An American National Standard

Designation: D 893 – 05a

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.

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

1.1 This test method covers the determination of pentane Petroleum Products
and toluene insolubles in used lubricating oils. D 4177 Practice for Automatic Sampling of Petroleum and
1.2 Procedure A covers the determination of insolubles Petroleum Products
without the use of coagulant in the pentane. It provides an 3. Terminology
indication of the materials that can readily be separated from
the oil-solvent mixtures by centrifuging. 3.1 Definitions:
1.3 Procedure B covers the determination of insolubles in 3.1.1 coagulate, v—to cause to become viscous or thick-
oils containing detergents and employs a coagulant for both the ened into a coherent mass.
pentane and toluene insolubles. In addition to the materials 3.1.2 coagulated pentane insolubles, n—in used oil analy-
separated by using Procedure A, this coagulation procedure sis, separated matter that results when a coagulant is added to
separates some finely divided materials that may be suspended a solution of used oil in pentane.
in the oil. 3.1.2.1 Discussion—The addition of a coagulant will aid in
separating finely divided materials that may have been held in
NOTE 1—Results obtained by Procedures A and B should not be suspension because of the dispersant characteristics of the oil.
compared since they usually give different values. The same procedure
3.1.3 coagulated toluene insolubles, n—in used oil analysis,
should be employed when comparing values obtained periodically on an
oil in use or when comparing results determined by two or more coagulated and separated matter not soluble in pentane or
laboratories. toluene.
3.1.4 pentane insolubles, n—in used oil analysis, separated
1.4 The values stated in SI units are to be regarded as
matter resulting when a used oil is mixed with pentane.
standard. No other units of measurement are included in this
3.1.4.1 Discussion—In this test method, the separation is
standard.
effected by centrifugation.
1.5 This standard does not purport to address all of the
3.1.5 toluene insolubles, n—in used oil analysis, the portion
safety concerns, if any, associated with its use. It is the
of pentane insolubles not soluble in toluene.
responsibility of the user of this standard to establish appro-
3.1.6 used oil, n—any oil that has been in a piece of
priate safety and health practices and determine the applica-
equipment (for example, an engine, gearbox, transformer, or
bility of regulatory limitations prior to use. For specific
turbine), whether operated or not.
warning statements, see Section 7 and 9.1.1.
3.1.6.1 Discussion—In this test method, the oil can be any
2. Referenced Documents oil that has been used for lubrication.
3.2 Definitions of Terms Specific to This Standard:
2.1 ASTM Standards: 2
3.2.1 insoluble resins, n—in used oil analysis, separated
D 1193 Specification for Reagent Water
matter soluble in toluene but not pentane.
3.2.1.1 Discussion—Insoluble resins can be calculated for
1
either Procedure A or B by subtracting the toluene insolubles
This test method is under the jurisdiction of ASTM Committee D02 on from the pentane insolubles.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.06 on Analysis of Lubricants.
Current edition approved Nov. 1, 2005. Published November 2005. Originally
4. Summary of Test Method
approved in 1967. Last previous edition approved in 2005 as D 893–05.
2
4.1 Procedure A—A representative sample of used lubricat-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ing oil is mixed with pentane and centrifuged. The oil solution
Standards volume information, refer to the standard’s Document Summary page on is decanted and the precipitate washed twice with pentane,
the ASTM website. dried, and weighed to give the pentane insolubles. For toluene

