ASTM D2982-07(2019)

Standard Test Methods for Detecting Glycol-Base Antifreeze in Used Lubricating Oils

SIGNIFICANCE AND USE
5.1 Leakage of glycol-base antifreeze into the crankcase is serious because the coolant tends to interfere with the lubricant and its ability to lubricate; it also promotes sludging. Ethylene glycol present in the coolant can increase varnish deposit formation in the crankcase as a result of glycol oxidation and the interaction between glycol and lubricant. Furthermore, because glycol is a higher boiling material than water, it will tend to stay longer in the crankcase oil than water. Lubricant displacement, sludging, and deposit formation all lead to engine malfunction and possible seizure.  
5.2 These tests are designed to detect glycol-base coolant contamination even at low levels because early detection enables corrective measures to be taken to prevent leaking coolant from accumulating and seriously damaging the engine.  
5.3 These test methods are also significant because the reagents can be packaged as a field kit, and the procedure can be followed at the site where there is a concern.
SCOPE
1.1 These test methods cover the qualitative determination of glycol-base antifreeze in used lubricating oils (mineral base) by two procedures, one using reagents in tablet form and the other using laboratory shelf reagents. Principally the test methods detect ethylene glycol but will also detect other 1,2-glycols that may be present.  
1.1.1 When a positive result is obtained and a sample of the unused oil is available, the unused oil is also tested and used as a reference.
Note 1: Since the inception of this test method (1971), there have been many changes in base stock technology and additive technology. Therefore, when available, the new, unused oil, or a sample of the same used oil, known to not contain antifreeze, is tested as a reference.  
1.2 The tablet procedure (Procedure A) is sensitive to about 100 mg/kg and the shelf reagent procedure (Procedure B) to about 300 mg/kg of ethylene glycol.  
1.3 Glycol-based coolant leaks into crankcases may not be detected or may result in a low bias using these test methods if the glycol has degraded or been thermally or otherwise oxidized. The conditions in crankcases may be such that contaminant glycols are oxidized or degraded to a degree to which the color indicator reaction does not occur or is biased enough so as to not trigger the color change. Other test methods for the detection of coolants or coolant additives in lubricating oils should be used if the results from these test methods alone are inconclusive or questionable.  
1.4 Carbohydrates such as sugars and sugar-containing substances are sometimes used for sabotage purposes. If the presence of these substances is suspected, Procedure A contains a modification to remove these interferences.  
1.5 Both procedures are adaptable to field kit use, and brief descriptions for converting to field kit form are given in Annex A1.  
1.5.1 Commercial field testing kits are available.2,3  
1.6 The results obtained by this method are qualitative expressions. However, for the preparation of reagents and in the procedures, acceptable SI units are to be regarded as the 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.

General Information

• Status: Published
• Publication Date: 30-Nov-2019
• ICS: 71.100.45 - Refrigerants and antifreezes
• 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 D2982-07(2013) - Standard Test Methods for Detecting Glycol-Base Antifreeze in Used Lubricating Oils
• Effective Date: 01-Dec-2019
• Refers: ASTM D4175-23a - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 15-Dec-2023
• Refers: ASTM D95-23 - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 01-Oct-2023
• Refers: ASTM D4175-23e1 - Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants
• Effective Date: 01-Jul-2023
• Refers: ASTM D4057-06(2011) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 01-Jun-2011
• Refers: ASTM D95-05(2010) - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 01-May-2010
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D95-05 - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 01-Jun-2005
• Refers: ASTM D95-05e1 - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 01-Jun-2005
• Refers: ASTM D4057-95(2000) - Standard Practice for Manual Sampling of Petroleum and Petroleum Products
• Effective Date: 10-Apr-2000
• Refers: ASTM D95-99e1 - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 10-Jun-1999
• Refers: ASTM D95-99 - Standard Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• Effective Date: 10-Jun-1999
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Referred By: ASTM B999-15(2022) - Standard Specification for Titanium and Titanium Alloys Plating, Electrodeposited Coatings of Titanium and Titanium Alloys on Conductive and Non-Conductive Substrate
• Effective Date: 01-Dec-2019

Overview

ASTM D2982-07(2019) Standard Test Methods for Detecting Glycol-Base Antifreeze in Used Lubricating Oils provides qualitative test methods to identify the presence of glycol-based antifreeze, particularly ethylene glycol, in used mineral-based lubricating oils. This standard addresses a critical maintenance and reliability issue in engines and machinery: the contamination of lubricants by antifreeze. Glycol contamination can cause significant engine problems, such as increased sludge and varnish deposits, loss of lubricating effectiveness, and potential engine failure. Early detection of coolant intrusion enables corrective actions to prevent major damage.

