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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
14-Jul-2014
Current Stage
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ASTM D7922-14 - Standard Test Method for Determination of Glycol for In-Service Engine Oils by Gas Chromatography
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D7922 − 14
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.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope E355PracticeforGasChromatographyTermsandRelation-
ships
1.1 This test method covers the determination of glycol
E594Practice for Testing Flame Ionization Detectors Used
based antifreeze for in-service engine oil by derivative
in Gas or Supercritical Fluid Chromatography
headspace/gas chromatography.
E1510Practice for Installing Fused Silica Open Tubular
1.2 Sample is derivatized in-situ directly in a headspace
Capillary Columns in Gas Chromatographs
samplingvialpriortovaporphaseextractionandinjectioninto
3. Terminology
a gas chromatograph.
3.1 Definitions:
1.3 The chemistry of the derivatization is unique to the
3.1.1 This test method makes reference to common gas
detection of the molecules of ethylene glycol and 1,2-
chromatographicprocedures,terms,andrelationships.Detailed
propylene glycol. 1,3-propylene glycol could also be detected
definitions of these can be found in Practices E355 and E594.
but is not used in any known anti-freeze at this time. Other
3.1.2 antifreeze, n—antifreeze is typically a dilution of
coolant analyses are beyond the scope of this test method.
ethylene glycol and possibly other glycols, and additives, in
1.4 The derivatization process does not affect glycol break-
water to act as a machine coolant. 1,2-propanediol is found in
down products such as glycolate and formate and hence the
some antifreeze formulations.
presence of these compounds in the oil will not be quantified.
3.1.3 derivitization reagent, n—a saturated solution of phe-
1.5 The test method concentration range is from 50 µg/g to
nylboronic acid (PBA) in solvent. Acetone and 2,2-
1000µg⁄g.Lowerlevelsarepossiblebymethodmodifications.
dimethoxypropane have been used successfully. Gentle warm-
Higher levels are possible through sample dilution.
ingat50°Cwillhastendissolution.Solutionisstableforthree
1.6 Units—The values stated in SI units are to be regarded
months at room temperature if kept away from moisture.
asstandard.Nootherunitsofmeasurementareincludedinthis
3.1.4 glycol, n—the amount, expressed as a percentage, of
standard.
glycol found in the in-service lubricating oil. The most
1.7 This standard does not purport to address all of the
common glycol formulated into antifreeze is ethylene glycol
safety concerns, if any, associated with its use. It is the
(CAS# 107-21-1) with some antifreeze also containing 1,2-
responsibility of the user of this standard to establish appro-
propanediol also known as propylene glycol (CAS# 57-55-6).
priate safety and health practices and determine the applica-
Another glycol such as 1,3-propanediol (CAS# 504-63-2) is
bility of regulatory limitations prior to use.
detected by this test method but is not commonly used in
antifreeze formulations.
2. Referenced Documents
3.1.5 glycols, n—the summed amount of individual glycols
2
2.1 ASTM Standards:
found in the in-service lubricating oil.
D4291Test Method for Trace Ethylene Glycol in Used
3.1.6 in-service oil, n—lubricating oil that is present in a
Engine Oil
machine that has been at operating temperature for at least 1h.
4. Summary of Test Method
1
This test method is under the jurisdiction of ASTM Committee D02 on
4.1 A representative aliquot of in-service engine oil is
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
introduced into a headspace sampling vial along with a
Subcommittee D02.04.0L on Gas Chromatography Methods.
derivatizing agent. The headspace vial is heated to volatilize
Current edition approved July 15, 2014. Published September 2014. DOI:
10.1520/D7922-14.
the derivatized glycol into the vapor phase. Using a small
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
aliquot of sample and derivatization reagent approaches a total
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
vaporization technique to minimize partition coefficient differ-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. ences in in-service oil samples.Arepresentative aliquot of the
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D7922 − 14
vapor sample is introduced to the gas chromatograph. Carrier 6.10 Daily column bake-out is recommended to get rid of
ga
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