This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D7889 − 21

Standard Test Method for

Field Determination of In-Service Fluid Properties Using IR
Spectroscopy1
This standard is issued under the fixed designation D7889; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.

1. Scope* 2. Referenced Documents

1.1 This test method describes the use of a grating spec- 2.1 ASTM Standards:2
trometer to analyze properties of an in-service fluid sample D4057 Practice for Manual Sampling of Petroleum and
which are indicative of the status of that fluid and related Petroleum Products
machinery. D7412 Test Method for Condition Monitoring of Phosphate
Antiwear Additives in In-Service Petroleum and Hydro-
1.2 This test method provides a means for the assessment of carbon Based Lubricants by Trend Analysis Using Fourier
in-service fluid properties using infrared spectroscopy. It de- Transform Infrared (FT-IR) Spectrometry
scribes a methodology for sampling, performing analysis, and D7414 Test Method for Condition Monitoring of Oxidation
providing key in-service fluid properties with a self-contained in In-Service Petroleum and Hydrocarbon Based Lubri-
unit that is meant for field use. It provides analysis of in-service cants by Trend Analysis Using Fourier Transform Infrared
fluids at any stage of their useful life, including newly utilized (FT-IR) Spectrometry
fluid. D7415 Test Method for Condition Monitoring of Sulfate
1.3 In particular, these key in-service fluid properties in- By-Products in In-Service Petroleum and Hydrocarbon
clude oxidation, nitration, sulfation, soot, and antiwear addi- Based Lubricants by Trend Analysis Using Fourier Trans-
tives. They are applicable for hydrocarbon type (API Group form Infrared (FT-IR) Spectrometry
I-IV) fluids from machinery lubricants, including reciprocating D7418 Practice for Set-Up and Operation of Fourier Trans-
engine oils, turbine oils, hydraulic oils, and gear oils. form Infrared (FT-IR) Spectrometers for In-Service Oil
Condition Monitoring
1.4 The values stated in SI units are to be regarded as D7624 Test Method for Condition Monitoring of Nitration in
standard. No other units of measurement are included in this In-Service Petroleum and Hydrocarbon-Based Lubricants
standard. by Trend Analysis Using Fourier Transform Infrared
1.4.1 Exception—The unit for wavenumbers is in cm-1. (FT-IR) Spectrometry
1.5 This standard does not purport to address all of the D7669 Guide for Practical Lubricant Condition Data Trend
safety concerns, if any, associated with its use. It is the Analysis
responsibility of the user of this standard to establish appro- D7720 Guide for Statistically Evaluating Measurand Alarm
priate safety, health, and environmental practices and deter- Limits when Using Oil Analysis to Monitor Equipment
mine the applicability of regulatory limitations prior to use. and Oil for Fitness and Contamination
D7844 Test Method for Condition Monitoring of Soot in
1.6 This international standard was developed in accor-
In-Service Lubricants by Trend Analysis using Fourier
dance with internationally recognized principles on standard-
Transform Infrared (FT-IR) Spectrometry
ization established in the Decision on Principles for the
E131 Terminology Relating to Molecular Spectroscopy
Development of International Standards, Guides and Recom-
E168 Practices for General Techniques of Infrared Quanti-
mendations issued by the World Trade Organization Technical
tative Analysis
Barriers to Trade (TBT) Committee.
E177 Practice for Use of the Terms Precision and Bias in
ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.96.03 on FTIR Testing Practices and Techniques Related to
2
In-Service Lubricants. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2021. Published August 2021. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2013. Last previous edition approved in 2013 as D7889 – 13. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7889-21. the ASTM website.