Key Topics

• Detection Methods: Two main procedures are described - one using reagent tablets (Procedure A) and one using laboratory shelf reagents (Procedure B). Both are designed to identify ethylene glycol and other 1,2-glycols, even at low levels.
• Sensitivity: Procedure A (tablet method) can detect glycol at concentrations as low as approximately 100 mg/kg, while Procedure B (shelf reagents) is sensitive to about 300 mg/kg of ethylene glycol.
• Interference and Verification: The methods can yield false positives from other glycols or carbohydrates (such as sugars used for sabotage). The standard includes instructions for modifications to address these interferences and guidance on using reference oil samples.
• Field Kit Adaptability: Both methods can be packaged as field kits, allowing for on-site testing and faster decision-making in maintenance scenarios.
• Qualitative Results: The results obtained indicate the presence or absence of glycol-based antifreeze but are not quantitative.

Applications

ASTM D2982 is widely applied in the following scenarios:

• Engine Maintenance and Reliability: Used by engine maintenance personnel to monitor lubricating oil condition and to detect coolant leaks, preventing catastrophic engine damage due to antifreeze contamination.
• Industrial Equipment: Suitable for gear boxes, turbines, and transformers, where maintaining oil purity is essential for optimal equipment performance.
• Oil Analysis Laboratories: Oil testing laboratories utilize these standard methods as part of routine used oil analysis programs for vehicle fleets, heavy machinery, and industrial plants.
• Field Testing: The development of commercial field test kits means that oil samples can be evaluated on-site, providing immediate information and reducing downtime.
• Failure Investigation: When engine or machinery failure occurs, this standard helps determine whether glycol-based coolant played a role, aiding in root cause analysis.

Related Standards

Several ASTM standards are referenced and complement ASTM D2982 in oil and coolant analysis:

• ASTM D95 – Test Method for Water in Petroleum Products and Bituminous Materials by Distillation
• ASTM D1193 – Specification for Reagent Water
• 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

These standards ensure reliability and consistency in sampling, reagent quality, and terminology across petroleum products testing.

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Key SEO keywords: glycol-base antifreeze, used lubricating oil, ethylene glycol detection, ASTM D2982, coolant contamination, oil analysis, field test kit, industrial maintenance, engine oil quality.

By following ASTM D2982-07(2019), maintenance professionals and laboratories can reliably detect and respond to glycol-base antifreeze contamination, protecting engines and equipment from avoidable damage.

