ASTM D893-05a(2010)

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Designation:D893–05a (Reapproved 2010)
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 Department of Defense.
1. Scope D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of pentane
D4177 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
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
coagulated and separated matter not soluble in pentane or
oil in use or when comparing results determined by two or more
toluene.
laboratories.
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
oil that has been used for lubrication.
2. Referenced Documents
3.2 Definitions of Terms Specific to This Standard:
2.1 ASTM Standards:
3.2.1 insoluble resins, n—in used oil analysis, separated
D1193 Specification for Reagent Water
matter soluble in toluene but not pentane.
3.2.1.1 Discussion—Insoluble resins can be calculated for
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.
4. Summary of Test Method
Current edition approved May 1, 2010. Published June 2010. Originally
4.1 Procedure A—Arepresentative sample of used lubricat-
approved in 1967. Last previous edition approved in 2005 as D893–05a. DOI:
10.1520/D0893-05AR10.
ing oil is mixed with pentane and centrifuged. The oil solution
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
is decanted and the precipitate washed twice with pentane,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
dried, and weighed to give the pentane insolubles. For toluene
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. insolubles, a separate sample of the oil is mixed with pentane
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D893–05a (2010)
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
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
indicatesachangeinoilwhichcouldleadtolubricationsystem
problems.
5.4 Insolubles measured can also assist in evaluating the
FIG. 1 ASTM Cone-Shaped Centrifuge Tube
performance characteristics of a used oil or in determining the
cause of equipment failure.
TABLE 1 Calibration Tolerances of Cone-Shaped Centrifuge Tube
6. Apparatus
Smallest Scale Maximum Scale
Range, mL
Division, mL Error, mL
6.1 Centrifuge Tube, cone-shaped, conforming to the di-
0to0.1 0.05 60.02
mensions given in Fig. 1, and made of thoroughly annealed
Over 0.1 to 0.3 0.05 60.03
glass. The graduations, numbered as shown in Fig. 1, shall be
Over 0.3 to 0.5 0.05 60.05
clear and distinct and the mouth constricted in shape for
Over 0.5 to 1.0 0.1 60.05
closure with a cork. Scale error tolerances and smallest Over 1.0 to 2.0 0.1 60.10
Over 2.0 to 3.0 0.2 60.10
graduations between various calibration marks are given in
Over 3.0 to 5.0 0.5 60.20
Table 1 and apply to calibrations made with air-free water at
Over 5.0 to 10.0 1.0 60.50
Over 10 to 25 5.0 61.0
20°C.
Over 25 to 100 25.0 61.0
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
A
Diameter of Swing, mm rpm at 600 rcf rpm at 700 rcf
Speed, rpm 5 1337 rcf/d (1)
=
483 1490 1610
where: 508 1450 1570
533 1420 1530
rcf = relative centrifugal force, and
559 1390 1500
d = diameter swing, mm, measured between tips of
A
Measured in millimetres between tips of opposite tubes when in rotating
opposite tubes when in rotating position.
position.
D893–05a (2010)
7. Reagents and Solvents 9. Procedure A for Pentane and Toluene Insolubles
Without Coagulant
7.1 Purity of Reagents—Reagent grade chemicals shall be
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 onAnalytical Reagents of theAmerican Chemical Society,
cool in a desiccator, and weigh to the nearest 1 mg.Weigh 10.0
where such specifications are available. 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-mLmark 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 D1193, Type IV.
fine jet, wash all insolubles from the stopper into the centrifuge
7.3 n–butyl diethanolamine (2,2 – (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 wit
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