*A Summary of Changes section appears at the end of this standard

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D7889 − 21
Determine the Precision of a Test Method
E932 Practice for Describing and Measuring Performance of
Dispersive Infrared Spectrometers
E1655 Practices for Infrared Multivariate Quantitative
Analysis
E2412 Practice for Condition Monitoring of In-Service Lu-
bricants by Trend Analysis Using Fourier Transform
Infrared (FT-IR) Spectrometry
E2617 Practice for Validation of Empirically Derived Mul-
tivariate Calibrations
3. Terminology
3.1 For definitions of terms relating to infrared spectroscopy
used in this test method, refer to Terminology E131. For
definition of terms related to infrared-based in-service fluid
condition monitoring, refer to Practice D7418.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 absorbance units (AU), n—units of measurement of
the raw absorbance spectrum which is obtained using the
definition described in Section 8 (Theory for a Single Com-
pound Analysis) of Practice E168, which is not normalized for
pathlength.
3.2.2 cell background, n—a single-beam spectrum that is
obtained on a clean, empty wipe-clean transmission cell.
3.2.3 mid-infrared grating spectrometer, n—a spectrometer
which operates in the mid-infrared spectral range, between at
least 960 cm-1 and 3040 cm-1 and creates an infrared spectrum
by means of a reflective diffraction grating.
3.2.3.1 Discussion—Such a grating spectrometer may be of
any of a variety of designs and optical configurations. Example
designs include monochrometer-type systems wherein the
grating is rotated to a single point infrared detector, or
array-type systems which utilize an infrared detector array at
the output and a fixed grating. Example optical configurations
include Rowland-Circle and Czerny-Turner systems. Typical
infrared detectors are uncooled thermal detectors such as
thermopile or pyroelectric-based sensors.
3.2.4 reporting units, n—specifies the reporting units of the
fluid analysis property.
3.2.5 self-contained field apparatus, n—a mid-infrared grat-
ing spectrometer which is of the form factor to allow it to
operate as an independent device suitable for field use.
3.2.6 wipe-clean transmission cell, n—an infrared transmis-
sion cell which is specifically tailored for field use.
3.2.6.1 Discussion—In particular, the cell may be utilized
and cleaned with a towel or rag and without the use of reagents
or chemicals of any sort, making it convenient for use as a field
device. Such transmission cells may accomplish this using
mechanisms for quick open/close of the cell such as by means
of a mechanical lever, demountable screw or press fit, or
magnetic coupling. To correct for any cell fringing effects, the
cell utilizes a wedged design both on the interior faces and
exterior faces of the cell windows: The cell windows them-
selves are wedged at an angle of less than 0.5 degrees. The
spacing between the two windows is wedged at an angle of
approximately 0.013 degrees. The cell is designed to be
nominally 100 µm in pathlength, with ZnSe windows.
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4. Summary of Test Method
4.1 This test method utilizes a self-contained field apparatus
to provide detailed information concerning the condition status
of in-service fluids. In particular, it provides readings of
oxidation, antiwear additive, sulfation, nitration and soot levels
in hydrocarbon type (API Group I-IV) fluids.
4.1.1 An absorbance spectrum of the sample under test is
obtained. For the background spectrum, the cell background is
used.
4.1.1.1 Test Methods have been developed for Fourier-
transform infrared (FTIR) devices using absorbance spectra
obtained using Practice D7418. Particular Test Methods devel-
oped for in-service monitoring of hydrocarbon type (API
Group I-IV) fluids include those established for Oxidation
(Test Method D7414, Procedure A), Antiwear Additive (Test
Method D7412, Procedure A), Sulfation (Test Method D7415,
Procedure A), Nitration (Test Method D7624, Procedure A),
and Soot (Test Method D7844, Procedure A). These test
methods have served to establish the signature infrared spec-
troscopic behavior associated with key in-service monitoring
properties. This test method provides property values based on
the examination of each property’s signature infrared spectro-
scopic behavior. The essence of this test method is to capture
the underlying chemical trends associated with each property
for in-service fluid analysis using a self-contained field appa-
ratus and coupled wipe-clean transmission cell.
4.1.2 From the infrared absorbance spectrum obtained with
the self-contained field apparatus, properties of the in-service
fluid are calculated. In particular, those properties in Table 1
are calculated by the device and presented to the user on the
display. Additional properties using infrared calibration meth-
ods may be calculated and displayed depending on the particu-
lar fluid being analyzed and availability of calibrations for that
fluid.
4.1.2.1 Infrared spectra generated by the described instru-
ment type can be used to provide a further set of properties of
interest to in-service fluid analysis of hydrocarbon type (API
Group I-IV) fluids. Such properties must be calibrated to the
particular fluid blend, and may be generated using ASTM
guidelines which govern the creation of such calibrations. Such
calibrations may be built from either standard regression
methods as described in Practice E168 or as described in
Practice E2412. Further, they may also be multivariate
calibrations, described in Practice E1655 and Practice E2617.
