ANALYTICAL METHOD - SPECIFICATION

PREPARED BY
ANALYTICAL SCIENCES LABORATORY

AM-S 1440-01
July 2001

EXXONMOBIL RESEARCH AND ENGINEERING COMPANY

600 BILLINGSPORT ROAD, PAULSBORO, NEW JERSEY 08066

SCREENING OF NEW OIL BLENDS AND ADDITIVES (INFRARED METHOD)

1.

Introduction

1.1 This revision includes both dual and

single beam instrument methods within one
procedure, reflecting the predominant use of
Fourier Transform Infrared technology.

standard does not purport to address all of the

safety problems associated with its use. It is the
responsibility of whoever uses this standard to
consult and establish appropriate safety and
health practices and to determine the applicability
of regulatory limitations prior to use.

1.2 The "Calculation" and "Report" sections

have been revised to include more clarity in the
interpretation of infrared test results as they relate
to complementary specification test results.

3.

1.3 The procedure for screening incoming

additives and base stocks, and greases has been
extracted from the comparative method for
finished lubricants, and moved to Appendix A.

3.2 ASTM E1421, Practice for Describing and

Measuring Performance of FT-IR Spectrometers.

Referenced Documents

3.1 MLP13, "Mobil Lab Practice 13, General

Methods of Infrared Absorption Analysis."

4.

Summary of Method

1.5 A procedure has been added that allows

visual comparison of the sample scan to reference
handblend scans that bracket the allowable
variation in additive content (Appendix B).

4.1 An infrared scan of the new oil and/or

additive blend is generated. The infrared
absorbance spectrum of the base oil, or primary
base stock component of the blend, is subtracted
from that of the sample scan. Comparison of key
additive peaks in the sample is made to a
reference handblend, which has been similarly
analyzed.

2.

5.

1.4 The procedure for preparing solid

samples for analysis has been included in
Appendix A.

Scope

2.1 This method is used primarily to identify

and comparatively quantify additives in new oil
and additive blends that have significant and
unique infrared (IR) absorbances. The method
may be used to confirm that no other nonformulation IR-absorbing additives or
contaminants are present at detectable levels.
2.2 The method also provides a screening
procedure for neat additives (not blended or
diluted by the plant) and base stocks to confirm
similarity to reference materials, and check for IRabsorbing contaminants. Similarly, greases can
be screened using this procedure.
2.3 The method is applicable to all petroleum
products and additives manufactured and/or
purchased by ExxonMobil that are liquid or solid
and which are compatible with potassium bromide
(KBr) or zinc selenide (ZnSe) cells.
2.4 This standard may involve hazardous
materials, operations, and equipment. This

Definitions/Terminology

5.1 HATR Accessory. Horizontal Attenuated

Total Reflectance accessory for use (in this
method) with very viscous liquids.
5.2 Reference Handblend. This is a
laboratory prepared sample containing all the
additives of the finished product, per each
formulation to be screened.

6.

Apparatus

6.1 Infrared Spectrophotometer, capable of

scanning from 4000 to 400 cm-1 (2.5 to 25 um).
Either single beam or dual beam instruments are
acceptable for use, Fourier Transform or
dispersive infrareds. Follow the manufacturer's
instructions for instrument setup, including dry gas
purge recommendations.
6.2 Potassium bromide (KBr) cells, assorted
pathlengths. Two matched KBr cells are required
if a dual beam instrument is in use. 0.2 mm (200
um) and 0.1mm (100 um) are most commonly

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used, but the cell pathlength should be

appropriate for the intensity of the absorbance
bands of interest in the sample.

8.2 Keep flammable solvents away from

infrared sources (inside instrument). Fire and/or
explosion may occur.

NOTE 1: If base oil and handblend reference

spectra are to be stored for later use, as in
automated calculation routines, cell pathlengths
for each cell used must be stored with the
associated spectra. For information on cell
calibration, consult MLP13.

8.3 Helium-Neon lasers used in FTIR

spectrometers can cause retinal damage if eyes
are exposed to beam. Keep the sample
compartment cover closed during operation to
avoid exposure.

