An American National Standard

Designation: D 7317 – 07

Standard Test Method for

Coagulated Pentane Insolubles in Used Lubricating Oils by
Paper Filtration (LMOA Method)1
This standard is issued under the fixed designation D 7317; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope D 4057 Practice for Manual Sampling of Petroleum and

1.1 This test method covers the determination of coagulated Petroleum Products
pentane insolubles in used lubricating oils by a paper filtration D 4175 Terminology Relating to Petroleum, Petroleum
method. Products, and Lubricants
1.2 This test method was originally developed by the Fuels, D 4177 Practice for Automatic Sampling of Petroleum and
Lubricants, and Environmental Committee (FL&E) of the Petroleum Products
Locomotive Maintenance Officer’s Association (LMOA).2 D 5967 Test Method for Evaluation of Diesel Engine Oils in
1.3 This test method is used primary for testing used diesel T-8 Diesel Engine
engine oils from railroad locomotive service. It may be applied
3. Terminology
to other samples types but precision, bias, and significance
have not been determined for samples other than used railroad 3.1 Definitions:
locomotive diesel engine oils. 3.1.1 coagulate, v—to cause to become viscous or thick-
1.4 This test method, in general, does not correlate with Test ened into a coherent mass. D 4175
Method D 893 on Insolubles in Lubricating Oils, since it uses 3.1.2 coagulated pentane insolubles, n—in used oil analy-
separation by centrifugation and a more concentrated solution sis, separated matter that results when a coagulant is added to
of anti-coagulant. a solution of used oil in pentane. D 4175
1.5 The correlation between this test method and Appendix 3.1.2.1 Discussion—The addition of a coagulant will aid in
A4 (Enhanced Thermal Gravimetric Analysis (TGA) Proce- separating finely divided materials that may have been held in
dure) in Test Method D 5967 has not been investigated. suspension because of the dispersant characteristics of the oil.
1.6 The values stated in SI units are to be regarded as the 3.1.2.2 Discussion—This test method uses a 1 % coagulant
standard. The values given in parentheses are for information solution. Test Method D 893 uses a 5 % coagulant solution.
only. 3.1.3 membrane filter, n—porous article of closely con-
1.7 This standard does not purport to address all of the trolled pore size through which a liquid is passed to separate
safety concerns, if any, associated with its use. It is the matter in suspension. D 4175
responsibility of the user of this standard to establish appro- 3.1.4 pentane insolubles, n—in used oil analysis, separated
priate safety and health practices and determine the applica- matter resulting when a used oil is dissolved in pentane.
bility of regulatory limitations prior to use. For specific D 4175
warning statements, see 7.2, 7.3, and 7.4. 3.1.4.1 Discussion—In this test method, the separation is
effected by paper filtration.
2. Referenced Documents 3.1.5 used oil, n—any oil that has been in a piece of
2.1 ASTM Standards: 3 equipment (for example, an engine, gearbox, transformer, or
D 893 Test Method for Insolubles in Used Lubricating Oils turbine), whether operated or not. D 4175
3.1.5.1 Discussion—In this test method, the oil can be any
oil that has been used for lubrication of a locomotive diesel
1
This test method is under the jurisdiction of ASTM Committee D02 on engine, whether engaged in railroad or other service.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 3.2 Definitions of Terms Specific to This Standard:
D02.06 on Analysis of Lubricants.
Current edition approved July 1, 2007. Published August 2007. Originally 3.2.1 locomotive diesel engine oil, n—lubricating oil formu-
approved in 2006. Last previous edition approved in 2006 as D 7317–06. lated to meet the chemical, physical, and performance require-
2
Locomotive Maintenance Officer’s Association (LMOA), 6047 South Mobile ments defined by the LMOA for service in diesel engines in
Avenue, Chicago, IL 60638.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
railroad locomotives.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 3.3 Acronyms:
Standards volume information, refer to the standard’s Document Summary page on 3.3.1 ILS—interlaboratory study
the ASTM website.