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: D2982 − 07 (Reapproved 2019)
Standard Test Methods for
Detecting Glycol-Base Antifreeze in Used Lubricating Oils
This standard is issued under the fixed designation D2982; 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.
2,3
1. Scope 1.5.1 Commercial field testing kits are available.
1.6 The results obtained by this method are qualitative
1.1 These test methods cover the qualitative determination
expressions. However, for the preparation of reagents and in
of glycol-base antifreeze in used lubricating oils (mineral base)
the procedures, acceptable SI units are to be regarded as the
by two procedures, one using reagents in tablet form and the
standard.
other using laboratory shelf reagents. Principally the test
methods detect ethylene glycol but will also detect other 1.7 This standard does not purport to address all of the
1,2-glycols that may be present.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
1.1.1 When a positive result is obtained and a sample of the
priate safety, health, and environmental practices and deter-
unused oil is available, the unused oil is also tested and used as
mine the applicability of regulatory limitations prior to use.
a reference.
1.8 This international standard was developed in accor-
NOTE1—Sincetheinceptionofthistestmethod(1971),therehavebeen
dance with internationally recognized principles on standard-
many changes in base stock technology and additive technology.
ization established in the Decision on Principles for the
Therefore, when available, the new, unused oil, or a sample of the same
Development of International Standards, Guides and Recom-
used oil, known to not contain antifreeze, is tested as a reference.
mendations issued by the World Trade Organization Technical
1.2 The tablet procedure (ProcedureA) is sensitive to about
Barriers to Trade (TBT) Committee.
100 mg/kg and the shelf reagent procedure (Procedure B) to
2. Referenced Documents
about 300 mg/kg of ethylene glycol.
2.1 ASTM Standards:
1.3 Glycol-based coolant leaks into crankcases may not be
D95 Test Method for Water in Petroleum Products and
detected or may result in a low bias using these test methods if
Bituminous Materials by Distillation
the glycol has degraded or been thermally or otherwise
D1193 Specification for Reagent Water
oxidized. The conditions in crankcases may be such that
D4057 Practice for Manual Sampling of Petroleum and
contaminant glycols are oxidized or degraded to a degree to
Petroleum Products
which the color indicator reaction does not occur or is biased
D4175 Terminology Relating to Petroleum Products, Liquid
enough so as to not trigger the color change. Other test
Fuels, and Lubricants
methods for the detection of coolants or coolant additives in
D4177 Practice for Automatic Sampling of Petroleum and
lubricating oils should be used if the results from these test
Petroleum Products
methods alone are inconclusive or questionable.
3. Terminology
1.4 Carbohydrates such as sugars and sugar-containing
3.1 Definitions:
substances are sometimes used for sabotage purposes. If the
3.1.1 glycol-base antifreeze, n—in engine coolants,ethylene
presence of these substances is suspected, Procedure A con-
or propylene glycol commonly used in admixture with water
tains a modification to remove these interferences.
and additives to lower the coolant freezing point.
1.5 Both procedures are adaptable to field kit use, and brief
descriptions for converting to field kit form are given in Annex
The sole source of supply of the apparatus known to the committee at this time
A1.
is the Gly-Tek Test Kit available from the Nelco Co., 1047 McKnight Rd., S., St.
Paul, MN 55119. In Canada, it is available from Metro Tech Preventative
Maintenance Ltd., 112-5621, 11th St., N.E., Calgary, AB, Canada T2E 6Z7.
If you are aware of alternative suppliers, please provide this information to
These test methods are under the jurisdiction of ASTM Committee D02 on ASTM International Headquarters. Your comments will receive careful consider-
Petroleum Products, Liquid Fuels, and Lubricants and are the direct responsibility ation at a meeting of the responsible technical committee, which you may attend.
of Subcommittee D02.06 on Analysis of Liquid Fuels and Lubricants. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2019. Published December 2019. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1971. Last previous edition approved in 2013 as D2982 – 07 (2013). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D2982-07R19. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2982 − 07 (2019)
3.1.2 used oil, n—any oil that has been in a piece of where such specifications are available. Other grades may be
equipment (for example, an engine, gear box, transformer, or used, provided it is first ascertained that the reagent is of
turbine) whether operated or not. sufficiently high purity to permit its use without lessening the
accuracy of the determination.
3.1.2.1 Discussion—In the development of this test method,
the used oil is a mineral lubricating oil from an engine
7.2 Purity of Water—Unless otherwise indicated, references
crankcase. D4175
to water shall be understood to mean distilled water conform-
ing to Type III of Specification D1193.
4. Summary of Test Methods
8. Sampling
4.1 Theethyleneglycolisextractedfromthesamplewithan
8.1 Ethylene glycol is immiscible with and heavier than
acid solution and oxidized to formaldehyde with periodic acid
mineral lubricating oil; hence, it will tend to settle. Do not take
which is detected colorimetrically with decolorized fuchsin.
a sample that is too large to shake vigorously in the laboratory
because vigorous shaking is required before conducting the
5. Significance and Use
test.
5.1 Leakage of glycol-base antifreeze into the crankcase is
8.2 If the sample delivered is too large to be shaken
serious because the coolant tends to interfere with the lubricant
