ASTM D893-97(2002)e1

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An American National Standard
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Designation:D893–97 (Reapproved 2002)
Standard Test Method for
Insolubles In Used Lubricating Oils
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.
e NOTE—Warning notes were editorially moved into the standard in March 2003.
1. Scope D 4175 Terminology Relating to Petroleum, Petroleum
Products, and Lubricants
1.1 This test method covers the determination of pentane
D 4177 Practice for Automatic Sampling of Petroleum and
and toluene insolubles in used lubricating oils.
Petroleum Products
1.2 Procedure A covers the determination of insolubles
without the use of coagulant in the pentane. It provides an
3. Terminology
indication of the materials that can readily be separated from
3.1 Definitions:
the oil-solvent mixtures by centrifuging.
3.1.1 coagulate, v—to cause to become viscous or thick-
1.3 Procedure B covers the determination of insolubles in
ened into a coherent mass.
oilscontainingdetergentsandemploysacoagulantforboththe
3.1.2 coagulated pentane insolubles, n—in used oil analy-
pentane and toluene insolubles. In addition to the materials
sis, separated matter that results when a coagulant is added to
separated by using Procedure A, this coagulation procedure
a solution of used oil in pentane.
separates some finely divided materials that may be suspended
3.1.2.1 Discussion—The addition of a coagulant will aid in
in the oil.
separating finely divided materials that may have been held in
1.4 The values stated in acceptable SI units are to be
suspension because of the dispersant characteristics of the oil.
regarded as the standard.
3.1.3 coagulated toluene insolubles, n—in used oil analysis,
NOTE 1—Results obtained by Procedures A and B should not be
coagulated and separated matter not soluble in pentane or
compared since they usually give different values. The same procedure
toluene.
should be employed when comparing values obtained periodically on an
3.1.4 pentane insolubles, n—in used oil analysis, separated
oil in use or when comparing results determined by two or more
matter resulting when a used oil is mixed with pentane.
laboratories.
3.1.4.1 Discussion—In this test method, the separation is
1.5 This standard does not purport to address all of the
effected by centrifugation.
safety concerns, if any, associated with its use. It is the
3.1.5 toluene insolubles, n—in used oil analysis, the portion
responsibility of the user of this standard to establish appro-
of pentane insolubles not soluble in toluene.
priate safety and health practices and determine the applica-
3.1.6 used oil, n—any oil that has been in a piece of
bility of regulatory limitations prior to use. For specific
equipment (for example, an engine, gearbox, transformer, or
precautionary statements, see 7.7, 7.8, 7.9, 9.1, and 9.7.
turbine), whether operated or not.
3.1.6.1 Discussion—In this test method, the oil can be any
2. Referenced Documents
oil that has been used for lubrication.
2.1 ASTM Standards:
3.2 Definitions of Terms Specific to This Standard:
D 1193 Specification for Reagent Water
3.2.1 insoluble resins, n—in used oil analysis, separated
D 4057 Practice for Manual Sampling of Petroleum and
matter soluble in toluene but not pentane.
Petroleum Products
3.2.1.1 Discussion—Insoluble resins can be calculated for
either Procedue A or B by subtracting the toluene insolubles
1 from the pentane insolubles.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
4. Summary of Test Method
D02.06 on Analysis of Lubricants.
Current edition approved Dec. 10, 2002. Published March 2003. Originally
4.1 Procedure A—Arepresentative sample of used lubricat-
approved in 1967. Last previous edition approved in 1997 as D 893 – 97.
ing oil is mixed with pentane and centrifuged. The oil solution
Annual Book of ASTM Standards, Vol 11.01.