9.
6.3 Horizontal Attenuated Total Reflectance
(HATR) accessory, for the analysis of viscous
additives, strongly absorbing additive
concentrates, and/or greases. A trough plate
accessory with a ZnSe crystal is recommended.
NOTE 2: HATR accessories are made by a
variety of manufacturers, and must be purchased
specifically for your instrument. Alternatively, two
KBr plates, 4 mm x 25 mm round, with a 0.025
mm (25 um) Teflon spacer, can be substituted. If
viscosity is not an issue, a 0.025 mm (25 um) KBr
cell can be used as well.

7.

Reagents and Materials

7.1 Reference Handblend, standard

laboratory blended sample containing all the
additives per each formulation to be screened. It
is important to make this sample as accurately as
possible to the formulation of the product being
tested.
7.2 Base stock(s) similar to that of the sample
being tested. The same base stock blend is best
if available. Synthetic PAO and ester stocks
should be used when appropriate.
7.3 Solvent for cleaning KBr cells. The
solvent must be capable of dissolving and
washing away residual lubes and/or additives. A
50/50 mixture of heptane and toluene has been
found suitable. See MLP13 for additional
information.

8.

Safety

8.1 Consult Material Safety Data Sheets for

information on the solvents used for cleaning
cells, as well as additives and base stocks used
for handblends. Establish and follow appropriate
safety and health practices.

Procedure
9.1 Instrument Performance Verification

9.1.1 Follow the instrument manufacturer's

recommendations for calibration and instrument
performance verification. This usually includes,
but is not limited to, running a polystyrene test
film. If a procedure is not provided by the
manufacturer, consult ASTM E1421 for guidance
on FTIR instrumentation; MLP13 for dispersive
instruments.
9.1.2 Many FTIR instruments will
automatically perform validation checks as part of
the instrument start-up routine.
9.2 Single Beam Spectrometer Method
9.2.1 Analysis of New Oil and FreeFlowing Additive Blends, Slurries, and
Premixes
9.2.1.1 Make certain the sample is free of
visible air bubbles. An ultrasonic bath can be
used to remove entrained air if necessary.
9.2.1.2 Fill the sample cell with the base oil or
base oil blend. Make sure the cell is filled
completely, and that there are no air bubbles.
Record a background spectrum, then record the
infrared absorbance spectrum. See Figure 1.
NOTE 3: A new background spectrum is typically
run before each sample for single beam
instruments. This may be unnecessary if
instruments are not purged. Each laboratory
should establish a frequency for running
background scans, recognizing that the frequency
can change in laboratories where climate control
is poor.
9.2.1.3 Using the manufacturer's software,
store this spectrum for later calculations (Srefb).

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9.2.1.4 Remove and clean the cell.

9.2.1.5 Fill the cell with the reference
handblend, and record the infrared absorbance
spectrum. See Figure 2.
9.2.1.6 Using the manufacturer's software,
store this spectrum (Sref).
9.2.1.7 Remove and clean the cell. Fill the
cell with the sample, and record the infrared
absorbance spectrum. Store this spectrum (Ssam).
9.2.2 Analysis of Strongly Absorbing
Liquid Additive Blends, Slurries, and Premixes
9.2.2.1 Follow the manufacturer's instructions
for use, care and cleaning of the HATR
accessory. Smear or pour a base stock similar to
that used in the additive blend, slurry, or premix
on the HATR window, being sure that no bubbles
are against the crystal face. Cover the crystal
face entirely.
9.2.2.2 If KBr disks are substituted for the
HATR accessory, place a drop of base stock on
one KBr disk. Place a 0.025 mm (25 um) Teflon
spacer on top of the disk. Carefully, to avoid
bubble formation, place a second plate on top,
and lightly press down to form a capillary film.
9.2.2.3 Record the infrared absorbance
spectrum of the base stock (Srefb).
9.2.2.4 After cleaning the HATR or KBr disks,
similarly prepare and record a spectrum of a
reference handblend of the additive blend, slurry,
or premix (Sref).
9.2.2.5 Clean the HATR or KBr disks, then
prepare and record an absorbance spectrum of
the sample (Ssam).
9.3 Dual Beam Spectrometer Method
9.3.1 Analysis of New Oil Blends and
Free-Flowing Additive Blends, Slurries, and
Premixes
9.3.1.1 Make certain the sample is free of
visible air bubbles. An ultrasonic bath can be
used to remove entrained air if necessary.
9.3.1.2 Fill reference cell with a base oil blend
similar to the formulated product or the neat
additive and place in the instrument reference