Example properties include Acid Number (AN), Base Number
(BN), water contamination, ethylene glycol, fluid mixture
content, and antioxidant depletion. It should be noted that, due
to the fact that these calibrations are sample-specific, this test
method does not provide a prescription for calculating such
properties.
TABLE 1 In-Service Lubricant Properties Reported by the Test
Method
Property Reporting Units
Oxidation Abs/0.1 mm
Antiwear Additive Abs/0.1 mm
Sulfation Abs/0.1 mm
Nitration Abs/cm
Soot Abs/cm
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 D7889 − 21
4.2 The results of the test method can be compared against for grating instruments as discussed in Practice E932 may be
pre-defined or user-defined limits so as to judge the condition performed. The absorbance spectrum of this material measured
of the in-service lubricant. Warning and alarm limits ex- with the spectrometer should show a peak at band number 12
ceedences which may be pre-defined or set by the user are (1028 cm-1) of approximately 0.29 AU and a peak at band
indicated by the property and associated value being high- number 2 (2924 cm-1) of approximately 0.56 AU. Other
lighted using coding established in Guide D7720, with either spectral resolutions may provide accurate results as well but
green (favorable alarm level designation showing acceptable the calculation parameters listed in Table 2 and Section 17 may
condition), yellow (intermediate level alarm designation warn- be different from those listed.
ing a fault condition is present and will likely need attention in 7.5 Spectral Range—Shall cover the frequencies necessary
the future), or red (high level alarm designation showing for calculation of all properties described in the method, which
significant deterioration) indicated by the self-contained field is 960 cm-1 to 3040 cm-1.
apparatus.
8. Reagents and Materials
5. Significance and Use
8.1 The only materials required to make a measurement are
5.1 This test method provides a means for obtaining useful
either a shop rag or lint-free paper towel to clean the wipe-
in-service fluid analysis properties in the field. It is not to be
clean transmission cell. No other materials or reagents are
confused with laboratory or portable FTIR devices which
necessary.
provide measurements per the existing Test Methods listed in
4.1.1.1. Each of these monitored properties has been shown
9. Hazards
over time to indicate either contamination in the fluid system or
a particular breakdown modality of the fluid, which is critical 9.1 The apparatus utilizes a certified Li-Ion battery.
information to assess the health of the fluid as well as the
machinery. By utilizing the field device, it is possible for those 10. Sampling, Test Specimens, and Test Units
operating machinery, in locations and situations where it is not 10.1 A sample of in-service fluid should be obtained. A
practical to gather a sample for the laboratory, to obtain quality minimum quantity of approximately 50 µL is needed to obtain
in-service fluid analysis. This may be due to the need to have one set of measurements as defined in Table 2. The sample
an analysis done in real-time, on-the-spot to maximize the should be representative of the system. If such equipment is
operational hours of equipment, or to have the analysis available, the sample is preferably obtained as described in
performed at a location where no laboratory analysis is Practice D4057.
available.
11. Preparation of Apparatus
6. Interferences
11.1 A quality collection of the infrared absorbance spec-
6.1 Spectral interferences due to very high levels of external trum is assured by several internal quality checks, which
contamination in the fluid can yield errors with these measure- include check fluid, pathlength, clean cell, and loaded cell
ments. Common contaminants include the presence of API monitoring.
Group V lubricants at levels exceeding 5 % and antifreeze 11.1.1 Check fluid and pathlength monitoring (described in
mixes at similar levels. Practice D7418) are performed on a periodic basis according to
manufacturer’s recommendations.
7. Apparatus
7.1 A self-contained mid-infrared grating spectrometer with
a coupled wipe-clean transmission cell as defined in Section 3.
TABLE 2 Specification for Calculation of Each In-Service Fluid
7.2 This spectrometer shall have specific performance char-
Property
acteristics indicated in 7.3 – 7.5, with a Spectral Format in the
Property Measurement, Baseline(s), Reporting
form of absorbance as a function of wavenumber reported at a (cm-1) (cm-1) Units
digital resolution of 2 cm-1. Oxidation Average Average Abs/0.1 mm
1800–1670 1815 to 1805
7.3 Signal-to-Noise Ratio (S/N)—shall be adequate to pro-
vide the desired precision as indicated in Section 17. Antiwear Additive Average Average Abs/0.1 mm
1025–960 1060 to 1030 and
Practically, this means that, over the range of measurement, the 1812 to 1803
standard deviation of the obtained absorbance should be less
than 0.001 AU. Based on the capabilities of the spectrometer Sulfation Average Average Abs/0.1 mm
1180–1120 1210 to 1200 and
system, this may be achieved by co-adding a number of scans 1115 to 1105
to improve the S/N as needed.
Nitration 100·Single Average Abs/cm
7.4 Spectral Resolution—shall be approximately 1.5 % of Point at 1630 1607 to 1597 and
frequency being measured across the measurement range. For 1847 to 1837
example, at 1000 cm-1, the spectral resolution should be
Soot 100·Single None Abs/cm
15 cm-1. In order to qualify this resolution, a simple test using Point at 2000
a 40 micron film of polystyrene, a standard reference material