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

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 D 7317 – 07
3.3.2 LMOA—Locomotive Maintenance Officer’s Associa- sufficiently high purity to permit its use without lessening the
tion accuracy of the determination. If industrial grade pentane is
3.3.3 RR—railroad used, it shall be filtered using 0.45 µm filter paper.
3.3.4 TGA—thermo-gravimetric analysis 7.2 n–butyl diethanolamine (2,2’– (butylimino) diethanol),
98 %. (Warning—May be harmful if inhaled or swallowed.)
4. Summary of Test Method 7.3 Pentane (n-pentane), 98 %. (Warning—Extremely
4.1 A representative sample of used lubricating oil is mixed flammable. Vapors may cause flash fires.)
with pentane-coagulant solution and filtered under vacuum. 7.4 Pentane-Coagulant Solution, 1 %—Add 5 mL of
The filter is washed with pentane, dried, and weighed to give n-butyl diethanolamine (Warning—Flammable.) to 500 mL of
coagulated pentane insolubles. n-pentane (Warning—May be harmful if inhaled or swal-
lowed.) and mix. Solution shall be used within one month and
5. Significance and Use should preferably be made within a week of using.
5.1 Coagulated pentane insolubles can include oil-insoluble
materials, some oil-insoluble resinous matter originating from 8. Sampling
oil or additive degradation, soot from incomplete diesel fuel 8.1 Obtain a sample using either Practice D 4057 or D 4177.
combustion, or a combination of all three. 8.2 Heat the sample of used oil to 50 6 5°C for 1⁄2 h 6 5
5.2 A significant change in coagulated pentane insolubles min in the original container and agitate until all sediment is
indicates a change in oil, and this could lead to lubrication homogeneously suspended in the oil. If the original container is
system problems. of opaque material, or if it is more than three-fourths full,
5.3 Coagulated pentane insolubles measurements can also transfer the entire sample to a clear glass bottle having a
assist in evaluating the performance characteristics of a used capacity at least one third greater than the volume of the
oil or in determining the cause of equipment failure. sample, and transfer all traces of sediment from the original
5.4 High values of coagulated pentane insolubles have been container to the bottle by vigorous agitation of portions of the
associated with plugged oil filters, leading to opening of the sample in the original container.
bypass valve and circulation of unfiltered oil in the engine. This
can lead to increased piston deposits, increased bearing wear, 9. Procedure
and premature engine failure. 9.1 Dry a clean filter membrane for 15 min in a desiccator,
place in a labeled aluminum weighing dish, and weigh to the
6. Apparatus (see Fig. 1) nearest 0.1 mg.
6.1 Smooth-tip Forceps. 9.2 Place a 50 mL graduated cylinder on the balance, and
6.2 Graduated Cylinder, 50 mL with stopper. tare it.
6.3 Oven, explosion-proof, capable of maintaining a tem- 9.3 Remove the oil from the oven. Vigorously shake the
perature of 50 6 3°C. sample by hand for a minimum of 30 s.
6.4 Oven, explosion-proof, capable of maintaining a tem- 9.4 Using a medicine dropper, weigh approximately 0.25 g
perature of 100 6 3°C. of oil sample into the graduated cylinder. Record the weight to
6.5 Filtering Flask, 1 L. the nearest 0.1 mg.
6.6 Filter Holders, borosilicate glass. 9.5 Add 10 mL pentane and agitate gently until the oil
6.7 Filter Membrane, 0.45 µm. sample is fully dissolved.
6.8 Weighing Dish, aluminum. 9.6 Bring the volume in the graduated cylinder up to the 50
6.9 Balance, capable of weighing to the nearest 0.0001 g mL mark with fresh 1 % coagulant solution. Stopper and shake
(0.1 mg) with a range of 160 g. gently, inverting the graduated cylinder four times in 4 to 5 s.
6.10 Vacuum, capable of maintaining 50.653 kPa (15 in. Allow to stand for 30 min. Shake the solution similarly every
Hg) minimum. 10 min of the 30 min.
6.11 Stopwatch or Other Timing Device, capable of measur- 9.7 Mount the filter on a dry holder and apply a vacuum.
ing to the nearest 0.1 s with a range of at least 5 min. Mount and securely clamp the filter funnel to the filter holder.
Ensure a minimum vacuum of 50.653 kPa (15 in. Hg) is
7. Reagents and Solvents attained and held.
7.1 Purity of Reagents—Reagent grade chemicals shall be 9.8 Shake the sample gently one last time, pour into the
used in all tests. Unless otherwise indicated, it is intended that filter funnel, and using the stopwatch or other timing device
all reagents shall conform to the specifications of the Commit- immediately start timing the flow rate.
tee on Analytical Reagents of the American Chemical Society, 9.9 Rinse the graduated cylinder twice using a minimum of
where such specifications are available.4 Other grades may be 35 mL pentane and pour the rinsings into the filter funnel.
used, provided it is first ascertained that the reagent is of 9.10 Stop timing when the last of the free liquid on the filter
disappears. Record the flow time to the nearest second.
9.11 If filter flow time exceeds 5 min, re-run 9.4 to 9.10 with
4
Reagent Chemicals, American Chemical Society Specifications, Am. Chemical 0.1 mg sample.
Soc., Washington, DC. For suggestions on the testing of reagents not listed by the
American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH
9.12 Rinse the funnel wall with pentane from a squirt bottle.
Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National 9.13 Remove the filter funnel from the filter holder and rinse
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD. the filter membrane with a stream of pentane from the squirt