beam. Make sure the cell is completely filled, and

that there are no air bubbles.
9.3.1.3 Similarly, fill the sample cell with the
reference handblend, making sure the cell is
completely filled and free of air bubbles.
9.3.1.4 Record the differential IR scan of the
reference in absorbance (DSref).
9.3.1.5 Remove and clean the sample cell.
Replace the IR pen with one containing a different
color of ink. Return the IR chart paper to the
beginning of the reference scan.
NOTE 4: If software that allows storage of spectra
is in use, the differential scan can be stored for
further calculations.
9.3.1.6 Refill the sample cell with the sample
to be screened and place in the sample beam.
9.3.1.7 With the different color pen, run an
absorbance scan on the same chart paper
(DSsam).
NOTE 5: If software that allows storage of spectra
is in use, the differential scan can be stored for
further calculations.
9.3.2 Analysis of Strongly Absorbing
Liquid Additive Blends, Slurries, and Premixes
9.3.2.1 Follow the procedure given in 9.2.2.1
and 9.2.2.2 for sample preparation.
9.3.2.2 Acquire spectra following 9.3.1.2
through 9.3.1.7.

10.

Calculations

10.1 If using a single beam instrument,

perform a 1:1 subtraction of the base stock
spectrum, Srefb, from the reference handblend
spectrum (Sref). For dual beam instruments, work
directly with the differential spectrum (DSref). All
spectra should be in absorbance. See Figure 3.
NOTE 6: A 1:1 subtraction can give negative
bands due to base stock absorbances, since base
stock is less concentrated in the sample than in
pure base stock. However, this will not affect
analysis of the additive components and should
be ignored. See Figures 4 and 5 for illustrations.

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10.2 Using the Formulation & Technical

Standard (F&TS), or similar product guidance,
identify key additive peaks. Ideally, these peaks
should be unique to a particular additive
component, or additive package. Avoid peaks
that have base stock interferences, such as
carbon-hydrogen bonding regions.
NOTE 7: Not all additives will be detected as
unique absorbances. Not all additives will have
detectable infrared absorbances in product
matrices when dosage levels are relatively low.

11.

11.1 Report as "Match" if sample meets all of

the following criteria:

Key additive peaks are within +/- 10% of the

reference additive peaks, or in the case of a
bulk receipt (non-manufacturing) facility, the
manufacturing plant has investigated any
additive levels outside of these limits, and
found them to be acceptable.

Sample shows no evidence of contamination

(peaks which are not present in the reference,
and are not associated with allowable base
stock interchange).

10.3 Measure either the net absorbance or

area of each of the key additive peaks. Record
these values. This is illustrated in Figures 4 and
5.
NOTE 8: Absorbances to be used in subsequent
measurements should fall below approximately
1.5 AU. Above this, instrument response is not
always linear. If the net absorbance value of the
band of interest is greater than 1.5 AU, choose a
cell with a smaller pathlength, or use HATR (See
6.2), and rerun the handblend, base stock, and
the sample.
10.4 Calculate the absorbance or area per
centimeter, by dividing by the cell pathlength in
centimeters (Aref1, Aref2, etc.).
NOTE 9: If software is available and used to
automate calculations, make sure cell pathlength
is accounted for in calculations. This may require
that cell calibration values are stored and
associated with specific reference scans.
10.5 Similarly, subtract the base stock
spectrum, Srefb, from the sample spectrum Ssam, or
use the differential scan for the sample (DSsam) if
obtained with a dual beam instrument. Measure
the net absorbance or area of each key additive
peak identified in the reference product, and
calculate the absorbance or area per centimeter
(Asam1, Asam2, etc.).
Compare the values obtained for the sample
spectrum components to the reference subtracted
spectrum. Determine the percentage of the
reference handblend for each component:
% Stock Component 1 = Asam1/Aref1 *100%
% Stock Component 2 = Asam2/Aref2 *100%

