ASTM D7317-07(2019)

Standard Test Method for Coagulated Pentane Insolubles in Used Lubricating Oils by Paper Filtration (LMOA Method)

SIGNIFICANCE AND USE
5.1 Coagulated pentane insolubles can include oil-insoluble materials, some oil-insoluble resinous matter originating from oil or additive degradation, soot from incomplete diesel fuel combustion, or a combination of all three.  
5.2 A significant change in coagulated pentane insolubles indicates a change in oil, and this could lead to lubrication system problems.  
5.3 Coagulated pentane insolubles measurements can also assist in evaluating the performance characteristics of a used oil or in determining the cause of equipment failure.  
5.4 High values of coagulated pentane insolubles have been associated with plugged oil filters, leading to opening of the bypass valve and circulation of unfiltered oil in the engine. This can lead to increased piston deposits, increased bearing wear, and premature engine failure.
SCOPE
1.1 This test method covers the determination of coagulated pentane insolubles in used lubricating oils by a paper filtration method.  
1.2 This test method was originally developed by the Fuels, Lubricants, and Environmental Committee (FL&E) of the Locomotive Maintenance Officer’s Association (LMOA).2  
1.3 This test method is used primary for testing used diesel engine oils from railroad locomotive service. It may be applied to other samples types but precision, bias, and significance have not been determined for samples other than used railroad locomotive diesel engine oils.  
1.4 This test method, in general, does not correlate with Test Method D893 on Insolubles in Lubricating Oils, since it uses separation by centrifugation and a more concentrated solution of anti-coagulant.  
1.5 The correlation between this test method and Appendix A4 (Enhanced Thermal Gravimetric Analysis (TGA) Procedure) in Test Method D5967 has not been investigated.  
1.6 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. For specific warning statements, see 7.2, 7.3, and 7.4.  
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.

General Information

• Status: Published
• Publication Date: 30-Apr-2019
• 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

Relations

• Replaces: ASTM D7317-07(2013) - Standard Test Method for Coagulated Pentane Insolubles in Used Lubricating Oils by Paper Filtration (LMOA Method)
• Effective Date: 01-May-2019
• Refers: ASTM D4175-23a - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 15-Dec-2023
• Refers: ASTM D4175-23e1 - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Jul-2023
• Refers: ASTM D893-14(2018) - Standard Test Method for Insolubles in Used Lubricating Oils
• Effective Date: 01-Oct-2018
• Refers: ASTM D5967-17 - Standard Test Method for Evaluation of Diesel Engine Oils in T-8 Diesel Engine
• Effective Date: 01-May-2017
• Refers: ASTM D5967-15a - Standard Test Method for Evaluation of Diesel Engine Oils in T-8 Diesel Engine
• Effective Date: 01-Oct-2015
• Refers: ASTM D5967-15 - Standard Test Method for Evaluation of Diesel Engine Oils in T-8 Diesel Engine
• Effective Date: 01-Apr-2015
• Refers: ASTM D5967-14 - Standard Test Method for Evaluation of Diesel Engine Oils in T-8 Diesel Engine
• Effective Date: 01-Oct-2014
• Refers: ASTM D893-14 - Standard Test Method for Insolubles in Used Lubricating Oils
• Effective Date: 01-May-2014
• Refers: ASTM D5967-13 - Standard Test Method for Evaluation of Diesel Engine Oils in T-8 Diesel Engine
• Effective Date: 01-May-2013
• Refers: ASTM D5967-12a - Standard Test Method for Evaluation of Diesel Engine Oils in T-8 Diesel Engine
• Effective Date: 01-Dec-2012
• Refers: ASTM D5967-12 - Standard Test Method for Evaluation of Diesel Engine Oils in T-8 Diesel Engine
• Effective Date: 15-Apr-2012
• Refers: ASTM D893-12 - Standard Test Method for Insolubles in Used Lubricating Oils
• Effective Date: 15-Apr-2012
• Refers: ASTM D893-11 - Standard Test Method for Insolubles in Used Lubricating Oils
• Effective Date: 01-Dec-2011
• Refers: ASTM D4057-06(2011) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 01-Jun-2011

Overview

ASTM D7317-07(2019), titled Standard Test Method for Coagulated Pentane Insolubles in Used Lubricating Oils by Paper Filtration (LMOA Method), is an internationally recognized standard developed by ASTM International. This test method is designed for the determination of coagulated pentane insolubles in used lubricating oils, especially those from railroad locomotive diesel engines. Through a paper filtration process, this standard provides a practical means to assess oil-insoluble contaminants that may indicate oil or additive degradation, soot accumulation, or other operational issues.

Understanding and measuring coagulated pentane insolubles is vital for monitoring lubricant quality and maintenance of diesel engines, helping to prevent equipment failures and optimize lubrication system performance.