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 D 7317 – 07

FIG. 1 Paper Filtration Apparatus

bottle. Ensure the edges of the filter funnel are rinsed well to 9.15 Remove the weighing dish and filter membrane and
remove any oil trapped beneath the funnel. cool to room temperature in a dessicator for a minimum of 1 h.
9.14 Release the vacuum, and using the smooth-tip forceps 9.16 Weigh the filter membrane and weighing dish and
transfer the filter membrane to its original weighing dish, and record the stabilized weight to the nearest 0.1 mg.
dry in the oven at 100 6 3°C for 1 h 6 5 min.

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 D 7317 – 07
TABLE 1 Calculated Precision at Selected Insolubles Levels 12.1.1 Repeatability—The difference between successive
Insolubles Result, Repeatability, Reproducibility, test results, obtained by the same operator with the same
% % (same units) % (same units)
apparatus under constant operating conditions on identical test
0.00 0.11 0.42 material would, in the long run, and in the normal and correct
0.20 0.12 0.47
0.40 0.13 0.51 operation of the test method, exceed the following values only
0.60 0.14 0.56 in one case in twenty:
0.80 0.16 0.61
1.0 0.17 0.66 0.061*~x 1 1.77! (2)
1.5 0.20 0.77
2.0 0.23 0.89 where:
2.5 0.26 1.0
3.0 0.29 1.1
x = average of the two results.
3.5 0.32 1.2 12.1.2 Reproducibility—The difference between two single
4.0 0.35 1.4
4.5 0.38 1.5
and independent results obtained by different operators work-
5.0 0.41 1.6 ing in different laboratories on identical test material would, in
the long run, and in the normal and correct operation of the test
method, exceed the following values only in one case in
10. Calculation twenty:
10.1 Calculate the percent coagulated pentane insolubles in 0.237*~x 1 1.77! (3)
the used oil as follows:
~A – B!
where:
I 5 100 C (1) x = average of the two results.
NOTE 1—Precision is finite at a determined value of zero. Since the
where:
result of this test method is the difference of two weight determinations,
I = coagulated pentane insolubles, %,
it is possible to obtain negative numbers for a blank sample (true zero
A = mass of filter and deposit, mg,
result) due to random weighing errors.
B = mass of filter, mg, and
C = mass of oil sample, mg. 12.1.3 Calculated repeatability and reproducibility at se-
lected insolubles values are given in Table 1.
11. Report
12.2 Bias—The procedure in this test method has no bias
11.1 Report the percentage of coagulated pentane insolubles
because the mass percent of insoluble materials can only be
to two significant figures.
defined in terms of this test method.
12. Precision and Bias 12.3 Relative Bias—Agreement between the results of this
12.1 Precision—The precision of this test method was test method and those from Test Method D 893 has not been
determined from the statistical analysis of an interlaboratory investigated. In general, the two test methods are not expected
study (ILS), comprising six used railroad diesel engine oils to correlate.
measured four times each in 12 laboratories.5
13. Keywords
5
Supporting data have been filed at ASTM International Headquarters and may 13.1 diesel; filtration; insolubles; LMOA; lubricating oil;
be obtained by requesting Research Report RR: D02–1610. pentane insolubles; used

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 D 7317 – 07

APPENDIX

(Nonmandatory Information)

X1. TROUBLESHOOTING GUIDE

X1.1 During the development of the test method, a number edge of the insolubles, or a blotchy surface appearance that is
of observations were made that helped operators recognize tacky.
problems. These are described below.
X1.4 In humid climates (>65 % relative humidity), the
X1.2 Repeatability was found to be best if the samples
cooling caused by pentane evaporation may cause frost to form
filtered in less than 5 min. With extended filter times, the
on both the filter and inside the holder while rinsing. If this
weights tend to be high, since the insolubles on blocked filters
happens, remove the filter after rinsing and dry for at least 1 h
cannot be rinsed enough to remove oil and coagulant residue.
in a 100°C oven. An oven or compressed air may be used to
X1.3 Residual coagulant will give high results. The follow- thoroughly dry out a holder. Warm the dried filter holders on
ing were found to indicate the presence of residual coagulant: top of the oven until ready for use. Avoid using any holder that
curling of the filter edges with drying, a yellow ring around the is still hot or damp.

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