Reporting

NOTE 10: It is suggested that the manufacturing

plant provide a copy of their infrared spectra and
results of key additive peaks to any internal bulk
receipt facilities for comparison.
11.2 Investigate any sample where key
additive peaks are outside of +/- 10% of the
reference additive peaks. Report as "Match" if
one or more of the following criteria are met:

Measured variation is equal to or less than

that specified in the product F&TS or similar
product guidance (example: allowable
variation of calcium level is 33% in some
products, which may translate to a 33%
allowable variation in measured sulfonate
value).

Specific additives are within formulation

tolerance as measured by a primary test
procedure (examples: phosphorus by ICP vs.
phosphate ester band by IR; phenolic inhibitor
by MM872 quantitative method).

Additive level can be varied to meet product

specifications per the product F&TS or similar
product guidance (example: adjustment with
additional pour point depressants).
11.3 Report as "No Match" if sample results

do not meet the above criteria.

12.

Quality Control

12.1 Quality control sample(s) can be chosen

that are representative of the particular products
manufactured or tested at a facility. Since the
reported results are "Match" and "No Match", the

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stock component percentages calculated in 10.6

can be either charted or logged as precision
monitors if desired.

13.

Precision and Bias

13.1 The standard estimates of repeatability

and reproducibility are not applicable to this
method.

Appendix B, "Visual Comparison Method"

Figures 1-5, Spectra from Single Beam

Spectrometer, Engine Oil and Hydraulic Oil

Figures 6-8, Visual Comparison Method

15.

Document History

1986

14.

Additional Information
1991, 1995
July 2001

14.1 Attached are:

Appendix A, "Screening Procedure for

Incoming Additives, Base Stocks, and
Greases"

Adopted Mobil Analytical

Method
Revised
Revised, ExxonMobil L&PS,
MTS Laboratory, Paulsboro,
NJ

DISCLAIMER
The method, and information upon which it is based, is believed by ExxonMobil to reflect sound scientific
analytical techniques; however, ExxonMobil does not represent that the analytical method is error free.
ExxonMobil makes no representations, warranties, or guarantees, with respect to its use. ExxonMobil shall
have no responsibility hereunder to (the other party) or to (such party's) employees for any injury or harm, for
loss of profits, consequential or indirect damages resulting from use of such information, or for liabilities
relating to negligent acts or omissions by ExxonMobil's employees.

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APPENDIX A
SCREENING PROCEDURE FOR INFRARED ANALYSIS OF INCOMING ADDITIVES, BASE STOCKS, AND
GREASES
A.1

Introduction

A.6.2.2 KBr pellet press and die

A.1.1 This appendix describes a procedure

for screening greases, incoming raw materials,
additives, and base stocks for contaminants using
infrared spectroscopy.

A.2

A.7

A.2.2 Additives can be free-flowing or

viscous liquids, or solids.
A.2.3 Greases can also be screened using
this procedure, compared to a laboratory or
production "reference" sample.

Referenced Documents

A.3.2 ASTM E1421, Practice for Describing

and Measuring Performance of FT-IR
Spectrometers.

Summary of Method

A.4.1 An infrared scan of the sample is

generated, and visually compared with that of a
reference material obtained in a similar manner.

A.5

Definitions/Terminology
A.5.1

A.6

See Section 5.

NOTE A1: It may not be possible to obtain a true

"reference" additive, but most suppliers will
provide a typical sample that can be used for
comparison with incoming shipments.
A.7.3 Potassium bromide (KBr) powder,
spectroscopic grade. Store in desiccator to avoid
exposure to atmospheric moisture.

A.8

Safety
A.8.1

A.9

See Section 8.

Procedure

A.9.1 Follow Section 9.1 for instrument

performance verification.
A.9.2

Sample Preparation

A.9.2.1 Free Flowing Additives and Base

Stocks: Follow Sections 9.2.1.1-9.2.1.2.
A.9.2.2 Viscous Liquid Additives, Strongly
Absorbing Additives, and Greases: Follow 9.2.2.19.2.2.2.
A.9.2.3 Solids

Apparatus
A.6.1

See Section 7.

