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ASTM D893-05a

(Test Method)

Standard Test Method for Insolubles In Used Lubricating Oils

Standard Test Method for Insolubles In Used Lubricating Oils

SIGNIFICANCE AND USE
Pentane insolubles can include oil-insoluble materials and some oil-insoluble resinous matter originating from oil or additive degradation, or both.
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.  
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.
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 the standard. The values given in parentheses are for information only.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see Section and .

General Information

Status
Historical
Publication Date
31-Oct-2005
ICS
75.100 - Lubricants, industrial oils and related products
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.06 - Analysis of Liquid Fuels and Lubricants
Current Stage
Ref Project

Relations

Replaces
ASTM D893-05 - Standard Test Method for Insolubles In Used Lubricating Oils
Effective Date
01-Nov-2005
Replaced By
ASTM D893-05a(2010) - Standard Test Method for Insolubles In Used Lubricating Oils
Effective Date
01-May-2010
Referred By
ASTM D7317-07(2019) - Standard Test Method for Coagulated Pentane Insolubles in Used Lubricating Oils by Paper Filtration (LMOA Method)
Effective Date
01-Nov-2005
Referred By
ASTM D5372-20 - Standard Guide for Evaluation of Hydrocarbon Heat Transfer Fluids
Effective Date
01-Nov-2005
Referred By
ASTM D7665-22 - Standard Guide for Evaluation of Biodegradable Heat Transfer Fluids
Effective Date
01-Nov-2005
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
01-Nov-2005
Referred By
ASTM D7155-20 - Standard Practice for Evaluating Compatibility of Mixtures of Turbine Lubricating Oils
Effective Date
01-Nov-2005
Referred By
ASTM D6224-22 - Standard Practice for In-Service Monitoring of Lubricating Oil for Auxiliary Power Plant Equipment
Effective Date
01-Nov-2005

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ASTM D893-05a - Standard Test Method for Insolubles In Used Lubricating OilsASTM D893-05a - Standard Test Method for Insolubles In Used Lubricating Oils
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ASTM D893-05a - Standard Test Method for Insolubles In Used Lubricating Oils
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Please contact ASTM International (www.astm.org) for the latest information.
Designation:D893–05a
Standard Test Method for
1
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 (ϵ) 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
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
1
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 Nov. 1, 2005. Published November 2005. Originally
4.1 Procedure A—Arepresentative sample of used lubricat-
approved in 1967. Last previous edition approved in 2005 as D893–05. DOI:
10.1520/D0893-05A.
ing oil is mixed with pentane and centrifuged. The oil solution
2
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
*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.
1

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NOTICE: This standard has either been superseded and replaced b
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Note 1: The user of this test method should be proficient in the use of Test Methods D412 (tensile properties), D471 (effect of rubber immersion in liquids), D2240 (Durometer hardness), and D5662 (gear oil compatibility with typical oil seal elastomers), all of which are involved in the execution of the operations of this test method.  
1.3 This test method provides a preliminary or first order evaluation of oil/elastomer compatibility only. Because seals might be subjected to static or dynamic loads, or both, and they can operate over a range of conditions, a complete evaluation of the potential sealing performance of any elastomer-oil combination in any service condition usually requires tests additional to those described in this test method.  
1.4 The several reference elastomer formulations specified in this test method were chosen to be representative of those used in both heavy-duty diesel engines (detailed in Annex A1) and passenger-car spark-ignition engines (the latter are covered in Annex A2). The procedures described in this test method can, however, also be used to evaluate the compatibility of automotive engine oils with different elastomer types/formulations or different test durations and temperatures to those employed in this test method.
Note 2: In such cases, the precision and bias statement in Section 12 does not apply. In addition to agreeing acceptable limits of precision, where relevant, the user and supplier should also agree:  (1) test temperatures and immersion times to be used; (2) the formulations and typical properties of the elastomers; and (3) the sourcing and quality control of the elastomer sheets.
Note 3: The TMC may also issue In...

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ASTM
ASTM D7918-23(Test Method)
Standard Test Method for Measurement of Flow Properties and Evaluation of Wear, Contaminants, and Oxidative Properties of Lubricating Grease by Die Extrusion Method and Preparation

SIGNIFICANCE AND USE
5.1 Trending the wear, contamination, consistency, and oxidative properties of a lubricating grease is a crucial part of condition-monitoring programs. Changes in these properties or deviations from the new grease can be indicative of problems within the lubricated component, such as the mixing of incompatible thickener types, excessive wear or contaminant levels, or significant depletion of antioxidant levels. These test methods also makes it possible to develop trends that can be used to predict failures before they occur and allow for corrective action to be taken.
SCOPE
1.1 This test method covers the determination and evaluation of flow properties, wear levels, contaminants, and oxidative condition of new and in-service lubricating grease.  
1.2 This test method provides guidance on evaluating in-service grease samples, NLGI grades 00 to 3, for wear, consistency, contamination, and oxidation.  
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.3.1 Exception—The exception to this will be where units of references were developed by the developers of the test equipment and necessary to report the results of the test.  
1.4 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.  
1.5 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.

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ASTM
ASTM D7922-23(Test Method)
Standard Test Method for Determination of Glycol for In-Service Engine Oils by Gas Chromatography

SIGNIFICANCE AND USE
5.1 Some glycol/antifreeze dilution of in-service engine oil is normal under typical operating conditions. However, excessive glycol dilution can lead to decreased performance, premature wear, or sudden engine failure. This test method provides a means of quantifying the level of glycol based antifreeze dilution, allowing the user to take necessary action.
SCOPE
1.1 This test method covers the determination of glycol based antifreeze for in-service engine oil by derivative headspace/gas chromatography.  
1.2 Sample is derivatized in-situ directly in a headspace sampling vial prior to vapor phase extraction and injection into a gas chromatograph.  
1.3 The chemistry of the derivatization is unique to the detection of the molecules of ethylene glycol and 1,2-propylene glycol. 1,3-propylene glycol could also be detected but is not used in any known anti-freeze at this time. Other coolant analyses are beyond the scope of this test method.  
1.4 The derivatization process does not affect glycol breakdown products such as glycolate and formate and hence the presence of these compounds in the oil will not be quantified.  
1.5 The test method concentration range is from 50 µg/g to 1000 µg/g. Lower levels are possible by method modifications. Higher levels are possible through sample dilution.  
1.6 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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.  
1.8 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.

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