the current user. If you are a member of the Group
“Administrators” in Spectrum software, then you will be able to share your flow cell
pathlength with all other Spectrum users using the Share Pathlength Utility. See Sharing your
pathlength with other users on page 46.
Two Quant methods for the determination of the flow cell pathlength are supplied with your
system: Pathlength - squalane.qmd and CELLPATH.md. The Pathlength - squalane.qmd
requires >99% squalane (OilExpress 4 Pathlength Calibration Fluid, part number N9308377).
The CELLPATH.md requires high-purity n-heptane.
NOTE: Determine the pathlength before running any samples. It is vital that the cell be
absolutely clean and dry before proceeding.
1. Start Spectrum Software.

The Spectrum start-up splash-screen is displayed, followed by a dialog that may require
your login details.
2. Enter your User name and Password, if required, and then click OK.
3. Select Instrument from the Setup menu.

The Setup Instrument tabs are displayed.
4. Select the Setup Instrument Basic tab.

5. Configure the instrument as follows, leaving all other settings at their default values.
Parameter Squalane Heptane sample

sample
Start 4000 cm−1 4000 cm−1
End 550 cm−1 550 cm−1
Resolution 4 cm−1 8 cm−1
Accumulations 4 scans 8 scans
6. Ensure that the sample compartment is empty, and then click on the
Measurement toolbar to collect a background spectrum.
7. Place the flow cell in the slide mount in the sample compartment.
8. Ensure that the waste tubing is connected to the flow cell and draining into the waste
container.
9. Fill one of the supplied 3 mL Luer lock syringes with approximately 3 mL of calibration
sample.
10. Hold the syringe pointing upwards and away from you and very carefully depress the
plunger slightly to remove any air bubble in the tip.
11. Attach the syringe to the lower port of the flow cell and then gently, but firmly, depress
the plunger to push approximately 2 mL of the calibration sample through the cell.
Move the plunger at about 0.5 mL per second. Ensure that there are no leaks or air
bubbles.
Leave the syringe in place during the scan.
12. Enter a suitable Sample ID in the Measurement toolbar.
13. Click on the Measurement toolbar to scan the spectrum.

The spectrum will be scanned and then displayed in the Samples View.
14. Remove the syringe from the flow cell.
15. If the sample does not drain into the waste container, fill the syringe with air, reattach it
to the cell and gently force the sample out of the cell.
16. Select Pathlength from the Setup menu.

The Setup Pathlength tab is displayed.
17. Select Enable Pathlength.

18. Ensure that Determine using Quant method is selected under Pathlength
Determination.
19. Select the appropriate Quant Type for the method you are using.
Select Beer’s Law for Pathlength – squalane.qmd. Select Quant+ for CELLPATH.md.
20. Click the Browse button, and then navigate to and select the Quant method.
The Pathlength - squalane.qmd is installed to the folder C:\pel_data\quant\methods and
the CELLPATH.MD method is installed to the folder C:\quant\pls1\METHODS.
21. Click OK.

The Component drop-down will update to display Pathlength (mm).
22. Ensure that your pathlength calibration sample spectrum is selected in the Data
Explorer at the top-left of the Spectrum window.
23. Click Calculate on the Setup Pathlength tab to determine the pathlength.
The calculation is performed, and the results are displayed in the Quant Analysis Details
dialog.
24. Compare the results with the criteria shown in Table 2 below.
Table 2 Acceptance criteria for pathlength results
Property or Component Allowable Range
Pathlength 0.09–0.125
Pathlength M Distance <3

(CELLPATH.MD only)
Pathlength Residual Ratio <20

(CELLPATH.MD only)
25. If your results are within the acceptance criteria, click OK to apply the pathlength.
The new pathlength value is displayed on the Setup Pathlength tab. It will be saved in
the header of all spectra collected using Spectrum or Spectrum Touch software,
provided that Enable Pathlength is selected. The pathlength value will be displayed
automatically in the Sample Information for samples collected using the Touch Apps.
OR
If the results are not within the acceptance criteria, or you do not want to apply the
changes, click Cancel.
Troubleshooting
If the pathlength check fails, refer to the following:
• Ensure that the correct calibration sample was used, and the sample is not
contaminated.
• Check that the flow cell is clean.
• Check that the correct instrument settings were used to collect the calibration sample.
• If using the CELLPATH.MD method, a residual ratio over 20 usually indicates that the
heptane used was of insufficient purity, or that the flow cell shows excessive
interference fringing.
• If heptane of at least 99 % purity was used, and the flow cell passed the fringe check
described in Performing the Empty Flow Cell Check on page 32, flush the cell with
10 mL heptane and repeat the test.
• If using the CELLPATH.MD method and the residual ratio is consistently over 20, contact
your local PerkinElmer Customer Care representative and arrange to have the flow cell
refurbished.
• If the measured pathlength is consistently less than 0.09 mm or greater than

0.125 mm, contact your local PerkinElmer Customer Care representative and arrange to
have the flow cell refurbished.
• If sufficiently high-purity squalane or heptane is not available, refer to the method

described in Appendix X2.2 of ASTM D7418-076.
Sharing your pathlength with other users
You may want to share the pathlength value you calculated with other Spectrum users. You
can do this using the Share Pathlength Utility. To run the utility you must be a member of
the group “Administrators” in Spectrum software.
The tool will apply the settings to all active Spectrum users. Each user must first log in to
Spectrum once.
To run the tool:
1. Exit Spectrum software.
2. Select All Programs > PerkinElmer Applications > Spectrum > Share Pathlength
Utility from the Windows Start menu.
The Share Pathlength Utility is displayed.
3. If you are certain that you wish to apply the pathlength to all users, click Apply
Pathlength to all Users.
The utility will enter the pathlength value in the Pathlength (mm) box and check the
Enable Pathlength option on the Setup Pathlength dialog. The pathlength value will be
displayed automatically in the Sample Information for samples collected using the
Touch Apps.
Alternatively, each user can select Enable Pathlength and then Set manually on the Setup
Pathlength tab, and then type in the calculated value into the Pathlength (mm) field.
Using the In-Service
Lubricants Analyzer
System Validation Checks

