ASTM D4291-21
(Test Method)Standard Test Method for Trace Ethylene Glycol in Used Engine Oil
Standard Test Method for Trace Ethylene Glycol in Used Engine Oil
SIGNIFICANCE AND USE
5.1 Leakage of aqueous engine coolant into the crank case weakens the ability of the oil to lubricate. If ethylene glycol is present, it promotes varnish and deposit formation. This test method is designed for early detection to prevent coolant from accumulating and seriously damaging the engine.
SCOPE
1.1 This test method covers the determination of ethylene glycol as a contaminant in used engine oil. This test method is designed to quantitate ethylene glycol in the range from 5 mass ppm to 200 mass ppm.
1.2 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.
Note 1: A qualitative determination of glycol-base antifreeze is provided in Test Methods D2982. Procedure A is sensitive to about 100 ppm.
1.3 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
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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: D4291 − 21
Standard Test Method for
1
Trace Ethylene Glycol in Used Engine Oil
This standard is issued under the fixed designation D4291; 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* 3. Terminology
1.1 This test method covers the determination of ethylene 3.1 Definitions:
glycol as a contaminant in used engine oil. This test method is 3.1.1 This test method makes reference to common gas
designed to quantitate ethylene glycol in the range from chromatographicprocedures,terms,andrelationships.Detailed
5 mass ppm to 200 mass ppm. definitions of these can be found in Practices E355 and E594,
and Terminology D4175.
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 The sample of oil is extracted with water and the
priate safety, health, and environmental practices and deter-
analysis is performed on the water extract. A reproducible
mine the applicability of regulatory limitations prior to use.
volume of the extract is injected into a gas chromatograph
For specific warning statements, see Section 7.
using on-column injection and the eluting compounds are
NOTE 1—A qualitative determination of glycol-base antifreeze is
detected by a flame ionization detector. The ethylene glycol
provided in Test Methods D2982. Procedure A is sensitive to about
peak area is determined and compared with areas obtained
100 ppm.
from the injection of freshly prepared known standards.
1.3 This international standard was developed in accor-
dance with internationally recognized principles on standard-
5. Significance and Use
ization established in the Decision on Principles for the
5.1 Leakage of aqueous engine coolant into the crank case
Development of International Standards, Guides and Recom-
weakens the ability of the oil to lubricate. If ethylene glycol is
mendations issued by the World Trade Organization Technical
present, it promotes varnish and deposit formation. This test
Barriers to Trade (TBT) Committee.
method is designed for early detection to prevent coolant from
accumulating and seriously damaging the engine.
2. Referenced Documents
2
2.1 ASTM Standards: 6. Apparatus
D1193 Specification for Reagent Water
6.1 Gas Chromatograph—Any gas chromatograph
D2982 Test Methods for Detecting Glycol-Base Antifreeze
equipped with the following:
in Used Lubricating Oils
6.1.1 Flame Ionization Detector, capable of operating con-
D4057 Practice for Manual Sampling of Petroleum and
tinuously at a temperature equivalent to the maximum column
Petroleum Products
temperature employed, and connected to the column so as to
D4175 Terminology Relating to Petroleum Products, Liquid
avoid any cold spots.
Fuels, and Lubricants
6.1.2 Sample Inlet System, providing for on-column injec-
E355 Practice for Gas Chromatography Terms and Relation-
tion and capable of operating continuously at a temperature
ships
equivalent to the maximum column temperature employed.
E594 Practice for Testing Flame Ionization Detectors Used
6.2 Recorder—Recording potentiometer with a full-scale
in Gas or Supercritical Fluid Chromatography
response time of 2 s or less may be used.
1
6.3 Columns—1.2 m by 6.4 mm (4 ft by ⁄4 in.) copper tube
1
This test method is under the jurisdiction of ASTM Committee D02 on
packed with 5 % by mass Carbowax 20-M liquid phase on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.04.0L on Gas Chromatography Methods.
30/60 mesh Chromosorb T solid support. As an alternative, a
Current edition approved Dec. 1, 2021. Published December 2021. Originally
fused silica capillary column, 15 m long with a 0.53 mm ID
approved in 1983. Last previous edition approved in 2017 as D4291 – 04 (2017).
and 2.0 micron film thickness of a bonded polyethylene glycol
DOI: 10.1520/D4291-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or can be used.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
6.4 Integrator—Manual, mechanical, or electronic integra-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. tion is required to determine the peak area. However, best
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4291 − 04 (Reapproved 2017) D4291 − 21
Standard Test Method for
1
Trace Ethylene Glycol in Used Engine Oil
This standard is issued under the fixed designation D4291; 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 Scope*
1.1 This test method covers the determination of ethylene glycol as a contaminant in used engine oil. This test method is designed
to quantitate ethylene glycol in the range from 5 mass ppm to 200 mass ppm.
1.2 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 67.
NOTE 1—A qualitative determination of glycol-base antifreeze is provided in Test Methods D2982. Procedure A is sensitive to about 100 ppm.
1.3 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.
2. Referenced Documents
2
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D2982 Test Methods for Detecting Glycol-Base Antifreeze in Used Lubricating Oils
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
E355 Practice for Gas Chromatography Terms and Relationships
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
3. Terminology
3.1 Definitions:
3.1.1 This test method makes reference to common gas chromatographic procedures, terms, and relationships. Detailed definitions
of these can be found in Practices E355 and E594, and Terminology D4175.
4. Summary of Test Method
4.1 The sample of oil is extracted with water and the analysis is performed on the water extract. A reproducible volume of the
1
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
D02.04.0L on Gas Chromatography Methods.
Current edition approved Oct. 1, 2017Dec. 1, 2021. Published November 2017December 2021. Originally approved in 1983. Last previous edition approved in 20132017
as D4291 – 04 (2013).(2017). DOI: 10.1520/D4291-04R17.10.1520/D4291-21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on 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
1
---------------------- Page: 1 ----------------------
D4291 − 21
extract is injected into a gas chromatograph using on-column injection and the eluting compounds are detected by a flame
ionization detector. The ethylene glycol peak area is determined and compared with areas obtained from the injection of freshly
prepared known standards.
5. Significance and Use
5.1 Leakage of aqueous engine coolant into the crank case weakens the ability of the oil to lubricate. If ethylene glycol is present,
it promotes varnish and deposit formation. This test method is designed for early detection to prevent coolant from accumulating
and seriously damaging the engine.
6. Apparatus
6.1 Gas Chromatograph—Any gas chromatograph equipped with the following:
6.1.1 Flame Ionization Detector, capable of operating continuously at a temperature equivalent to the maximum column
temperature employed, and connected to the column so as to avoid any cold spots.
6.1.2 Sample Inlet System, providing for on-column injection and capable of operating continuously at a temperature equivalent
to the maximum column temperature employed.
6.2 Recorder—Recording potentiometer with a full-scale response time of 2 s or less may be used.
1
6.3 Columns—1.2 m by 6.4 mm (4 ft by ⁄4 in.) copper tube packed with 5 % by mass Carbowax
...
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