Designation: D 893 – 97 An American National Standard

Standard Test Method for

Insolubles In Used Lubricating Oils1
This standard is issued under the fixed designation D 893; 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.
This standard has been approved for use by agencies of the Department of Defense.
This test method has been adopted for use by government agencies to replace Method D 3121 of Federal Test Method Standard No.
791b.

1. Scope
Petroleum Products3
1.1 This test method covers the determination of pentane
and toluene insolubles in used lubricating oils. 3. Terminology
1.2 Procedure A covers the determination of insolubles 3.1 Definitions:
without the use of coagulant in the pentane. It provides an 3.1.1 coagulate, v—to cause to become viscous or thick-
indication of the materials that can readily be separated from ened into a coherent mass.
the oil-solvent mixtures by centrifuging. 3.1.2 coagulated pentane insolubles, n—in used oil analy-
1.3 Procedure B covers the determination of insolubles in sis, separated matter that results when a coagulant is added to
oils containing detergents and employs a coagulant for both a solution of used oil in pentane.
the pentane and toluene insolubles. In addition to the materials 3.1.2.1 Discussion—The addition of a coagulant will aid in
separated by using Procedure A, this coagulation procedure separating finely divided materials that may have been held in
separates some finely divided materials that may be suspended suspension because of the dispersant characteristics of the oil.
in the oil. 3.1.3 coagulated toluene insolubles, n—in used oil
1.4 The values stated in acceptable SI units are to be analysis, coagulated and separated matter not soluble in
regarded as the standard. pentane or toluene.
NOTE 1—Results obtained by Procedures A and B should not be 3.1.4 pentane insolubles, n— in used oil analysis, separated
compared since they usually give different values. The same procedure matter resulting when a used oil is mixed with pentane.
should be employed when comparing values obtained periodically on an 3.1.4.1 Discussion—In this test method, the separation is
oil in use or when comparing results determined by two or more effected by centrifugation.
laboratories. 3.1.5 toluene insolubles, n— in used oil analysis, the
1.5 This standard does not purport to address all of the portion of pentane insolubles not soluble in toluene.
safety concerns, if any, associated with its use. It is the 3.1.6 used oil, n—any oil that has been in a piece of
responsibility of the user of this standard to establish appro- equipment (for example, an engine, gearbox, transformer, or
priate safety and health practices and determine the applica- turbine), whether operated or not.
bility of regulatory limitations prior to use. For specific 3.1.6.1 Discussion—In this test method, the oil can be any
precautionary statements, see 7.7, 7.8, 7.9, 9.1, and 9.7. oil that has been used for lubrication.
3.2 Definitions of Terms Specific to This Standard:
2. Referenced Documents 3.2.1 insoluble resins, n— in used oil analysis, separated
2.1 ASTM Standards: matter soluble in toluene but not pentane.
D 1193 Specification for Reagent Water2 3.2.1.1 Discussion—Insoluble resins can be calculated for
D 4057 Practice for Manual Sampling of Petroleum and either Procedue A or B by subtracting the toluene insolubles
Petroleum Products3 from the pentane insolubles.
D 4175 Terminology Relating to Petroleum, Petroleum
Products, and Lubricants3 4. Summary of Test Method
D 4177 Practice for Automatic Sampling of Petroleum and 4.1 Procedure A— A representative sample of used lubri-
cating oil is mixed with pentane and centrifuged. The oil
1
solution is decanted and the precipitate washed twice with
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee pentane, dried, and weighed to give the pentane insolubles.
D02.06 on Analysis of Lubricants. For toluene insolubles a separate sample of the oil is mixed
Current edition approved Dec. 10, 1997. Published February 1998. Originally with pentane and then centrifuged. The precipitate is washed
issued as D 893 – 67. Last previous edition D 893 – 92.
2
Annual Book of ASTM Standards, Vol 11.01. twice with pentane, once with toluene-alcohol solution, and
3
Annual Book of ASTM Standards, Vol 05.02. once with toluene. The insoluble material is then dried and
weighed