Key Topics

• Coagulated Pentane Insolubles: Refers to oil-insoluble contaminants and resinous materials resulting from degradation, combustion byproducts (such as soot), and other insoluble matter present in used oils.
• Paper Filtration Technique: A laboratory method that uses a vacuum-driven paper filtration apparatus to separate and quantify insoluble materials after adding a pentane-coagulant solution.
• Significance for Maintenance: High levels of insolubles are closely linked to maintenance concerns, such as plugged oil filters, increased engine deposits, bearing wear, and risk of engine failure.
• Diesel Locomotive Focus: Primarily developed for and applied to used diesel engine oils from railroad locomotives, where oil condition monitoring is critical for service continuity and equipment longevity.
• Comparison with Other Methods: This method does not generally correlate with ASTM D893 due to differences in separation technique and reagent concentration, nor has it been compared directly with TGA methods described in ASTM D5967.
• Precision and Bias: Established precision and reproducibility values are provided for used railroad diesel engine oils; for other oil types, these characteristics have not been determined.

Applications

The ASTM D7317-07(2019) standard delivers practical value in several areas of lubricant testing and equipment maintenance:

• Routine Oil Analysis: Enables scheduled monitoring of insoluble content in used diesel locomotive oils, supporting proactive maintenance strategies.
• Troubleshooting Equipment Failures: Aids in diagnosing causes of lubrication-related failures by identifying abnormal increases in insoluble contaminants.
• Filter Performance Assessment: Helps evaluate oil filter clogging tendencies, predicting bypass valve operation that could lead to unfiltered oil circulating through an engine.
• Establishing Baseline Data: Supports the creation of baseline insoluble levels for specific engine types and operational environments, improving reliability and extending equipment service life.
• Quality Assurance in Maintenance Programs: Integrates seamlessly into oil condition monitoring programs for the rail industry and other heavy-duty diesel applications.
• Applicability to Other Used Oils: While primarily validated for locomotive diesel engine oils, it may serve as a reference for testing other used lubricating oils with expert caution.

Related Standards

The ASTM D7317-07(2019) standard interacts with several other important ASTM standards and industry test methods, including:

• ASTM D893 – Test Method for Insolubles in Used Lubricating Oils (uses centrifugation and higher anti-coagulant concentration, not directly comparable).
• ASTM D5967 – Test Method for Evaluation of Diesel Engine Oils in T-8 Diesel Engine (includes a TGA-based procedure for insolubles).
• ASTM D4057 – Practice for Manual Sampling of Petroleum and Petroleum Products.
• ASTM D4175 – Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants.
• ASTM D4177 – Practice for Automatic Sampling of Petroleum and Petroleum Products.

By adhering to ASTM D7317-07(2019), organizations ensure reliable, consistent measurements of insoluble contaminants in used lubricating oils, supporting predictive maintenance and reducing risk in diesel locomotive operations.