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 D7889 − 21
11.1.2 In order to verify that the wipe-clean transmission
cell is empty and clean, a cell background is taken in real-time
and a raw absorbance spectrum is calculated using a previously
archived, known, empty, and clean cell background.
11.1.2.1 By measuring the maximum peak height between
3000 cm-1 and 2800 cm-1 relative to a baseline at 2700 cm-1, it
can be determined whether the cell is clean. When the
absorbance value is greater than a pre-set limit of 0.2 AU, the
cell is considered not clean.
11.1.2.2 This check is performed before any cell back-
ground to be used in the calculation of fluid properties is
obtained, and the user is warned if the check fails.
11.1.3 A cell loading check (as described in Practice D7418)
is performed on each loaded sample to ensure that the cell is
fully loaded. Such a check is performed according to manu-
facturer’s recommendations.
11.1.3.1 If the cell is determined to not be fully loaded, a
message that the cell is not fully loaded is displayed alongside
the results of the analysis. It should be noted that due to the
nature of the design for field use, the wipe clean transmission
cell has no need for fringe correction.
11.2 Ensure that wipe-clean transmission cell is clean by
visual inspection.
11.3 Gather approximately two drops of sample (on the
order of 50 µL).
11.3.1 This may be accomplished using a dropper, syringe,
or simply by using drops from a fluid dipstick, for example.
12. Calibration and Standardization
12.1 A check fluid is supplied with the apparatus as a
qualification test. This fluid should be run after each set of 100
samples to ensure that the unit remains within calibration.
12.2 If this qualification test fails, the user should follow
manufacturer’s recommendations regarding calibration and
standardization.
13. Conditioning
13.1 The field apparatus does not require conditioning nor
does the sample being analyzed.
14. Procedure
14.1 Whenever prompted, collect a cell background on the
device.
14.1.1 The cell background must be taken periodically
according to (a) the time from the last cell background (must
not be greater than 30 min) and (b) the current device
temperature relative to the temperature at which the previous
cell background was obtained (must not be greater than 3 K)
exceeding maximum allowable thresholds.
14.2 Place the two drops of in-service fluid on the wipe-
clean transmission cell.
14.2.1 Once the wipe-clean transmission cell is loaded with
sample, the user initiates a measurement. This measurement
comprises gathering the single-beam infrared spectrum of the
fluid.
14.3 From that single-beam spectrum (=P(counts(ν))), the
last saved cell background (=B(counts(ν))), and a pathlength
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normalization of the resulting spectrum (=PL(microns)), the
infrared absorbance spectrum (=A(ν)) of the fluid is calculated
by the apparatus:
A ~ v ! 5 2 ~ 100 ⁄ PL! · log10~ P ~ v ! ⁄B ~ v !! @ Abs/0.1 mm# (1)
14.3.1 The units of A(v), the infrared absorbance
spectrum, as indicated are Abs/0.1 mm.
15. Calculation or Interpretation of Results
15.1 Calculation of in-service fluid properties proceeds
according to the spectral analysis detailed in Table 2. These
analyses proceed using the signature infrared absorption bands
gleaned from the obtained infrared absorbance spectrum of the
fluid.
15.1.1 Properties are obtained from the absorbance spec-
trum using the measurement and baseline regions listed in
Table 2. Properties are presented to the user in the reporting
units specified.
15.1.1.1 Oxidation is obtained from calculating the average
absorbance (Abs/0.1 mm) in the measurement region between
1800 cm-1 and 1670 cm-1 Abs,av(1800 to 1670) and performing
a weighted subtraction from the average baseline absorbance
(Abs/0.1 mm) in the region between 1815 cm-1 and 1805 cm-1
Abs,av(1815 to 1805). The resulting units of measurement are
Abs/0.1 mm:
Oxidation=130 · Abs,av~ 1800 to 1670!
2 38.5 · Abs,av~ 1815 to 1805! @ Abs/0.1 mm# (2)
15.1.1.2 Antiwear additive is obtained from calculating the
average absorbance (Abs/0.1 mm) in the measurement region
between 1025 cm-1 and 960 cm-1 Abs,av(1025 to 960) and
performing a weighted subtraction from the average baseline
absorbance (Abs/0.1 mm) in the region between 1060 cm-1 and
1030 cm-1 Abs,av(1060 to 1030) as well as the region between
1812 cm-1 and 1803 cm-1 Abs,av(1812 to 1803). The resulting