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 D 893
to give the insolubles. centrifuge is in motion. The
4.2 Procedure B— A representative sample of used lubri-
cating oil is mixed with pentane-coagulant solution and cen-
trifuged. The precipitate is washed twice with pentane, dried,
and weighed to give coagulated pentane insolubles. For
coagu- lated toluene insolubles a separate sample of the oil is
mixed with pentane-coagulant solution and centrifuged. The
precipi- tate is washed twice with pentane, once with toluene-
alcohol solution, and once with toluene. The insoluble
material is then dried and weighed to give coagulated toluene
insolubles.
5. Significance and Use
5.1 Pentane insolubles can include oil-insoluble materials
and some oil-insoluble resinous matter originating from oil or
additive degradation, or both.
5.2 Toluene insoluble materials can come from (1) external
contamination, (2) fuel carbon and highly carbonized
materials from degradation of fuel, oil, and additives, or (3)
engine wear and corrosion materials.
5.3 A significant change in pentane insolubles, toluene
insolubles (with or without coagulant) and insoluble resins
indicates a change in oil which could lead to lubrication
system problems.
5.4 Insolubles measured can also assist in evaluating the
performance characteristics of a used oil or in determining the
cause of equipment failure.
6. Apparatus
6.1 Centrifuge Tube, cone-shaped, conforming to the di-
mensions given in Fig. 1, and made of thoroughly annealed
glass. The graduations, numbered as shown in Fig. 1, shall be
clear and distinct and the mouth constricted in shape for
closure with a cork. Scale error tolerances and smallest
graduations between various calibration marks are given in
Table 1 and apply to calibrations made with air-free water at

TABLE 1 Calibration Tolerances of Cone-Shaped Centrifuge Tube

Smallest Scale Maximum Scale
Range, mL
Division, mL Error, mL
0 to 0.1 0.05 60.02
Over 0.1 to 0.3 0.05 60.03
Over 0.3 to 0.5 0.05 60.05
Over 0.5 to 1.0 0.1 60.05
Over 1.0 to 2.0 0.1 60.10
Over 2.0 to 3.0 0.2 60.10
Over 3.0 to 5.0 0.5 60.20
Over 5.0 to 10.0 1.0 60.50
Over 10 to 25 5.0 61.0
Over 25 to 100 25.0 61.0

20°C.
6.2 Centrifuge, meeting all safety requirements for normal
use and capable of whirling two or more filled centrifuge
tubes at a speed that can be controlled to give a relative
centrifugal force (rcf) between 600 and 700 at the tips of the
tubes. The revolving head, trunnion rings, and trunnion cups,
including the rubber cushion, shall be soundly constructed to
withstand the maximum centrifugal force capable of being
delivered by the power source. The trunnion cups and
cushions shall firmly support the tubes when the
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 D 893

FIG. 1 ASTM Cone-Shaped Centrifuge Tube

centrifuge shall be enclosed by a metal shield or case strong

enough to eliminate danger if any breakage occurs. Calculate
the speed of the rotating head as follows:
Speed, rpm 5 1337 =rcf/d (1)
where:
rcf 5 relative centrifugal force, and
d 5 diameter swing, mm, measured between tips of
opposite tubes when in rotating position.
Table 2 shows the relationship between the diameter of
swing, ref and rpm.
6.3 Oven, explosion-proof, capable of maintaining a
tem- perature of 105 6 3°C.
6.4 Balance, having a sensitivity of 0.5 mg for weighing
the 100-mL beaker and centrifuge tube, and a balance having
a sensitivity of 0.1 g for weighing the oil sample.

7. Reagents and Solvents

7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended
that

TABLE 2 Rotation Speeds for Centrifuges of Various

Diameters of Swing
Diameter of Swing, mmA rpm at 600 rcf rpm at 700 rcf
483 1490 1610
508 1450 1570
533 1420 1530
559 1390 1500
A
Measured in millimetres between tips of opposite tubes when in rotating
position.

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 D 893
all reagents shall conform to the specifications of the Commit- MD.
tee on Analytical Reagents of the American Chemical Society,
where such specifications are available.4 Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
7.2 Purity of Water— Unless otherwise indicated
references to water shall be understood to mean water in
accordance with Specification D 1193, Type IV.
7.3 n–butyl diethanolamine (2,21– (butylimino) diethanol) (
Warning—see Note 5).
7.4 Ethanol, denatured, (Warning—see Note 3) conform-
ing to either Formula 30 or 3A of the US Bureau of Internal
Revenue.
7.5 Pentane (Warning—see Note 4).
7.6 Propan–2–ol (isopropyl alcohol), (Warning—see Note
3).
7.7 Toluene (Warning—See Note 2).
NOTE 2—Warning: Flammable. Vapor harmful.
7.8 Toluene-Alcohol Solution, wash solvent, made by mix-
ing 1 volume of toluene (7.7) with 1 volume of denatured
ethanol (Warning—See Note 3) conforming to either
Formula No. 30 or 3A of the U.S. Bureau of Internal Revenue.
NOTE 3—Warning: Flammable. Denatured. Cannot be made nontoxic.
NOTE 4—Warning: Extremely flammable. Vapors may cause flash
fires.
7.9 Pentane-Coagulant Solution—Add 50 mL of n-butyl
diethanolamine (Warning—see Note 6) and 50 mL of isopro-
pyl alcohol (2-propanol) (Warning—See Note 7) to 1 L of
n-pentane ( Warning—See Note 5) and mix.
NOTE 5—Warning: May be harmful if inhaled or swallowed.
NOTE 6—Warning: Flammable.

