ASTM D893-97

Standard Test Method for Insolubles In Used Lubricating Oils

SCOPE
1.1 This test method covers the determination of pentane and toluene insolubles in used lubricating oils.  
1.2 Procedure A covers the determination of insolubles without the use of coagulant in the pentane. It provides an indication of the materials that can readily be separated from the oil-solvent mixtures by centrifuging.  
1.3 Procedure B covers the determination of insolubles in oils containing detergents and employs a coagulant for both the pentane and toluene insolubles. In addition to the materials separated by using Procedure A, this coagulation procedure separates some finely divided materials that may be suspended in the oil.  Note 1-Results obtained by Procedures A and B should not be compared since they usually give different values. The same procedure should be employed when comparing values obtained periodically on an oil in use or when comparing results determined by two or more laboratories.
1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.> For specific precautionary statements, see 7.3, 7.4, 7.5, 7.6, 9.1, and 9.7.

General Information

• Status: Historical
• Publication Date: 09-Dec-1997
• Technical Committee: D02 - Petroleum Products, Liquid Fuels, and Lubricants
• Drafting Committee: D02.06.0B - Physical Testing

Relations

• Replaced By: ASTM D893-97(2002)e1 - Standard Test Method for Insolubles In Used Lubricating Oils
• Effective Date: 10-Dec-2002
• Referred By: ASTM D5372-20 - Standard Guide for Evaluation of Hydrocarbon Heat Transfer Fluids
• Effective Date: 10-Dec-1997
• Referred By: ASTM D7317-07(2019) - Standard Test Method for Coagulated Pentane Insolubles in Used Lubricating Oils by Paper Filtration (LMOA Method)
• Effective Date: 10-Dec-1997
• Referred By: ASTM D5704-22a - Standard Test Method for Evaluation of the Thermal and Oxidative Stability of Lubricating Oils Used for Manual Transmissions and Final Drive Axles
• Effective Date: 10-Dec-1997
• Referred By: ASTM D7665-22 - Standard Guide for Evaluation of Biodegradable Heat Transfer Fluids
• Effective Date: 10-Dec-1997
• Referred By: ASTM D6224-22 - Standard Practice for In-Service Monitoring of Lubricating Oil for Auxiliary Power Plant Equipment
• Effective Date: 10-Dec-1997
• Referred By: ASTM D7155-20 - Standard Practice for Evaluating Compatibility of Mixtures of Turbine Lubricating Oils
• Effective Date: 10-Dec-1997