A.7.2 Reference additives and base stocks,

representative of production as supplied by
manufacturer. Grease handblend or
representative production sample.

A.3.1 MLP13, "General Methods of Infrared

Absorption Analysis".

A.4

Reagents and Materials

A.7.1

Scope

A.2.1 This appendix provides a screening

procedure for neat additives (not blended or
diluted by the plant) and base stocks to confirm
similarity to reference materials, and check for IRabsorbing contaminants.

A.3

A.6.2.3 Pellet holder for instrument sample

compartment.

See Section 6.

A.6.2 The following are required to prepare

solid samples:

A.9.2.3.1 Weigh 1-3 mg of the solid

reference sample into an agate mortar.
A.9.2.3.2 Using the pestle, grind the sample
until it is very finely divided.

A.6.2.1 Agate mortar and pestle

6

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A.9.2.3.3 Add 300 mg KBr powder in

approximately three equal portions, using the
pestle to mix, not grind, the sample and KBr
powder uniformly together.
A.9.2.3.4 Pour the mixture into the die and
place the die in the press.
A.9.2.3.5 Follow the manufacturer's
instructions to operate the press. Usually, 8-10
tons of pressure is required for 3-5 minutes, but
some "micro" or hand presses have specific
recommended conditions for preparation.
A.9.2.3.6 Carefully remove the newly
formed pellet from the die and place it in a pellet
holder.

A.11

Report

A.11.1 Report as "Match" any sample scan

that is similar to that of its reference, with no
evidence of contamination.
A.11.2 Report as "No Match" if dissimilar to
reference, or any contaminants are detected.

A.12

Quality Control

A.12.1 Not applicable.

A.13

Precision and Bias

A.13.1 The standard estimates of

repeatability and reproducibility are not applicable
to this method.

A.9.3 Record the absorbance spectrum of

the reference. If using software, store this
spectrum (Sref).
A.9.4 Clean the cell, HATR, KBr disk, or
mortar, pestle, and die. Similarly, prepare the
sample in question.
A.9.5 Record the sample spectrum in a
similar manner, either storing the spectrum (Ssam),
or using a different pen color on the same piece of
chart paper.

A.10

Calculations

A.10.1 If the spectra have been stored

electronically, recall the reference scan, and
overlay the sample scan (Sref overlaid with Ssam).
A.10.2 Examine the spectra carefully for
similarities and differences in peak location and
relative intensity. Note the presence of any
contaminants.
NOTE A2: If examining spectra generated on
solids prepared in KBr, bands in the OH regions
can be due to water absorbed by the KBr. Follow
the die and press manufacturer's instructions to
minimize exposure to moisture during sample
preparation. Suspected water contamination in
solid additives may need to be confirmed by
another technique.

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APPENDIX B
VISUAL COMPARISON METHOD

B.1

Introduction

B.1.1 This procedure allows an alternate

means of determining whether a new oil or
additive blend meets the criteria of AM-S 1440
using visual comparison.

B.2

Scope

B.2.1 This method is used to identify and

comparatively quantify additives in new oil and
additive blends that have significant and unique
infrared (IR) absorbances. The method may be
used to confirm that IR-absorbing additives and
contaminants that should not be present are not
detected in the sample.
B.2.2 This procedure is useful for
laboratories that do not have electronic data
handling capabilities.

Based on this visual plot, a judgement is made as

to whether the sample falls within the +/- 10%
allowance for the method.
B.4.4 This method cannot be used where
additive solubility prevents proper preparation of a
handblend at other than target dosages.
Handblends made at other than the target additive
dosages must be similar in appearance to the
target blend. The blend should be clear and
bright with no sediment.
NOTE B1: Some finished products have an
allowable slight hazy appearance. In this case,
any handblends made at other than target
dosages should be similar in appearance, with no
significant increase in haze.

B.5

Definitions/Terminology

See Section 5.

B.3

Referenced Documents
B.6

B.3.1 MLP13, "General Methods of Infrared

Absorption Analysis"

See Section 6.