8. Sampling
8.1 Obtain a sample using either Practice D 4057 or D 4177.
8.2 Heat the sample of used oil to 60 6 5°C in the
original container and agitate until all sediment is
homogeneously suspended in the oil (Note 2). If the
original container is of opaque material, or if it is more than
three-fourths full, transfer the entire sample to a clear glass
bottle having a capacity at least one third greater than the
volume of the sample, and transfer all traces of sediment
from the original container to the bottle by violent agitation
of portions of the sample in the original container. After
complete suspension of all sediment, strain the sample or a
convenient aliquot through a 150-µm (No. 100) sieve to
remove large contaminating particles.
NOTE 7—As used oil may change appreciably in storage, samples
should be tested as soon as possible after removal from the lubricating
system and the dates of sampling and testing should be noted.

4
“Reagent Chemicals, American Chemical Society Specifications,” Am.
Chemi- cal Soc., Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see “Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,

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 D 893
9. Procedure A for Pentane and Toluene 9.10 Dry for1h at 105 6 3°C (Note 3), cool in a desiccator,
Insolubles Without Coagulant
Pentane Insolubles
9.1 Dry a clean centrifuge tube for 30 min at 105 6 3°C,
cool in a desiccator, and weigh to the nearest 1 mg. Weigh
10.0
6 0.1 g of the prepared sample of used oil into the tube and
fill to the 100-mL mark with pentane (Warning—See
Note 5). Stopper the tube and shake until the mixture is
homogeneous. Do not allow the mixture to stand more than
3 h.
9.2 Remove the stopper, and using a wash bottle having
a fine jet, wash all insolubles from the stopper into the
centrifuge tube with a minimum of pentane. Balance the
weights of each pair of filled centrifuge tubes, place them
in the centrifuge on opposite sides of the head, and
centrifuge for 20 6 1 min at a rate calculated in accordance
with 6.2, sufficient to produce a relative centrifugal force
(rcf) between 600 and 700 at the tips of the whirling tubes.
(See Table 2.) Carefully decant the supernatant liquid
without disturbing or dispersing the precipi- tate, leaving not
more than 3 mL of liquid in the centrifuge tube.
9.3 Add 10 6 1 mL of pentane to the tube. Dislodge and
break up all of the insolubles from the bottom of the tube
by means of a clean stiff wire. Wash all insolubles adhering
to the wire back into the tube with pentane, filling the tube
to the 50-mL mark. Stopper the tube and shake until the
mixture is homogeneous. Remove and wash the stopper.
Centrifuge for 20 6 1 min. Pour the supernatant liquid from
the centrifuge tube, using care to avoid disturbing the cake
of insolubles in the bottom of the tube.
9.4 Repeat the entire operation described in 9.3.
9.5 Dry the centrifuge tube containing the washed
precipi- tate for 30 min at 105 6 3°C, cool in desiccator,
and weigh to the nearest 1 mg.
9.6 With relatively heavy precipitates there can be some
spattering if the tube is placed directly from the centrifuge
into the oven. In such cases, the precipitate may be partially
dried by weathering at room or slightly higher temperatures
before being placed in the oven.

