ASTM D893-14(2018)
(Test Method)Standard Test Method for Insolubles in Used Lubricating Oils
Standard Test Method for Insolubles in Used Lubricating Oils
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.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Section 7 and 9.1.1.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D893 − 14 (Reapproved 2018)
Standard Test Method for
Insolubles in Used Lubricating Oils
This standard is issued under the fixed designation D893; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 2. Referenced Documents
2.1 ASTM Standards:
1.1 This test method covers the determination of pentane
D1193 Specification for Reagent Water
and toluene insolubles in used lubricating oils.
D4057 Practice for Manual 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
D4177 Practice for Automatic Sampling of Petroleum and
indication of the materials that can readily be separated from
Petroleum Products
the oil-solvent mixtures by centrifuging.
3. Terminology
1.3 Procedure B covers the determination of insolubles in
3.1 Definitions:
oilscontainingdetergentsandemploysacoagulantforboththe
3.1.1 coagulate, v—tocausetobecomeviscousorthickened
pentane and toluene insolubles. In addition to the materials
into a coherent mass.
separated by using Procedure A, this coagulation procedure
separates some finely divided materials that may be suspended
3.1.2 coagulated pentane insolubles, n—in used oil
in the oil.
analysis, separated matter that results when a coagulant is
NOTE 1—Results obtained by Procedures A and B should not be added to a solution of used oil in pentane.
compared since they usually give different values. The same procedure
3.1.2.1 Discussion—The addition of a coagulant will aid in
should be employed when comparing values obtained periodically on an
separating finely divided materials that may have been held in
oil in use or when comparing results determined by two or more
suspension because of the dispersant characteristics of the oil.
laboratories.
3.1.3 coagulated toluene insolubles, n—in used oil analysis,
1.4 The values stated in SI units are to be regarded as
coagulated and separated matter not soluble in pentane or
standard. No other units of measurement are included in this
toluene.
standard.
3.1.4 pentane insolubles, n—in used oil analysis, separated
1.5 This standard does not purport to address all of the
matter resulting when a used oil is mixed with pentane.
safety concerns, if any, associated with its use. It is the
3.1.4.1 Discussion—In this test method, the separation is
responsibility of the user of this standard to establish appro-
effected by centrifugation.
priate safety, health, and environmental practices and deter-
3.1.5 toluene insolubles, n—in used oil analysis, the portion
mine the applicability of regulatory limitations prior to use.
of pentane insolubles not soluble in toluene.
For specific warning statements, see Section 7 and 9.1.1.
3.1.6 used oil, n—any oil that has been in a piece of
1.6 This international standard was developed in accor-
equipment (for example, an engine, gearbox, transformer, or
dance with internationally recognized principles on standard-
turbine), whether operated or not.
ization established in the Decision on Principles for the
3.1.6.1 Discussion—In this test method, the oil can be any
Development of International Standards, Guides and Recom-
oil that has been used for lubrication.
mendations issued by the World Trade Organization Technical
3.2 Definitions of Terms Specific to This Standard:
Barriers to Trade (TBT) Committee.
3.2.1 insoluble resins, n—in used oil analysis, separated
matter soluble in toluene but not pentane.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2018. Published November 2018. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1967. Last previous edition approved in 2014 as D893 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D0893-14R18. the ASTM website.
*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
D893 − 14 (2018)
3.2.1.1 Discussion—Insoluble resins can be calculated for
either Procedure A or B by subtracting the toluene insolubles
from the pentane insolubles.
4. Summary of Test Method
4.1 Procedure A—Arepresentative sample of used lubricat-
ing 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—Arepresentative 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
washedtwicewithpentane,oncewithtoluene-alcoholsolution,
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
FIG. 1 ASTM Cone-Shaped Centrifuge Tube
additive degradation, or both.
TABLE 1 Calibration Tolerances of Cone-Shaped Centrifuge Tube
5.2 Toluene insoluble materials can come from (1) external
Smallest Scale Maximum Scale
contamination, (2) fuel carbon and highly carbonized materials
Range, mL
Division, mL Error, mL
from degradation of fuel, oil, and additives, or (3) engine wear
0 to 0.1 0.05 ±0.02
and corrosion materials.
Over 0.1 to 0.3 0.05 ±0.03
Over 0.3 to 0.5 0.05 ±0.05
5.3 A significant change in pentane insolubles, toluene
Over 0.5 to 1.0 0.1 ±0.05
insolubles (with or without coagulant), and insoluble resins
Over 1.0 to 2.0 0.1 ±0.10
indicatesachangeinoilwhichcouldleadtolubricationsystem
Over 2.0 to 3.0 0.2 ±0.10
Over 3.0 to 5.0 0.5 ±0.20
problems.
Over 5.0 to 10.0 1.0 ±0.50
5.4 Insolubles measured can also assist in evaluating the Over 10 to 25 5.0 ±1.0
Over 25 to 100 25.0 ±1.0
performance characteristics of a used oil or in determining the
cause of equipment failure.
the power source. The trunnion cups and cushions shall firmly
6. Apparatus
support the tubes when the centrifuge is in motion. The
6.1 Centrifuge Tube, cone-shaped, conforming to the di-
centrifuge shall be enclosed by a metal shield or case strong
mensions given in Fig. 1, and made of thoroughly annealed
enough to eliminate danger if any breakage occurs. Calculate
glass. The graduations, numbered as shown in Fig. 1, shall be
the speed of the rotating head as follows:
clear and distinct and the mouth constricted in shape for
closure with a cork. Scale error tolerances and smallest
Speed, rpm 5 1337 =rcf/d (1)
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 oppo-
6.2 Centrifuge, meeting all safety requirements for normal
site 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
revolving head, trunnion rings, and trunnion cups, including 6.3 Oven, either explosion-proof, Class A, safety rated, or
the rubber cushion, shall be soundly constructed to withstand solvent venting, capable of maintaining a temperature of
the maximum centrifugal force capable of being delivered by 105 °C 6 3 °C.
D893 − 14 (2018)
TABLE 2 Rotation Speeds for Centrifuges of Various Diameters
8. Sampling
of Swing
8.1 Obtain a sample using either Practice D4057 or D4177.
A
Diameter of Swing, mm rpm at 600 rcf rpm at 700 rcf
8.2 If the original container is of opaque material, or if it is
483 1490 1610
508 1450 1570
more than three-fourths full, transfer the entire sample to a
533 1420 1530
clear glass bottle having a capacity at least one third greater
559 1390 1500
than the volume of the sample, and transfer all traces of
A
Measured in millimetres between tips of opposite tubes when in rotating position.
sediment from the original container to the bottle by violent
agitation of portions of the sample in the original container.
Heat the sample of used oil at 60 °C 6 5 °C for 30 min 6
1 min and agitate until all sediment is homogeneously sus-
6.4 Balance, having a sensitivity of 0.5 mg for weighing the
pended in the oil. After complete suspension of all sediment,
100 mL beaker and centrifuge tube, and a balance having a
strain the sample or a convenient aliquot through a 150 µm
sensitivity of 0.1 g for weighing the oil sample.
(No. 100) sieve to remove large contaminating particles.
7. Reagents and Solvents
NOTE 2—When the sample is clear and transparent and visibly free of
sediment, the straining procedure described above can be omitted.
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
9. Procedure A for Pentane and Toluene Insolubles
all reagents shall conform to the specifications of the Commit-
Without Coagulant
tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
9.1 Pentane Insolubles:
used, provided it is first ascertained that the reagent is of
9.1.1 Dry a clean centrifuge tube for 30 min 6 1 min at
sufficiently high purity to permit its use without lessening th
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.