*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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 D 893 – 05a
insolubles, a separate sample of the oil is mixed with pentane
and then centrifuged. The precipitate is washed twice with
pentane, once with toluene-alcohol solution, and once with
toluene. The insoluble material is then dried and weighed to
give the insolubles.
4.2 Procedure B—A representative sample of used lubricat-
ing oil is mixed with pentane-coagulant solution and centri-
fuged. The precipitate is washed twice with pentane, dried, and
weighed to give coagulated pentane insolubles. For coagulated
toluene insolubles a separate sample of the oil is mixed with
pentane-coagulant solution and centrifuged. The precipitate 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.
FIG. 1 ASTM Cone-Shaped Centrifuge Tube
5.4 Insolubles measured can also assist in evaluating the
performance characteristics of a used oil or in determining the
TABLE 1 Calibration Tolerances of Cone-Shaped Centrifuge Tube
cause of equipment failure.
Smallest Scale Maximum Scale
Range, mL
Division, mL Error, mL
6. Apparatus
0 to 0.1 0.05 60.02
6.1 Centrifuge Tube, cone-shaped, conforming to the di- Over 0.1 to 0.3 0.05 60.03
mensions given in Fig. 1, and made of thoroughly annealed Over 0.3 to 0.5 0.05 60.05
Over 0.5 to 1.0 0.1 60.05
glass. The graduations, numbered as shown in Fig. 1, shall be Over 1.0 to 2.0 0.1 60.10
clear and distinct and the mouth constricted in shape for Over 2.0 to 3.0 0.2 60.10
closure with a cork. Scale error tolerances and smallest Over 3.0 to 5.0 0.5 60.20
Over 5.0 to 10.0 1.0 60.50
graduations between various calibration marks are given in Over 10 to 25 5.0 61.0
Table 1 and apply to calibrations made with air-free water at 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 Table 2 shows the relationship between the diameter of
force (rcf) between 600 and 700 at the tips of the tubes. The swing, ref and rpm.
revolving head, trunnion rings, and trunnion cups, including 6.3 Oven, explosion-proof, capable of maintaining a tem-
the rubber cushion, shall be soundly constructed to withstand perature of 105 6 3°C.
the maximum centrifugal force capable of being delivered by 6.4 Balance, having a sensitivity of 0.5 mg for weighing the
the power source. The trunnion cups and cushions shall firmly 100-mL beaker and centrifuge tube, and a balance having a
support the tubes when the centrifuge is in motion. The sensitivity of 0.1 g for weighing the oil sample.
centrifuge shall be enclosed by a metal shield or case strong
enough to eliminate danger if any breakage occurs. Calculate TABLE 2 Rotation Speeds for Centrifuges of Various Diameters
the speed of the rotating head as follows: of Swing
Speed, rpm 5 1337 =rcf/d (1) Diameter of Swing, mmA rpm at 600 rcf rpm at 700 rcf
483 1490 1610
where: 508 1450 1570
rcf = relative centrifugal force, and 533 1420 1530
559 1390 1500
d = diameter swing, mm, measured between tips of
A
opposite tubes when in rotating position. Measured in millimetres between tips of opposite tubes when in rotating
position.