Toluene Insolubles
9.7 Starting with a fresh sample of used oil, precipitate and
centrifuge the pentane insolubles as described in 9.1-9.4, but
do not dry the insolubles in the centrifuge tube.
9.8 Add 10 6 1 mL of toluene-alcohol solution (See Note
2 and Note 3). Break up and dislodge all of the insolubles
from the bottom of the centrifuge tube by means of a
clean, stiff wire. Wash any insolubles adhering to the wire
back into the tube with toluene-alcohol solution, using a
sufficient amount of this solvent to fill the tube to the 50-mL
mark. Stopper the tube and shake until the mixture is
homogeneous. Remove the stopper and wash the adhering
insolubles back into the tube with a minimum amount of
toluene. Centrifuge until no visible insolubles remain in
suspension in the solvent; 10 to 20 min are usually sufficient.
Decant the clear solution, taking care not to disturb the
precipitate.
9.9 Repeat the washing procedure described in 9.7, substi-
tuting toluene for the toluene-alcohol solution.
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 D 893
and weigh to the nearest 1 mg.
0.3 0.12
10. Procedure B for Coagulated Pentane and Toluene 0.4 0.14
0.5 0.15
Insolubles 0.6 0.17
10.1 Coagulated Pentane Insolubles—Proceed in accor- 0.7 0.18
0.8 0.19
dance with 9.1 and 9.2, except in 9.1 use pentane-coagulant A
These precision data were derived as follows:
solution (7.9) in place of pentane. Wash the precipitate twice Repeatability 5 0.216 = I
with pentane, dry and weigh as directed in 9.3, 9.4, and 9.5. where I 5 toluene insolubles or coagulated toluene insolubles.
10.2 If the sample is known to contain water, or if water 13.1.2 Reproducibility— The difference between two,
is indicated by a gummy precipitate, repeat the determination single and independent results obtained by different operators
on a sample that has been dried by heating to 105 6 3°C in working in different laboratories on identical test material
an open beaker. would, in the long run, and in the normal and correct operation
10.3 Coagulated Toluene Insolubles—Proceed in accor- of the test method, exceed the following values only in one
dance with 9.1 and 9.2 except in 9.1 use pentane-coagulant case in twenty:
solution (7.9) in place of pentane. Wash twice with pentane as 13.1.2.1 Procedure A, pentane insolubles, and Procedure B,
directed in 9.3 and 9.4. Wash with toluene-alcohol solution coagulated pentane insolubles:
and toluene, dry, and weigh as directed in 9.7-9.9. Insolubles, % Reproducibility, Same Units
0.0 to 1.0 0.10
11. Calculation over 1.0 15 % of mean

11.1 Calculate the percentage of insolubles in the used oil 13.1.2.2 Procedure A, toluene insolubles:
Average Insolubles, % Reproducibility, Same UnitsA
as follows: 0.1 0.14
Insolubles, % 5 10 ~B 2 A! (2) 0.2 0.20
0.3 0.24
0.4 0.28
where: 0.5 0.31
A 5 mass of clean, dried, centrifuge tube, g, and 0.6 0.34
B 5 mass of dried insolubles and centrifuge tube, g. 0.7 0.37
0.8 0.39
0.9 0.42
12. Report 1.0 0.44
12.1 If Procedure A (Section 9) was employed, report the 1.1 0.46
percentages of pentane insolubles and toluene insolubles.
A
These precision data were derived as follows:
Reproducibility 5 0.441 = IA
12.2 If Procedure B (Section 10) was employed, report the where IA 5 toluene insolubles.
percentages of coagulated pentane insolubles and coagulated 13.1.2.3 Procedure B, coagulated toluene insolubles (see
toluene insolubles. Note 8):
12.3 Insoluble resins or coagulated insoluble resins may be Average Insolubles, % Reproducibility, Same UnitsA
reported for either Procedure A or B, respectively, by subtract- 0.1 0.30
ing toluene insolubles from pentane insolubles. 0.2 0.43
0.3 0.53
0.4 0.60
13. Precision and Bias 0.5 0.68
0.6 0.74
13.1 Precision—The following criteria should be used for 0.7 0.80
judging the acceptability of results (95 % confidence): 0.8 0.86
13.1.1 Repeatability— The difference between successive 0.9 0.91
1.0 0.96
test results, obtained by the same operator with the same 1.1 1.00
apparatus under constant operating conditions on identical test A
These precision data were derived as follows:
material would, in the long run, and in the normal and correct Reproducibility 5 0.957 = IB
operation of the test method, exceed the following values only where IB 5 coagulated toluene insolubles.
in one case in twenty:
NOTE 8—The poor interlaboratory precision (reproducibility) of this
13.1.1.1 Procedure A, pentane insolubles, and Procedure B, portion of this test is such that Procedure B coagulated toluene
coagulated pentane insolubles: insolubles, is unsuitable for the purpose of comparison of interlaboratory
Insolubles, % Repeatability, Same Units results.
0.0 to 1.0 0.07
Over 1.0 10 % of mean 13.2 Bias—The procedure in this test method has no bias
because the mass percent of insoluble materials can only be
13.1.1.2 Procedure A, toluene insolubles, and Procedure B,
defined in terms of this test method.
coagulated toluene insolubles:
Average Insolubles, % Repeatability, Same UnitsA 14. Keywords
0.1 0.068
0.2 0.097 14.1 insoluble resins; insolubles; lubricating oil; used; pen-
tane insolubles; toluene insolubles

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 D 893
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