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: D7317 − 07 (Reapproved 2019)
Standard Test Method for
Coagulated Pentane Insolubles in Used Lubricating Oils by
Paper Filtration (LMOA Method)
This standard is issued under the fixed designation D7317; 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.
1. Scope mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This test method covers the determination of coagulated
pentane insolubles in used lubricating oils by a paper filtration
2. Referenced Documents
method.
2.1 ASTM Standards:
1.2 This test method was originally developed by the Fuels,
D893 Test Method for Insolubles in Used Lubricating Oils
Lubricants, and Environmental Committee (FL&E) of the
D4057 Practice for Manual Sampling of Petroleum and
Locomotive Maintenance Officer’s Association (LMOA).
Petroleum Products
1.3 This test method is used primary for testing used diesel
D4175 Terminology Relating to Petroleum Products, Liquid
engine oils from railroad locomotive service. It may be applied Fuels, and Lubricants
to other samples types but precision, bias, and significance D4177 Practice for Automatic Sampling of Petroleum and
have not been determined for samples other than used railroad Petroleum Products
locomotive diesel engine oils. D5967 Test Method for Evaluation of Diesel Engine Oils in
T-8 Diesel Engine
1.4 Thistestmethod,ingeneral,doesnotcorrelatewithTest
Method D893 on Insolubles in Lubricating Oils, since it uses
3. Terminology
separation by centrifugation and a more concentrated solution
3.1 Definitions:
of anti-coagulant.
3.1.1 coagulate, v—tocausetobecomeviscousorthickened
1.5 The correlation between this test method and Appendix
into a coherent mass. D4175
A4 (Enhanced Thermal Gravimetric Analysis (TGA) Proce-
3.1.2 coagulated pentane insolubles, n—in used oil
dure) in Test Method D5967 has not been investigated.
analysis, separated matter that results when a coagulant is
1.6 The values stated in SI units are to be regarded as
added to a solution of used oil in pentane. D4175
standard. No other units of measurement are included in this
3.1.2.1 Discussion—The addition of a coagulant will aid in
standard.
separating finely divided materials that may have been held in
1.7 This standard does not purport to address all of the
suspension because of the dispersant characteristics of the oil.
safety concerns, if any, associated with its use. It is the 3.1.2.2 Discussion—This test method uses a 1 % coagulant
responsibility of the user of this standard to establish appro-
solution. Test Method D893 uses a 5 % coagulant solution.
priate safety, health, and environmental practices and deter-
3.1.3 membrane filter, n—porous article of closely con-
mine the applicability of regulatory limitations prior to use.
trolled pore size through which a liquid is passed to separate
For specific warning statements, see 7.2, 7.3, and 7.4.
matter in suspension. D4175
1.8 This international standard was developed in accor-
3.1.4 pentane insolubles, n—in used oil analysis, separated
dance with internationally recognized principles on standard-
matterresultingwhenausedoilisdissolvedinpentane. D4175
ization established in the Decision on Principles for the
3.1.4.1 Discussion—In this test method, the separation is
Development of International Standards, Guides and Recom-
effected by paper filtration.
3.1.5 used oil, n—any oil that has been in a piece of
equipment (for example, an engine, gearbox, transformer, or
This test method is under the jurisdiction of ASTM Committee D02 on
turbine), whether operated or not. D4175
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.
CurrenteditionapprovedMay1,2019.PublishedJuly2019.Originallyapproved
in 2006. Last previous edition approved in 2013 as D7317 – 07 (2013). DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D7317-07R19. contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Locomotive Maintenance Officer’s Association (LMOA), 6047 South Mobile Standards volume information, refer to the standard’s Document Summary page on
Avenue, Chicago, IL 60638, http://lmoarail.com/. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7317 − 07 (2019)
3.1.5.1 Discussion—In this test method, the oil can be any 6.11 Stopwatch or Other Timing Device, capable of measur-
oil that has been used for lubrication of a locomotive diesel ing to the nearest 0.1 s with a range of at least 5 min.
engine, whether engaged in railroad or other service.
7. Reagents and Solvents
3.2 Definitions of Terms Specific to This Standard:
7.1 Purity of Reagents—Reagent grade chemicals shall be
3.2.1 locomotive diesel engine oil, n—lubricating oil formu-
used in all tests. Unless otherwise indicated, it is intended that
lated to meet the chemical, physical, and performance require-
all reagents shall conform to the specifications of the Commit-
ments defined by the LMOA for service in diesel engines in
tee onAnalytical Reagents of theAmerican Chemical Society,
railroad locomotives.
where such specifications are available. Other grades may be
3.3 Acronyms:
used, provided it is first ascertained that the reagent is of
3.3.1 ILS—interlaboratory study
sufficiently high purity to permit its use without lessening the
3.3.2 LMOA—Locomotive Maintenance Officer’s Associa-
accuracy of the determination. If industrial grade pentane is
tion
used, it shall be filtered using 0.45 µm filter paper.
3.3.3 RR—railroad
7.2 n–butyl diethanolamine (2,2’– (butylimino) diethanol),
3.3.4 TGA—thermo-gravimetric analysis 98 %. (Warning—May be harmful if inhaled or swallowed.)
7.3 Pentane (n-pentane), 98 %. (Warning—Extremely
4. Summary of Test Method
flammable. Vapors may cause flash fires.)
4.1 Arepresentative sample of used lubricating oil is mixed
7.4 Pentane-Coagulant Solution, 1 %—Add 5 mL of
with pentane-coagulant solution and filtered under vacuum.
n-butyl diethanolamine (Warning—Flammable.) to 500 mLof
The filter is washed with pentane, dried, and weighed to give
n-pentane (Warning—May be harmful if inhaled or swal-
coagulated pentane insolubles.
lowed.) and mix. Solution shall be used within one month and
should preferably be made within a week of using.
5. Significance and Use
5.1 Coagulated pentane insolubles can include oil-insoluble
8. Sampling
materials, some oil-insoluble resinous matter originating from
8.1 Obtain a sample using either Practice D4057 or D4177.
oil or additive degradation, soot from incomplete diesel fuel
8.2 Heat the sample of used oil to 50 °C 6 5 °C for ⁄2 h 6
combustion, or a combination of all three.
5 min in the original container and agitate until all sediment is
5.2 A significant change in coagulated pentane insolubles
homogeneouslysuspendedintheoil.Iftheoriginalcontaineris
indicates a change in oil, and this could lead to lubrication
of opaque material, or if it is more than three-fourths full,
system problems.
transfer the entire sample to a clear glass bottle having a
5.3 Coagulated pentane insolubles measurements can also
capacity at least one third greater than the volume of the
assist in evaluating the performance characteristics of a used
sample, and transfer all traces of sediment from the original
oil or in determining the cause of equipment failure.
container to the bottle by vigorous agitation of portions of the
sample in the original container.
5.4 High values of coagulated pentane insolubles have been
associated with plugged oil filters, leading to opening of the
9. Procedure
bypassvalveandcirculationofunfilteredoilintheengine.This
9.1 Dry a clean filter membrane for 15 min in a desiccator,
can lead to increased piston deposits, increased bearing wear,
place in a labeled aluminum weighing dish, and weigh to the
and premature
...