Annual Book of ASTM Standards, Vol 05.02. is decanted and the precipitate washed twice with pentane,
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D893–97 (2002)
dried, and weighed to give the pentane insolubles. For toluene
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 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
FIG. 1 ASTM Cone-Shaped Centrifuge Tube
indicatesachangeinoilwhichcouldleadtolubricationsystem
problems. TABLE 1 Calibration Tolerances of Cone-Shaped Centrifuge Tube
5.4 Insolubles measured can also assist in evaluating the Smallest Scale Maximum Scale
Range, mL
Division, mL Error, mL
performance characteristics of a used oil or in determining the
0to0.1 0.05 60.02
cause of equipment failure.
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
6. Apparatus
Over 1.0 to 2.0 0.1 60.10
Over 2.0 to 3.0 0.2 60.10
6.1 Centrifuge Tube, cone-shaped, conforming to the di-
Over 3.0 to 5.0 0.5 60.20
mensions given in Fig. 1, and made of thoroughly annealed
Over 5.0 to 10.0 1.0 60.50
glass. The graduations, numbered as shown in Fig. 1, shall be
Over 10 to 25 5.0 61.0
Over 25 to 100 25.0 61.0
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
where:
Table 1 and apply to calibrations made with air-free water at
rcf = relative centrifugal force, and
20°C.
d = diameter swing, mm, measured between tips of
6.2 Centrifuge, meeting all safety requirements for normal
opposite tubes when in rotating position.
use and capable of whirling two or more filled centrifuge tubes
Table 2 shows the relationship between the diameter of
at a speed that can be controlled to give a relative centrifugal
swing, ref and rpm.
force (rcf) between 600 and 700 at the tips of the tubes. The
6.3 Oven, explosion-proof, capable of maintaining a tem-
revolving head, trunnion rings, and trunnion cups, including
perature of 105 6 3°C.
the rubber cushion, shall be soundly constructed to withstand
the maximum centrifugal force capable of being delivered by
TABLE 2 Rotation Speeds for Centrifuges of Various Diameters
the power source. The trunnion cups and cushions shall firmly
of Swing
A
support the tubes when the centrifuge is in motion. The
Diameter of Swing, mm rpm at 600 rcf rpm at 700 rcf
centrifuge shall be enclosed by a metal shield or case strong
483 1490 1610
enough to eliminate danger if any breakage occurs. Calculate 508 1450 1570
533 1420 1530
the speed of the rotating head as follows:
559 1390 1500
A
Speed, rpm 5 1337 =rcf/d (1)
Measured in millimetres between tips of opposite tubes when in rotating
position.
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D893–97 (2002)
6.4 Balance, having a sensitivity of 0.5 mg for weighing the 9. Procedure A for Pentane and Toluene Insolubles
100-mL beaker and centrifuge tube, and a balance having a Without Coagulant
sensitivity of 0.1 g for weighing the oil sample. Pentane Insolubles
9.1 Dry a clean centrifuge tube for 30 min at 105 6 3°C,
7. Reagents and Solvents
cool in a desiccator, and weigh to the nearest 1 mg.Weigh 10.0
7.1 Purity of Reagents—Reagent grade chemicals shall be
6 0.1 g of the prepared sample of used oil into the tube and fill
used in all tests. Unless otherwise indicated, it is intended that
to the 100-mLmark with pentane (Warning—May be harmful
all reagents shall conform to the specifications of the Commit-
if inhaled or swallowed.). Stopper the tube and shake until the
tee onAnalytical Reagents of theAmerican Chemical Society,
mixture is homogeneous. Do not allow the mixture to stand
where such specifications are available. Other grades may be
more than 3 h.
used, provided it is first ascertained that the reagent is of
9.2 Remove the stopper, and using a wash bottle having a
sufficiently high purity to permit its use without lessening the
fine jet, wash all insolubles from the stopper into the centrifuge
accuracy of the determination.
tube with a minimum of pentane. Balance the weights of each
7.2 Purity of Water—Unless otherwise indicated references
pair of filled centrifuge tubes, place them in the centrifuge on
to water shall be understood to mean water in accordance with
opposite sides of the head, and centrifuge for 20 6 1 min at a
Specification D 1193, Ty
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