Standards Content (Sample)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
An American National Standard
Designation: D 893 – 97
METRIC
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.
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 Products
D 4175 Terminology Relating to Petroleum, Petroleum
1.1 This test method covers the determination of pentane
Products, and Lubricants
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
indication of the materials that can readily be separated from
3. Terminology
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
1.4 The values stated in acceptable SI units are to be
separating finely divided materials that may have been held in
regarded as the standard.
suspension because of the dispersant characteristics of the oil.
NOTE 1—Results obtained by Procedures A and B should not be
3.1.3 coagulated toluene insolubles, n—in used oil analysis,
compared since they usually give different values. The same procedure
coagulated and separated matter not soluble in pentane or
should be employed when comparing values obtained periodically on an
toluene.
oil in use or when comparing results determined by two or more
3.1.4 pentane insolubles, n— in used oil analysis, separated
laboratories.
matter resulting when a used oil is mixed with pentane.
1.5 This standard does not purport to address all of the
3.1.4.1 Discussion—In this test method, the separation is
safety concerns, if any, associated with its use. It is the
effected by centrifugation.
responsibility of the user of this standard to establish appro-
3.1.5 toluene insolubles, n— in used oil analysis, the
priate safety and health practices and determine the applica-
portion of pentane insolubles not soluble in toluene.
bility of regulatory limitations prior to use. For specific
3.1.6 used oil, n—any oil that has been in a piece of
precautionary statements, see 7.7, 7.8, 7.9, 9.1, and 9.7.
equipment (for example, an engine, gearbox, transformer, or
turbine), whether operated or not.
2. Referenced Documents
3.1.6.1 Discussion—In this test method, the oil can be any
2.1 ASTM Standards:
oil that has been used for lubrication.
D 1193 Specification for Reagent Water
3.2 Definitions of Terms Specific to This Standard:
D 4057 Practice for Manual Sampling of Petroleum and
3.2.1 insoluble resins, n— in used oil analysis, separated
matter soluble in toluene but not pentane.
3.2.1.1 Discussion—Insoluble resins can be calculated for
This test method is under the jurisdiction of ASTM Committee D-2 on
either Procedue A or B by subtracting the toluene insolubles
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
from the pentane insolubles.
D02.06 on Analysis of Lubricants.
Current edition approved Dec. 10, 1997. Published February 1998. Originally
issued as D 893 – 67. Last previous edition D 893 – 92.
Annual Book of ASTM Standards, Vol 11.01. 3
Annual Book of ASTM Standards, Vol 05.02.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D893–97
4. Summary of Test Method
4.1 Procedure A— A representative sample of used lubri-
cating oil is mixed with pentane and centrifuged. The oil
solution is decanted and the precipitate washed twice with
pentane, 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
FIG. 1 ASTM Cone-Shaped Centrifuge Tube
from degradation of fuel, oil, and additives, or (3) engine wear
and corrosion materials.
TABLE 1 Calibration Tolerances of Cone-Shaped Centrifuge Tube
5.3 A significant change in pentane insolubles, toluene
Smallest Scale Maximum Scale
insolubles (with or without coagulant) and insoluble resins
Range, mL
Division, mL Error, mL
indicates a change in oil which could lead to lubrication system
0 to 0.1 0.05 60.02
problems.
Over 0.1 to 0.3 0.05 60.03
5.4 Insolubles measured can also assist in evaluating the
Over 0.3 to 0.5 0.05 60.05
Over 0.5 to 1.0 0.1 60.05
performance characteristics of a used oil or in determining the
Over 1.0 to 2.0 0.1 60.10
cause of equipment failure.
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
6. Apparatus
Over 10 to 25 5.0 61.0
Over 25 to 100 25.0 61.0
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
Speed, rpm 5 1337 =rcf/d (1)
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
force (rcf) between 600 and 700 at the tips of the tubes. The
TABLE 2 Rotation Speeds for Centrifuges of Various Diameters
revolving head, trunnion rings, and trunnion cups, including
of Swing
the rubber cushion, shall be soundly constructed to withstand
A
Diameter of Swing, mm rpm at 600 rcf rpm at 700 rcf
the maximum centrifugal force capable of being delivered by
483 1490 1610
the power source. The trunnion cups and cushions shall firmly
508 1450 1570
support the tubes when the centrifuge is in motion. The
533 1420 1530
centrifuge shall be enclosed by a metal shield or case strong
559 1390 1500
enough to eliminate danger if any breakage occurs. Calculate
A
Measured in millimetres between tips of opposite tubes when in rotating
the speed of the rotating head as follows: position.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D893–97
swing, ref and rpm. transfer all traces of sediment from the original container to the
6.3 Oven, explosion-proof, capable of maintaining a tem- bottle by violent agitation of portions of the sample in the
perature of 105 6 3°C. original container. After complete suspension of all sediment,
6.4 Balance, having a sensitivity of 0.5 mg for weighing the strain the sample or a convenient aliquot through a 150-μm
100-mL beaker and centrifuge tube, and a balance having a (No. 100) sieve to remove large contaminating particles.
sensitivity of 0.1 g for weighing the oil sample.
NOTE 7—As used oil may change appreciably in storage, samples
should be tested as soon as possible after removal from the lubricating
7. Reagents and Solvents
system and the dates of sampling and testing should be noted.
7.1 Purity of Reagents—Reagent grade chemicals shall be
9. Procedure A for Pentane and Toluene Insolubles
used in all tests. Unless otherwise indicated, it is intended that
Without Coagulant
all reagents shall conform to the specifications of the Commit-
Pentane Insolubles
tee on Analytical Reagents of the American Chemical Society,
9.1 Dry a clean centrifuge tube for 30 min at 105 6 3°C,
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of 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
sufficiently high purity to permit its use without lessening the
accuracy of the determination. to the 100-mL mark with pentane (Warning—See Note 5).
Stopper the tube and shake until the mixture is homogeneous.
7.2 Purity of Water— Unless otherwise indicated references
to water sha
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