B.3.2 ASTM E1421, Practice for Describing

and Measuring Performance of FTIR
Spectrometers.

B.7

B.4

B.8

Summary of Method

Apparatus

Reagents and Materials

See Section 7.

Safety

B.4.1 An infrared scan of the new oil and/or

additive blend is generated. The infrared
absorbance spectrum of the base oil, or primary
base stock component of the blend, is subtracted
from that of the sample scan.

See Section 8.

B.4.2 Comparison of this subtracted scan is

made visually to three reference handblend
scans. One is prepared to contain an additional
10% of all of the additives present; one is
prepared with the targeted amounts; and the third
is made with 10% less of all additives.

B.9.1.1 Using the formulation for the desired

product, prepare:

B.4.3 Absorbance spectra are overlaid,

after base stock absorbances are subtracted.
8

B.9

Procedure
B.9.1

Handblend Preparation

A reference handblend at the targeted

additive dosages,

A reference handblend containing all of

the additives at a 10% greater dosage
level, and

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A reference handblend containing all the

additives at a10% lower dosage than
targeted.

B.9.2 Instrument Performance

Verification
B.9.2.1 Follow Section 9.1.1.
B.9.3

Single Beam Spectrometer Method

B.9.3.1 Follow Section 9.2.

B.9.3.2 Collect spectra for all three reference
handblends, the appropriate base stock or base
stock blends, and the sample.
B.9.3.3 Store all spectra using the
manufacturer's software.
B.9.4

Dual Beam Spectrometer Method

B.9.4.1 Follow Section 9.3

B.9.4.2 Collect spectra for all three reference
handblends, and the sample, using the
appropriate base stock or base stock blend in the
reference beam.
B.9.4.3 Either record all four spectra on the
same chart paper, or store the spectra for later
analysis using manufacturer's software.

B.10

Calculations

B.10.1 If using a single beam instrument,

perform a 1:1 subtraction of the base stock
spectrum, Srefb, from the each reference
handblend (Sref1,2,3). Store each differential
spectrum (DSref1,2,3). For dual beam instruments,
work directly with the differential spectra that were
recorded in B9.4.3.
B.10.2 See Section 10.2, and Note 7.

sample, and base stock in a smaller cell or use

HATR.
B.10.4 Similarly, use a 1:1 subtraction to
subtract the base stock spectrum, Srefb, from the
sample spectrum, Ssam. Store this differential
spectrum, DSsam. If working with a dual beam
instrument, the differential scan has already been
created for the sample in B9.4.2, and either
charted, or stored electronically.
B.10.5 If spectra are stored electronically,
recall the differential scans of the "on target"
handblend, and both the +/-10% blends. Recall
the sample differential. Overlay these spectra on
the same scale. Take care to ensure that the
baselines are not offset. See Figures 6-7.
B.10.6 Looking at the overlaid spectra,
whether recalled electronically, or plotted on chart
paper, ensure that the key additive peaks for the
sample in question lie within the absorbance
minimum and maximum limits created by the
handblends. See Figure 8.
B.10.7 Examine the differential spectra
carefully for evidence of contamination (peaks
which are not present in the handblend, and are
not associated with allowable base stock
interchange).

B.11

Report

B.11.1 See Section 11.

B.12

Quality Control

B.12.1 See Section 12.

B.13

Precision and Bias

B.13.1 The standard estimates of

repeatability and reproducibility are not applicable
to this method.

B.10.3 See Note 8. If absorbance values for

key peaks exceed 1.5 AU, rerun the handblends,

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FIGURES 1-5
SPECTRA FROM SINGLE BEAM SPECTROMETER, ENGINE OIL AND HYDRAULIC OIL
1. This is a typical absorbance spectrum of a base stock, 200 um cell.
Paraffinic Neutral Base Stock, 200 um
3.0