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 D 893 – 05a
7. Reagents and Solvents 9. Procedure A for Pentane and Toluene Insolubles
7.1 Purity of Reagents—Reagent grade chemicals shall be Without Coagulant
used in all tests. Unless otherwise indicated, it is intended that 9.1 Pentane Insolubles:
all reagents shall conform to the specifications of the Commit- 9.1.1 Dry a clean centrifuge tube for 30 min at 105 6 3°C,
tee on Analytical Reagents of the American Chemical Society, cool in a desiccator, and weigh to the nearest 1 mg. Weigh 10.0
where such specifications are available.3 Other grades may be 6 0.1 g of the prepared sample of used oil into the tube and fill
used, provided it is first ascertained that the reagent is of to the 100-mL mark with pentane (Warning—May be harmful
sufficiently high purity to permit its use without lessening the if inhaled or swallowed.). Stopper the tube and shake until the
accuracy of the determination. mixture is homogeneous. Do not allow the mixture to stand
7.2 Purity of Water—Unless otherwise indicated references more than 3 h.
to water shall be understood to mean water in accordance with 9.1.2 Remove the stopper, and using a wash bottle having a
Specification D 1193, Type IV. fine jet, wash all insolubles from the stopper into the centrifuge
7.3 n–butyl diethanolamine (2,21– (butylimino) diethanol). tube with a minimum of pentane. Balance the weights of each
(Warning—May be harmful if inhaled or swallowed.) pair of filled centrifuge tubes, place them in the centrifuge on
7.4 Ethanol, denatured—conforming to either Formula 30 opposite sides of the head, and centrifuge for 20 6 1 min at a
or 3A of the U.S. Bureau of Internal Revenue. (Warning— rate calculated in accordance with 6.2, sufficient to produce a
Flammable. Denatured. Cannot be made nontoxic.) relative centrifugal force (rcf) between 600 and 700 at the tips
7.5 Pentane—(Warning—Extremely flammable. Vapors of the whirling tubes. (See Table 2.) Carefully decant the
may cause flash fires.) supernatant liquid without disturbing or dispersing the precipi-
7.6 Propan–2–ol (isopropyl alcohol)—(Warning— tate, leaving not more than 3 mL of liquid in the centrifuge
Flammable. Denatured. Cannot be made nontoxic.) tube.
7.7 Toluene—(Warning—Flammable. Vapor harmful.)
7.8 Toluene-Alcohol Solution, wash solvent, made by mix- NOTE 3—Due to safety concerns when handling flammable materials,
ing 1 volume of toluene (7.7) with 1 volume of denatured some laboratories have found it suitable to use refrigerated or explosion-
proof centrifuges or hermetically sealed centrifuge cups with screw caps
ethanol conforming to either Formula No. 30 or 3A of the U.S.
and seals.
Bureau of Internal Revenue. (Warning—Flammable. Dena-
tured. Cannot be made nontoxic.) 9.1.3 Add 10 6 1 mL of pentane to the tube. Dislodge and
7.9 Pentane-Coagulant Solution—Add 50 mL of n-butyl break up all of the insolubles from the bottom of the tube by
diethanolamine (Warning—Flammable) and 50 mL of isopro- means of a clean stiff wire. Wash all insolubles adhering to the
pyl alcohol (2-propanol) (Warning—As used oil may change wire back into the tube with pentane, filling the tube to the
appreciably in storage, samples should be tested as soon as 50-mL mark. Stopper the tube and shake until the mixture is
possible after removal from the lubricating system and the homogeneous. Remove and wash the stopper. Centrifuge for 20
dates of sampling and testing should be noted) to 1 L of 6 1 min. Pour the supernatant liquid from the centrifuge tube,
n-pentane (Warning—May be harmful if inhaled or swal- using care to avoid disturbing the cake of insolubles in the
lowed) and mix. bottom of the tube.
9.1.4 Repeat the entire operation described in 9.1.3.
8. Sampling 9.1.5 Dry the centrifuge tube containing the washed precipi-
8.1 Obtain a sample using either Practice D 4057 or D 4177. tate for 30 min at 105 6 3°C, cool in desiccator, and weigh to
8.2 Heat the sample of used oil to 60 6 5°C in the original the nearest 1 mg.
container and agitate until all sediment is homogeneously 9.1.6 With relatively heavy precipitates there can be some
suspended in the oil. If the original container is of opaque spattering if the tube is placed directly from the centrifuge into
material, or if it is more than three-fourths full, transfer the the oven. In such cases, the precipitate may be partially dried
entire sample to a clear glass bottle having a capacity at least by weathering at room or slightly higher temperatures before
one third greater than the volume of the sample, and transfer all being placed in the oven.
traces of sediment from the original container to the bottle by 9.2 Toluene Insolubles:
violent agitation of portions of the sample in the original 9.2.1 Starting with a fresh sample of used oil, precipitate
container. After complete suspension of all sediment, strain the and centrifuge the pentane insolubles as described in 9.1.1-
sample or a convenient aliquot through a 150-µm (No. 100) 9.1.4, but do not dry the insolubles in the centrifuge tube.
sieve to remove large contaminating particles.
9.2.2 Add 10 6 1 mL of toluene-alcohol solution. Break up
NOTE 2—When the sample is clear and transparent and visibly free of and dislodge all of the insolubles from the bottom of the
sediment, the straining procedure described above can be omitted. 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
3
Reagent Chemicals, American Chemical Society Specifications, American solvent to fill the tube to the 50-mL mark. Stopper the tube and
Chemical Society, Washington, DC. For suggestions on the testing of reagents not shake until the mixture is homogeneous. Remove the stopper
listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and wash the adhering insolubles back into the tube with a
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, minimum amount of toluene. Centrifuge until no visible
MD. insolubles remain in suspension in the solvent; 10 to 20 min are