vigorously, then draw the sample to be tested from a low point
and its ability to lubricate; it also promotes sludging. Ethylene
in the container.
glycol present in the coolant can increase varnish deposit
formation in the crankcase as a result of glycol oxidation and
8.3 Under some circumstances ethylene glycol will emul-
the interaction between glycol and lubricant. Furthermore,
sify with the oil to form a sludge. If the sample to be tested is
because glycol is a higher boiling material than water, it will
a sludge, then dilute the sample with a solvent, such as naphtha
tend to stay longer in the crankcase oil than water. Lubricant
or toluene. (Warning—These solvents are toxic and flam-
displacement, sludging, and deposit formation all lead to
mable.) Use a volume of solvent sufficient to provide a fluid
engine malfunction and possible seizure.
sample for the test.
5.2 These tests are designed to detect glycol-base coolant 8.4 When drawing a sample directly from an engine or
contamination even at low levels because early detection machine, ensure that the sample is representative by drawing it
enables corrective measures to be taken to prevent leaking just after the engine or machine has been shut down. If the
coolant from accumulating and seriously damaging the engine. engine or machine has seized, or it has not seized but is not to
be turned over, draw the sample from a low point so as to
5.3 These test methods are also significant because the
sample the settled glycol if present. (Warning—Avoid a top or
reagents can be packaged as a field kit, and the procedure can
dipstick sample because the glycol portion, if present, can be
be followed at the site where there is a concern.
missed.)
8.5 Where applicable, Practice D4057 (manual sampling)
6. Interferences
and Practice D4177 (automatic sampling) will provide useful
6.1 The reactions are not specific to ethylene glycol; other
direction for obtaining consistent and representative samples.
1,2-glycols and many carbohydrates will give a positive test.
Consistent and representative sampling is especially important
6.2 Hexylene glycol and methoxy glycol, which are often when the lubricant is in equipment which is still operational
and other tests on the sample are also required.
used as gasoline anti-icing additives, do not interfere when
present in gasoline-diluted used oils.
PROCEDURE A—USING TABLETS
6.3 Oil oxidation products present do not interfere with the
9. Apparatus
test.
9.1 Graduated Cylinder, glass-stoppered, 100 mL, with
6.4 Some new oils can contain small amounts of glycol
1 mL graduations (two required).
derivativesaspartoftheirmakeupandthusgiveapositivetest.
These oils, after use, invariably give a negative or trace
9.2 Tablet Press—See 10.2.
reaction as the glycol derivatives are slowly destroyed under
conditions of use in the engine. 10. Reagents and Materials
10.1 Acid Solution (12 % by volume)—Add and mix slowly
6.5 AmodificationisdescribedinProcedureAforremoving
with caution 12 volumes of concentrated sulfuric acid (H SO ,
interferences caused by carbohydrates such as sugars and
2 4
relative density 1.84) into 88 volumes of water. (Warning—
sugar-containing substances that are sometimes used for sabo-
Corrosive. Causes severe burns. Mixing sulfuric acid with
tage purposes.
7. Purity of Reagents
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
7.1 Purity of Reagents—Reagent grade chemicals shall be
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
used in all tests. Unless otherwise indicated, it is intended that
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
all reagents shall conform to the specifications of the Commit-
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
tee onAnalytical Reagents of theAmerican Chemical Society, copeial Convention, Inc. (USPC), Rockville, MD.
D2982 − 07 (2019)
water generates heat.Always add the acid to the water and add 11. Preparation of Apparatus
it slowly. Never add the water to the acid.)
11.1 Rinsethecylinderfirstwithtoluenetoremovetheused
6,3
10.2 Potassium Periodate Tablet —(Warning—Toxic. oil/toluene mixture and then with hot water. Dry.
Hazardous.)
11.2 Warning—Do not use soaps or detergents for cleaning
10.2.1 Composition of Tablet:
because they can leave residues that can interfere with the
Ingredient Amount Function
separation of the aqueous layer.
Potassium periodate (Warning—Toxic. 0.3 g ± 0.01 g oxidizing
12. Procedure
Hazardous.) agent
Ammonium chloride 0.9 g ± 0.03 g diluent
12.1 Bring the sample to room temperature and shake well
Sodium bicarbonate 0.3 g ± 0.01 g diffusing agent
toensureevendistributionofanyglycolthroughoutthesample
Polyvinylpyrrolidone (5 mass % 0.01 g binder
7,3
dissolved in isopropyl alcohol)
(Section 8). Use only reagents at room temperature (above
18 °C).
Total weight 1.5 g ± 0.05 g
12.2 Pour toluene into a 100 mLglass-stoppered cylinder to
10.2.2 Preparation of Tablet—Bind chemicals into tablet
the 80 mLmark.Add the well-mixed oil sample to the 100 mL
form not to exceed 13 mm in diameter. The tablet should
mark. Stopper the cylinder and mix well.
withstand reasonable handling and be readily soluble in the
acid solution (Note 2). Store in amber glass bottles with a
12.3 Pouracidsolutionintoanother100 mLglass-stoppered
plastic cap at room temperature and out of direct rays of the
cylinder to the 60 mL mark. Drop a potassium periodate tablet
sun. In this way the tablet will remain stable for at least five
into the acid solution and allow it to dissolve. Bring to the
years.
80 mL mark with the well-mixed toluene/oil mixture from the
other cylinder. Shake vigorously for 1 min, being careful to
NOTE 2—Exercise care in the preparation of the tablets to assure that
avoid leakage of liquid from around the stopper. Remove the
they are not so brittle that they will crumble in handling or not so compact
that they will
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