2.5
A
b
s
o
r
b
a
n
c
e

2.0

1.5

1.0

0.5

0.0
4000

3500

3000

2500

2000

1500

1000

500

1000

500

Wavenumbers
1: LPM3052: Paraffinic Neutral Base Stock, 200 um

2. This is a typical engine oil absorbance spectrum, 200 um.

Typical Engine Oil, 200 um
3.0

2.5
A
b
s
o
r
b
a
n
c
e

2.0

1.5

1.0

0.5

4000

3500

3000

2500

2000

1500
Wavenumbers

1: RN4598AA: Typical Engine Oil, 200 um

10

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3. When the base stock is subtracted from the reference handblend or sample spectrum, a differential
spectrum like the one below results.
Subtracted Spectrum, Engine Oil - Base Stock, 200 um

0.6

A
b
s
o
r
b
a
n
c
e

0.4

0.2

0.0

-0.2

4000

3500

3000

2500

2000

1500

1000

500

Wavenumbers
1: RN4598AA: Subtracted Spectrum, Engine Oil - Base Stock, 200 um

4. Some of the key additive peaks are identified below, and their net absorbance values given. The
hydrocarbon regions, which can give regions of negative absorbance after subtraction, are outlined in red,
and should be ignored. The green box shows a negative absorbance due to carbon dioxide vapor
differences, and should be ignored.
Engine Oil Spectrum after Base Oil Subtraction, 200 um

0.5

A
b
s
o
r
b
a
n
c
e

0.2649

0.4
0.1773

0.3

0.1234

0.1325
0.2

0.1

0.0

-0.1

4000

3500

3000

2500

2000

1500

1000

500

Wavenumbers
1: RN4598A: Engine Oil Spectrum after Base Oil Subtraction, 200 um

COPYRIGHT 2001
EXXONMOBIL RESEARCH AND ENGINEERING COMPANY
ALL RIGHTS RESERVED

11

AM-S 1440-01
July 2001

5. In this subtracted spectrum of a hydraulic oil, hydrocarbon regions are noted by red boxes, and should be
ignored. Carbon dioxide vapor differences are outlined in green and should be ignored. In this product, key
additive bands are noted with their net absorbance values.
Hydraulic Oil after Base Stock Subtraction, 200 um

1.2

0.8947
1.0

A
b
s
o
r
b
a
n
c
e

0.8

0.6

0.4

0.2

0.0343

-0.0

-0.2

4000

3500

3000

2500

2000

1500

1000

Wavenumbers
1: RL1546E-: Hydraulic Oil after Base Stock Subtraction, 200 um

12

COPYRIGHT 2001
EXXONMOBIL RESEARCH AND ENGINEERING COMPANY
ALL RIGHTS RESERVED

500

AM-S 1440-01
July 2001

FIGURES 6-8
APPENDIX B: VISUAL COMPARISON METHOD
6. Below are three difference spectra of reference handblends prepared to contain 90 (green), 100 (blue),
and 110% (red) of the targeted additive dosages.
Reference Handblends, Difference Spectra, 90, 100, and 110% of Target Dosages

0.8

A
b
s
o
r
b
a
n
c
e

0.6

0.4

0.2

0.0

-0.2
3500

3000

2500

2000

1500

1000

500

Wavenumbers

7. The difference scan for the sample is overlaid (in black).

Reference Handblends, Difference Spectra, 90, 100, and 110% of Target Dosages

0.8

A
b
s
o
r
b
a
n
c
e

0.6

0.4

0.2

0.0

-0.2
3500

3000

2500

2000

1500

1000

500

Wavenumbers

COPYRIGHT 2001
EXXONMOBIL RESEARCH AND ENGINEERING COMPANY
ALL RIGHTS RESERVED

13

AM-S 1440-01
July 2001

8. Key additive regions are expanded below to show that the production sample is between 90 and 100% of
the target additive dosage.
Production Sample vs. Reference Handblends

1706.51, 0.3655

0.40

A
b
s
0.30
o
r
b
a
n
c 0.20
e

0.10

1780

1760

1740

1720

1700

1680

1660

Wavenumbers

Production Sample vs. Reference Handblends

974.84, 0.6446

0.70
1229.59, 0.5465

A 0.60
b
s
o
0.50
r
b
a
n 0.40
c
e
0.30

0.20

1300

1200

1100

1000

Wavenumbers

14

COPYRIGHT 2001
EXXONMOBIL RESEARCH AND ENGINEERING COMPANY
ALL RIGHTS RESERVED

900