3
 D 893 – 05a
usually sufficient. Decant the clear solution, taking care not to 13.1.1.2 Procedure A, toluene insolubles, and Procedure B,
disturb the precipitate. coagulated toluene insolubles:
9.2.3 Repeat the washing procedure described in 9.2.2, Average Insolubles, % Repeatability, Same UnitsA
substituting toluene for the toluene-alcohol solution. 0.1 0.068
0.2 0.097
9.2.4 Dry for 1 h at 105 6 3 °C, cool in a desiccator, and 0.3 0.12
weigh to the nearest 1 mg. 0.4 0.14
0.5 0.15
0.6 0.17
10. Procedure B for Coagulated Pentane and Toluene 0.7 0.18
Insolubles 0.8 0.19
A
10.1 Coagulated Pentane Insolubles—Proceed in accor- These precision data were derived as follows:
Repeatability 5 0.216= I
dance with 9.1.1 and 9.1.2, except in 9.1.1 use pentane- where I = toluene insolubles or coagulated toluene insolubles.
coagulant solution (7.9) in place of pentane. Wash the precipi- 13.1.2 Reproducibility—The difference between two, single
tate twice with pentane, dry and weigh as directed in 9.1.3, and independent results obtained by different operators work-
9.1.4, and 9.1.5. ing in different laboratories on identical test material would, in
10.2 If the sample is known to contain water, or if water is the long run, and in the normal and correct operation of the test
indicated by a gummy precipitate, repeat the determination on method, exceed the following values only in one case in
a sample that has been dried by heating to 105 6 3°C in an twenty:
open beaker. 13.1.2.1 Procedure A, pentane insolubles, and Procedure B,
10.3 Coagulated Toluene Insolubles—Proceed in accor- coagulated pentane insolubles:
dance with 9.1.1 and 9.1.2 except in 9.1.1 use pentane- Insolubles, % Reproducibility, Same Units
coagulant solution (7.9) in place of pentane. Wash twice with 0.0 to 1.0 0.10
over 1.0 15 % of mean
pentane as directed in 9.1.3 and 9.1.4. Wash with toluene-
alcohol solution and toluene, dry, and weigh as directed in 13.1.2.2 Procedure A, toluene insolubles:
9.2.2-9.2.4. Average Insolubles, % Reproducibility, Same UnitsA
0.1 0.14
0.2 0.20
11. Calculation 0.3 0.24
11.1 Calculate the percentage of insolubles in the used oil as 0.4 0.28
0.5 0.31
follows: 0.6 0.34
Insolubles, % 5 10 ~B 2 A! (2) 0.7 0.37
0.8 0.39
0.9 0.42
where: 1.0 0.44
A = mass of clean, dried, centrifuge tube, g, and 1.1 0.46
B = mass of dried insolubles and centrifuge tube, g. A
These precision data were derived as follows: Reproducibility 5
0.441= IA
where IA = toluene insolubles.
12. Report
13.1.2.3 Procedure B, coagulated toluene insolubles (see
12.1 If Procedure A (Section 9) was employed, report the Note 4):
percentages of pentane insolubles and toluene insolubles. Average Insolubles, % Reproducibility, Same UnitsA
12.2 If Procedure B (Section 10) was employed, report the 0.1 0.30
percentages of coagulated pentane insolubles and coagulated 0.2 0.43
0.3 0.53
toluene insolubles. 0.4 0.60
12.3 Insoluble resins or coagulated insoluble resins may be 0.5 0.68
reported for either Procedure A or B, respectively, by subtract- 0.6 0.74
0.7 0.80
ing toluene insolubles from pentane insolubles. 0.8 0.86
0.9 0.91
13. Precision and Bias 1.0 0.96
1.1 1.00
13.1 Precision—The following criteria should be used for A
These precision data were derived as follows: Reproducibility 5
judging the acceptability of results (95 % confidence): 0.957= IB
13.1.1 Repeatability—The difference between successive where IB = coagulated toluene insolubles.
test results, obtained by the same operator with the same NOTE 4—The poor interlaboratory precision (reproducibility) of this
apparatus under constant operating conditions on identical test portion of this test is such that Procedure B coagulated toluene insolubles,
material would, in the long run, and in the normal and correct is unsuitable for the purpose of comparison of interlaboratory results.
operation of the test method, exceed the following values only 13.2 Bias—The procedure in this test method has no bias
in one case in twenty: because the mass percent of insoluble materials can only be
13.1.1.1 Procedure A, pentane insolubles, and Procedure B, defined in terms of this test method.
coagulated pentane insolubles:
14. Keywords
Insolubles, % Repeatability, Same Units
0.0 to 1.0 0.07 14.1 insoluble resins; insolubles; lubricating oil; pentane
Over 1.0 10 % of mean insolubles; toluene insolubles; used

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 D 893 – 05a

SUMMARY OF CHANGES

Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D 893–05) that may impact the use of this standard. (Approved Nov. 1, 2005.)

(1) Added Note 3.

Subcommittee D02.06 has identified the location of selected changes to this standard since the last issue
(D 893–97(2002)e1) that may impact the use of this standard. (Approved Feb. 1, 2005.)

(1) Added a new Note 2 to allow the option of not straining the
sample if there is no visible sediment in the sample.

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