units of measurement are Abs/0.1 mm:
Antiwear Additive 5 65 · Abs,av~ 1025 to 960!
2 8.4 · Abs,av~ 1060 to 1030!
2 10.8 · Abs,av~ 1812 to 1803! @ Abs/0.1 mm# (3)
15.1.1.3 Sulfation is obtained from calculating the average
absorbance (Abs/0.1 mm) in the measurement region between
1180 cm-1 and 1120 cm-1 Abs,av(1180 to 1120) and performing
a weighted subtraction from the average baseline absorbance
(Abs/0.1 mm) in the region between 1210 cm-1 and 1200 cm-1
Abs,av(1210 to 1200) as well as the region between 1115 cm-1
and 1105 cm-1 Abs,av(1115 to 1105). The resulting units of
measurement are Abs/0.1 mm:
Sulfation560 · Abs,av~ 1180 to 1120! 2 11 · Abs,av~ 1210 to 1200!
2 5 · Abs,av~ 1115 to 1105! @ Abs/0.1 mm# (4)
15.1.1.4 Nitration is calculated by measuring the absor-
bance (Abs/0.1 mm) of the sample at 1630 cm-1 Abs(1630),
and performing a weighted subtraction from the average
baseline absorbance (Abs/0.1 mm) in the region between
1607 cm-1 and 1597 cm-1 Abs,av(1607 to 1597) as well as the
region between 1847 cm-1 and 1837 cm-1 Abs,av(1847 to 1837).
The units of this calculation are Abs/0.1 mm. The final result is
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 D7889 − 21
obtained by multiplying the result by 100, yielding a result in
units of Abs/cm (100*Abs/0.1 mm = Abs/0.001 mm = Abs/
cm). This allows for easy-to-read numerical results in a typical
numerical range > 1 Abs/cm. The calculation is detailed as
follows:
Nitration=100 · ~ Abs ~ 1630!
2 0.89 · Abs,av~ 1607 to 1597!
2 0.11 · Abs,av~ 1847 to 1837!! @ Abs/ cm#
(5)
15.1.1.5 Soot is calculated by measuring the absorbance of
the sample at 2000 cm-1 (Abs/0.1 mm) and multiplying the
result by 100, yielding a result in units of Abs/cm. This allows
for numerical results in a typical range of 0 Abs ⁄cm to
100 Abs ⁄cm.
15.1.2 In the following we provide examples for each of the
five (5) properties detailed in 15.1.1:
15.1.2.1 Oxidation Example—Fig. 1 presents a schematic
illustration of the calculation for the oxidation property. In this
case, the average value of absorbance in the oxidation mea-
surement region is approximately 0.1216 Abs/0.1 mm, and the
baseline average is -0.005 Abs/0.1 mm. This yields an oxida-
tion value of 16 Abs/0.1 mm:
Oxidation = 130 · ~ 0.1216! 2 38.5 · ~ 2 0.005! 5 16 @ Abs/0.1 mm#
(6)
15.1.2.2 Antiwear Additive Example—Fig. 2 presents a
schematic illustration of the calculation for the antiwear
additive property. In this case, the average value of absorbance
in the antiwear additive measurement region is approximately
0.385 Abs/0.1 mm, and the baseline averages are 0.298 Abs/0.1
mm and 0.165 Abs/0.1 mm for the low and high frequency
baselines, respectively. This yields an antiwear additive value
of 20.7 Abs/0.1 mm:
FIG. 1 Illustration of Oxidation Measurement as Specified in Table 2
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Antiwear Additive 5 65 · ~ 0.385! 2 8.4 · ~ 0.298! 2 10.8 · ~ 0.165!
5 20.7 @ Abs/0.1 mm# (7)
15.1.2.3 Sulfation Example—Fig. 3 presents a schematic
illustration of the calculation for the sulfation property. In this
case, the average value of absorbance in the sulfation measure-
ment region is approximately 0.258 Abs/0.1 mm, and the
baseline averages are 0.168 Abs/0.1 mm and 0.285 Abs/0.1 mm
for the low and high frequency baselines, respectively. This
yields a sulfation value of 11.5 Abs/0.1 mm:
Sulfation 5 60 · ~ 0.258! 2 11 · ~ 0.285! 2 5 · ~ 0.168!
5 11.5 @ Abs/0.1 mm# (8)
15.1.2.4 Nitration Example—Fig. 4 presents a schematic
illustration of the calculation for the nitration property. In this
case, the absorbance at 1630 cm-1 is 0.246 Abs/0.1 mm, and the
baseline averages are 0.22 Abs/0.1 mm and 0.004 Abs/0.1 mm
for the low and high frequency baselines, respectively. This
yields a nitration value of 5 Abs/cm:
Nitration 5 100 · ~ 0.246 2 0.89 · ~ 0.22! 2 0.11 · ~ 0.004!!
5 5 @ Abs/cm# (9)
15.1.2.5 Soot Example—Fig. 5 presents a schematic illus-
tration of the calculation of soot. In this case, the absorbance at
2000 cm-1 is 0.31 Abs/0.1 mm. Multiplying this value by 100
we obtain a soot value of 31 Abs/cm:
Soot 5 100 · ~ 0.31! 5 31 @ Abs/cm# (10)
15.1.3 These methods are chosen so as to give the user a
reported value which does not rely on any spectral reference.
This is in keeping with the apparatus being used as a field tool.
15.1.4 Limits for each particular fluid of interest may be
tailored considering the typical range of that particular fluid.
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 D7889 − 21

