ASTM D7922-23
(Test Method)Standard Test Method for Determination of Glycol for In-Service Engine Oils by Gas Chromatography
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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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: D7922 − 23
Standard Test Method for
Determination of Glycol for In-Service Engine Oils by Gas
1
Chromatography
This standard is issued under the fixed designation D7922; 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* 2. Referenced Documents
2
2.1 ASTM Standards:
1.1 This test method covers the determination of glycol
D4175 Terminology Relating to Petroleum Products, Liquid
based antifreeze for in-service engine oil by derivative
Fuels, and Lubricants
headspace/gas chromatography.
D4291 Test Method for Trace Ethylene Glycol in Used
1.2 Sample is derivatized in-situ directly in a headspace
Engine Oil
sampling vial prior to vapor phase extraction and injection into
E355 Practice for Gas Chromatography Terms and Relation-
a gas chromatograph.
ships
E594 Practice for Testing Flame Ionization Detectors Used
1.3 The chemistry of the derivatization is unique to the
in Gas or Supercritical Fluid Chromatography
detection of the molecules of ethylene glycol and 1,2-
E1510 Practice for Installing Fused Silica Open Tubular
propylene glycol. 1,3-propylene glycol could also be detected
Capillary Columns in Gas Chromatographs
but is not used in any known anti-freeze at this time. Other
coolant analyses are beyond the scope of this test method.
3. Terminology
1.4 The derivatization process does not affect glycol break-
3.1 Definitions:
down products such as glycolate and formate and hence the
3.1.1 This test method makes reference to common gas
presence of these compounds in the oil will not be quantified.
chromatographic procedures, terms, and relationships. Detailed
1.5 The test method concentration range is from 50 μg/g to
definitions of these can be found in Practices E355 and E594
1000 μg ⁄g. Lower levels are possible by method modifications.
and Terminology D4175.
Higher levels are possible through sample dilution.
3.1.2 antifreeze, n—antifreeze is typically a dilution of
ethylene glycol and possibly other glycols, and additives, in
1.6 Units—The values stated in SI units are to be regarded
water to act as a machine coolant. 1,2-propanediol is found in
as standard. No other units of measurement are included in this
some antifreeze formulations.
standard.
3.1.3 derivitization reagent, n—a saturated solution of phe-
1.7 This standard does not purport to address all of the
nylboronic acid (PBA) in solvent. Acetone and 2,2-
safety concerns, if any, associated with its use. It is the
dimethoxypropane have been used successfully. Gentle warm-
responsibility of the user of this standard to establish appro-
ing at 50 °C will hasten dissolution. Solution is stable for three
priate safety, health, and environmental practices and deter-
months at room temperature if kept away from moisture.
mine the applicability of regulatory limitations prior to use.
3.1.4 glycol, n—the amount, expressed as a percentage, of
1.8 This international standard was developed in accor-
glycol found in the in-service lubricating oil. The most
dance with internationally recognized principles on standard-
common glycol formulated into antifreeze is ethylene glycol
ization established in the Decision on Principles for the
(CAS# 107-21-1) with some antifreeze also containing 1,2-
Development of International Standards, Guides and Recom-
propanediol also known as propylene glycol (CAS# 57-55-6).
mendations issued by the World Trade Organization Technical
Another glycol such as 1,3-propanediol (CAS# 504-63-2) is
Barriers to Trade (TBT) Committee.
detected by this test method but is not commonly used in
antifreeze formulations.
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
2
Subcommittee D02.04.0L on Gas Chromatography Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2023. Published October 2023. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2014. Last previous edition approved in 2021 as D7922 – 21. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D7922-23. 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 ----------------------
...
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: D7922 − 21 D7922 − 23
Standard Test Method for
Determination of Glycol for In-Service Engine Oils by Gas
1
Chromatography
This standard is issued under the fixed designation D7922; 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*
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.
2. Referenced Documents
2
2.1 ASTM Standards:
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 Nov. 1, 2021Oct. 1, 2023. Published November 2021October 2023. Originally approved in 2014. Last previous edition approved in 20142021
as D7922 – 14.D7922 – 21. DOI: 10.1520/D7922-21.10.1520/D7922-23.
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 ----------------------
D7922 − 23
D4175 Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
D4291 Test Method for Trace Ethylene Glycol in Used Engine Oil
E355 Practice for Gas Chromatography Terms and Relationships
E594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography
E1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
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.
3.1.2 antifreeze, n—antifreeze is typically a dilution of ethylene glycol and possibly other glycols, and additives, in water to act
as a machine coolant. 1,2-propanediol is found in some antifreeze formulations.
3.1.3 derivitization reagent, n—a saturated solution of phenylboronic acid (PBA) in solvent. Acetone and 2,2-dimethoxypropane
have been used successfully. Gentle warming at 50 °C will hasten dissolution. Solution is stable for three months at room
temperature if kept away from moisture.
3.1.4 glycol, n—the amount, expressed as a percentage, of glycol found in the in-service lubricating oil. The most common glycol
formulated into antifreeze is ethylene glycol (CAS# 107-21-1) with some antifreeze also containing 1,2-propanediol also
...
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