There are several checks that you can perform to ensure that the Analyzer is functioning
correctly.
Flow Cell Contamination Check

Before running the Touch App:
• Ensure that the 4 cm−1 J-stop card is inserted in the left-hand side of the Spectrum Two
spectrometer slide holder.
automated J-stop and do not require a card to be fitted.
• Perform an AVI calibration.

You only need to do this once at installation and then after instrument maintenance (for
example, source replacement). Refer to AVI Calibration on page 27.
• Determine the pathlength of your cell as described in Calibrating the Flow Cell
Pathlength on page 39.
• Ensure that you have cleaned your cell as described in Step 14 of Analyzing Samples on
page 64.
• Obtain a sample of completely clean and clear solvent or oil having no absorption in any
of the following spectral regions:
– 3500–3250 cm−1
– 2000–1900 cm−1
– 1800–1700 cm−1
HPLC- or spectroscopic-grade n-heptane is recommended.
NOTE: You can also access this SOP for the Flow Cell Contamination Check App from within
the Touch App.
Using the In-Service Lubricants Analyzer . 49
To run the Touch App:
1. From the Start menu select All Programs; the PerkinElmer Applications group; the
Spectrum Touch sub-group and then the Spectrum Touch application.
The Spectrum Touch Log-in screen is displayed.
2. Press the appropriate user icon , and then enter your password.
The Main Menu screen is displayed.

L1050222 - In-Service Lubricants Analyzer User's Guide (001-049)

Încărcat de

Informații document

Titlu original

Drepturi de autor

Formate disponibile

Partajați acest document

Partajați sau inserați document

Opțiuni de partajare

Vi se pare util acest document?

Este necorespunzător acest conținut?

Drepturi de autor:

Formate disponibile

L1050222 - In-Service Lubricants Analyzer User's Guide (001-049)

Încărcat de

Drepturi de autor:

Formate disponibile

MOLECULAR SPECTROSCOPY

Part Number Release Publication Date

L1050222 D May 2013

Or emailed to: info@perkinelmer.com

Copyright © 2013 PerkinElmer, Inc.

Produced in the UK.

PerkinElmer is a registered trademark of PerkinElmer, Inc.

About the In-Service Lubricants FT-IR Analysis

Figure 1 In-Service Lubricants FT-IR Analysis Pack

Bold text refers to text that is displayed on the screen.

Notes, Warnings and Cautions

Introduction to In-Service Lubricant Analysis

An example of the changes seen as a lubricant wears is shown in Figure 2.

Anti-wear additives, such as di-alkyl or di-aryl dithiophosphates (ZDDPs) prevent direct

Water and glycol

Standard Methods for Lubricants Analysis by FT-IR

Standard practices and test methods

ASTM International publishes several documents discussing lubricants analysis by FT-IR,

Quantitative calibrations and additional analytes

Touch App Type Summary

Lubricants ASTM E2412: Spectral- See ASTM E2412–101.

Lubricants ASTM E2412: Direct-

Lubricants Other: Other Estimates the aromatic, napthenic and paraffinic

Lubricants Other: Direct- Contains additional calculations for turbine fluids,

Lubricants Other: Direct- Measures analytes relevant to synthetic turbine

Lubricants Tools: Other Checks the fringe-suppression performance of the

Lubricants Tools: Other Checks for the presence of contamination build-up on

Spectrometer Safety Summary

Use of Flammable Solvents and Samples

Flammable solvents or samples should not be stored on or near the

Some chemicals used with this instrument may be hazardous or may

• DO clean up leakages and spillages immediately and thoroughly.

Description Clear, colorless liquid with a faint gasoline-like odor

Boiling point 98°C

Specific gravity 0.6837

Solubility in water Insoluble

Vapor pressure 40 mmHg at 20°C

Vapor density 3.45

Fire and explosion hazard

Heptane is flammable (USA definition)/highly flammable (European definition)

Explosive limits 1.05–6.7%

Ignition temperature 223 °C

Storage and handling

Material Safety Data Sheets

4. Select the MSDS document you want to view.

3. Log in to Spectrum software.

4. Ensure that your instrument is included in the list of available instruments.

8. Perform the AVI Calibration as described in AVI Calibration on page 27.

Unpacking the Kit

Part Number Description Quantity

LX108938 In-Service Lubricants FT-IR Touch App™ Software Kit 1

L1272309 Used-Oil Flow Cell (with ZnSe windows) 1

L1608117 IR Flow Cell Waste Tubing with Luer Fitting 1

L1608118 Plastic Syringe 3 mL Luer Lock (pack of 100) 1

04821008 PTFE Stopper – Luer Fitting (pack of 6) 1

L9003631 Torque Driver (24 cNm) 1

L9003632 Hexagonal Bit (3.0 mm) 1

Additional Materials Required

• Sample for pathlength determination

• Waste bottle with a drilled cap.

• Lens tissue or cotton buds

2. Start Spectrum Software.

4. Select Standardize from the Measurement menu.