FIG. 2 Illustration of Antiwear Additive Measurement as Specified in Table 2

FIG. 3 Illustration of Sulfation Measurement as Specified in Table 2

16. Report
16.1 Properties are calculated as described in Section 15 and
reported in units as described in Table 2.
16.2 Trending and Alarm Limits—As defined by the user,
the apparatus will acquire, report, and log the fluid measured
properties on a periodic basis. The user may monitor this
trending behavior and as well set alarm limits in the apparatus
for each particular fluid being analyzed. Guidance on perform-
ing trending analysis and setting alarm limits on in-service
lubricants is provided in Guide D7669 and Guide D7720.
16.3 Effects of Fluid Formulation—For each measured
property, the reported values as well as the trending tendencies
are in general different for each fluid type. The apparatus may
be designed so that each fluid type may be tracked separately
with trend histories being viewed and alarm limits set on the
apparatus per these fluid types.

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FIG. 4 Illustration of Nitration Measurement as Specified in Table 2

FIG. 5 Illustration of Soot Measurement as Specified in Table 2

17. Precision and Bias analysis of the data; the details are given in ASTM Research
17.1 The precision of this test method is based on an Report RR:D02-2021.3
interlaboratory study conducted in 2021. Seven laboratories
tested 18 different materials. Every “test result” represents an
individual determination. Each laboratory was asked to submit 3
Supporting data have been filed at ASTM International Headquarters and may
two replicate test results, from a single operator, for each be obtained by requesting Research Report RR:D02-2021. Contact ASTM Customer
material. Practice E691 was followed for the design and Service at service@astm.org.

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17.1.1 Repeatability Limit (r)—The value below which the R 5 0.0011x 2 2 0.0464x13.2305 ~Soot! (20)
absolute difference between two individual test results obtained
where:
under repeatability conditions may be expected to occur with a
probability of approximately 0.95 (95 %). x = the average of two test results.
17.1.1.1 Repeatability limits are estimated by the equations: NOTE 1—Practice E691 does not provide a standardized methodology
to arrive at equations describing the relationship between precision versus
r 5 20.0002x 2 10.0233x10.1082 ~Oxidation! (11) level. These equations are an empirical fit of the data.
2
r 5 0.0002x 2 0.0043x10.5079 ~Nitration! (12) 17.1.3 Precision Data—Tables 3 and 4 list the precision
r 5 0.0018x 2 2 0.0895x11.4689 ~Sulfation! (13) data obtained for specific samples from the interlaboratory
study.
r 5 0.023x10.1254 ~Antiwear Additive! (14)
17.1.4 The above terms (repeatability limit and reproduc-
2
r 5 0.0003x 2 0.0074x10.2494 ~Soot! (15) ibility limit) are used as specified in Practice E177.
where: 17.1.5 Any judgment in accordance with statements 17.1.1
x = the average of two test results. and 17.1.2 would have an approximate 95 % probability of
being correct.
17.1.2 Reproducibility Limit (R)—The value below which
the absolute difference between two test results obtained under 17.2 Bias—The values obtained for each procedure in this
reproducibility conditions may be expected to occur with a test method are defined only in terms of the test method. There
probability of approximately 0.95 (95 %). has been no bias established for comparison with the FTIR test
17.1.2.1 Reproducibility limits are estimated by the equa- methods listed in 4.1.1.1.
tions:
18. Keywords
R 5 0.0004x 2 10.1442x 2 0.6922 ~Oxidation! (16)
R 5 0.003x 2 2 0.0585x12.8061 ~Nitration! (17)
18.1 antiwear additives; condition monitoring; direct trend-
ing; field-based devices; grating spectrometers; handheld de-
R 5 0.0016x 2 10.0215x10.7229 ~Sulfation! (18) vices; infrared spectroscopy; in-service fluid analysis; multi-
R 5 0.0918x10.0917 ~Antiwear Additive! (19) variate analysis; nitration; oxidation; soot; sulfation

TABLE 3 Calculated Repeatability (r) of Mean ILS Sample Results

Antiwear Additive Oxidation Nitration Sulfation Soot
Abs/ 0.1 mm Abs / 0.1 mm Abs / cm Abs / 0.1 mm Abs / cm
ILS sample
Oil Provenance mean r mean r mean r mean r mean r
#
18 Mineral-based Steam Turbine 7.6 0.2 1.5 0.8 2.5 0.2 10.0 2.3 –6.7 0.2
11 Synthetic Hydraulic 6.8 0.2 1.3 0.1 2.6 0.4 7.0 0.6 –5.9 0.2
14 Gear - Wind Turbine 8.5 0.2 1.4 0.2 -1.0 0.4 7.3 0.1 –6.5 0.2
17 Synthetic Air Compressor 40.5 0.7 88.8 0.8 -29.6 0.8 44.6 0.9 –4.7 0.2
16 Synthetic Hydraulic 30.3 1.4 43.5 2.2 -3.1 0.6 86.0 11.0 –5.0 0.4
3 Gasoline Engine - Auto Garage 16.8 0.3 32.9 0.4 34.3 0.6 40.0 0.6 –3.7 0.1
4 Gasoline Engine - Auto Garage 16.4 0.4 18.3 0.2 5.9 0.6 21.3 0.2 –6.0 0.6
5 Gasoline Engine - Auto Garage 16.4 0.4 31.9 0.5 21.3 0.5 36.3 0.5 –4.7 0.3
8 Gasoline Engine - Auto Garage -
14.4 0.4 22.5 0.5 25.6 0.3 30.0 0.7 –5.9 0.2
High Mileage
12 Gasoline Engine - Specialised Base 29.9 0.7 55.8 0.6 5.0 0.2 85.8 2.9 –5.3 0.3
6 Diesel Engine - On Highway 16.0 0.3 10.8 0.3 -0.3 0.3 17.8 0.3 –6.6 0.2
7 Diesel Engine - On Highway 14.6 0.4 25.3 0.6 41.6 0.8 30.6 0.7 –6.0 0.6
10 Diesel Engine - Railroad 16.7 0.4 15.3 0.2 7.3 0.5 20.9 0.2 9.9 0.1
9 Diesel Engine - City Public Transit 12.3 0.5 11.2 0.2 0.4 0.4 18.2 0.3 15.4 0.3
2 Diesel Engine - City Public Transit 17.0 1.0 15.0 0.2 6.8 0.7 20.9 0.2 22.5 0.3
1 Diesel Engine - City Public Transit 17.1 0.4 14.9 0.1 6.6 0.7 21.3 0.3 36.1 0.3
15 Diesel Engine - City Public Transit
17.5 0.8 15.1 0.8 6.1 0.8 21.8 0.6 51.7 0.7
(high soot)
13 Diesel Engine - City Public Transit
17.5 0.9 14.6 0.3 5.8 0.9 21.6 0.3 66.8 1.1
(high soot)

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TABLE 4 Calculated Reproducibility (R) of Mean ILS Sample Results
Antiwear Additive Oxidation Nitration Sulfation Soot
Abs / 0.1 mm Abs / 0.1 mm Abs / cm Abs / 0.1 mm Abs / cm
ILS sample Oil Provenance
mean R mean R mean R mean R mean R
#
18 Mineral-based Steam Turbine 7.6 0.6 1.5 0.9 2.5 1.6 10.0 2.8 –6.7 3.8
11 Synthetic Hydraulic 6.8 0.6 1.3 0.4 2.6 1.6 7.0 0.9 –5.9 3.1
14 Gear - Wind Turbine 8.5 0.9 1.4 0.5 -1.0 2.4 7.3 0.9 –6.5 3.8
17 Synthetic Air Compressor 40.5 3.9 88.8 14.3 -29.6 7.8 44.6 7.9 –4.7 3.3
16 Synthetic Hydraulic 30.3 2.5 43.5 9.9 -3.1 3.7 86.0 13.5 –5.0 3.5
3 Gasoline Engine - Auto Garage 16.8 1.3 32.9 3.4 34.3 4.4 40.0 3.5 –3.7 3.5
4 Gasoline Engine - Auto Garage 16.4 1.5 18.3 1.4 5.9 4.0 21.3 1.7 –6.0 3.6
5 Gasoline Engine - Auto Garage 16.4 1.4 31.9 2.4 21.3 6.0 36.3 2.8 –4.7 3.7
Gasoline Engine - Auto Garage -
8 14.4 1.0 22.5 1.5 25.6 3.7 30.0 2.2 –5.9 3.7
High Mileage
12 Gasoline Engine - Specialised Base 29.9 2.8 55.8 11.9 5.0 3.1 85.8 14.4 –5.3 3.4
6 Diesel Engine - On Highway 16.0 1.3 10.8 0.9 -0.3 2.1 17.8 1.5 –6.6 3.2
7 Diesel Engine - On Highway 14.6 1.2 25.3 1.7 41.6 4.3 30.6 2.1 –6.0 3.8
10 Diesel Engine - Railroad 16.7 1.2 15.3 1.0 7.3 2.1 20.9 1.5 9.9 2.7
9 Diesel Engine - City Public Transit 12.3 1.5 11.2 1.2 0.4 2.3 18.2 1.4 15.4 2.8
2 Diesel Engine - City Public Transit 17.0 1.6 15.0 1.1 6.8 2.3 20.9 1.6 22.5 2.6
1 Diesel Engine - City Public Transit 17.1 1.8 14.9 1.1 6.6 1.9 21.3 1.7 36.1 3.2
Diesel Engine - City Public Transit
15 17.5 2.6 15.1 1.4 6.1 2.4 21.8 1.7 51.7 3.9
(high soot)
Diesel Engine - City Public Transit
13 17.5 3.0 14.6 1.2 5.8 2.4 21.6 1.7 66.8 5.2
(high soot)

SUMMARY OF CHANGES

Subcommittee D02.96.03 has identified the location of selected changes to this standard since the last issue
(D7889 – 13) that may impact the use of this standard. (Approved July 1, 2021.)

(1) Added Practices E177 and E691 to Section 2. (2) Replaced Section 17 with new Precision and Bias data.

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