ASTM D2982-98
(Test Method)Standard Test Methods for Detecting Glycol-Base Antifreeze in Used Lubricating Oils
Standard Test Methods for Detecting Glycol-Base Antifreeze in Used Lubricating Oils
SCOPE
1.1 These test methods describe 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 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.
1.4 Both procedures are adaptable to field kit use, and brief descriptions for converting to field kit form are given in .
1.4.1 Commercial field testing kits are available.
1.5 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.
1.6 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.
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Designation: D 2982 – 98
Standard Test Methods for
Detecting Glycol-Base Antifreeze in Used Lubricating Oils
This standard is issued under the fixed designation D 2982; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope D 95 Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation
1.1 These test methods describe the qualitative determina-
D 1193 Specification for Reagent Water
tion of glycol-base antifreeze in used lubricating oils (mineral
D 4057 Practice for Manual Sampling of Petroleum and
base) by two procedures, one using reagents in tablet form and
Petroleum Products
the other using laboratory shelf reagents. Principally the test
D 4175 Terminology Relating to Petroleum, Petroleum
methods detect ethylene glycol but will also detect other
Products, and Lubricants
1,2-glycols that may be present.
D 4177 Practice for Automatic Sampling of Petroleum
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
3. Terminology
a reference.
3.1 Definitions:
NOTE 1—Since the inception of this test method (1971), there have
3.1.1 glycol-base antifreeze, n— in engine coolants, ethyl-
been many changes in base stock technology and additive technology.
ene or propylene glycol commonly used in admixture with
Therefore, when available, the new, unused oil, or a sample of the same
water and additives to lower the coolant freezing point.
used oil, known to not contain antifreeze, is tested as a reference.
3.1.2 used oil, n—any oil that has been in a piece of
1.2 The tablet procedure (Procedure A) is sensitive to about
equipment (for example, an engine, gear box, transformer, or
100 mg/kg and the shelf reagent procedure (Procedure B) to
turbine) whether operated or not.
about 300 mg/kg of ethylene glycol.
3.1.2.1 Discussion—In the development of this test method,
1.3 Carbohydrates such as sugars and sugar-containing
the used oil is a mineral lubricating oil from an engine
substances are sometimes used for sabotage purposes. If the
crankcase. D 4175
presence of these substances is suspected, Procedure A con-
tains a modification to remove these interferences.
4. Summary of Test Methods
1.4 Both procedures are adaptable to field kit use, and brief
4.1 The ethylene glycol is extracted from the sample with an
descriptions for converting to field kit form are given in Annex
acid solution and oxidized to formaldehyde with periodic acid
A1.
which is detected colorimetrically with decolorized fuchsin.
1.4.1 Commercial field testing kits are available.
1.5 The results obtained by this method are qualitative 5. Significance and Use
expressions. However, for the preparation of reagents and in
5.1 Leakage of glycol-base antifreeze into the crankcase is
the procedures, acceptable SI units are to be regarded as the
serious because the coolant tends to interfere with the lubricant
standard.
and its ability to lubricate; it also promotes sludging. Ethylene
1.6 This standard does not purport to address all of the
glycol present in the coolant can increase varnish deposit
safety concerns, if any, associated with its use. It is the
formation in the crankcase as a result of glycol oxidation and
responsibility of the user of this standard to establish appro-
the interaction between glycol and lubricant. Furthermore,
priate safety and health practices and determine the applica-
because glycol is a higher boiling material than water, it will
bility of regulatory limitations prior to use.
tend to stay longer in the crankcase oil than water. Lubricant
displacement, sludging, and deposit formation all lead to
2. Referenced Documents
engine malfunction and possible seizure.
2.1 ASTM Standards:
5.2 These tests are designed to detect glycol-base coolant
contamination even at low levels because early detection
These test methods are under the jurisdiction of ASTM Committee D-2 on
enables corrective measures to be taken to prevent leaking
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
coolant from accumulating and seriously damaging the engine.
tee D02.06 on Analysis of Lubricants.
5.3 These test methods are also significant because the
Current edition approved Dec. 10, 1998. Published February 1999. Originally
published as D 2982 – 71 T. Last previous edition D 2982 – 93.
The Gly-Tek Test Kit is available from the Nelco Co., 1047 McKnight Rd., S.,
St. Paul, MN 55119, and in Canada, it is available from Metro Tech Preventative Annual Book of ASTM Standards, Vol 05.01.
Maintenance Ltd., 112-5621, 11th St., N.E., Calgary, AB, Canada T2E 6Z7. Test Annual Book of ASTM Standards, Vol 11.01.
instructions are provided with the kit. Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 2982
reagents can be packaged as a field kit, and the procedure can just after the engine or machine has been shut down. If the
be followed at the site where there is a concern. 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
6. Interferences
sample the settled glycol if present.
6.1 The reactions are not specific to ethylene glycol; other
NOTE 3—Caution: Avoid a top or dipstick sample because the glycol
1,2-glycols and many carbohydrates will give a positive test.
portion, if present, can be missed.
6.2 Hexylene glycol and methoxy glycol, which are often
8.5 Where applicable, Practice D 4057 (manual sampling)
used as gasoline anti-icing additives, do not interfere when
and Practice D 4177 (automatic sampling) will provide useful
present in gasoline-diluted used oils.
direction for obtaining consistent and representative samples.
6.3 Oil oxidation products present do not interfere with the
Consistent and representative sampling is especially important
test.
when the lubricant is in equipment which is still operational
6.4 Some new oils can contain small amounts of glycol
and other tests on the sample are also required.
derivatives as part of their makeup and thus give a positive test.
These oils, after use, invariably give a negative or trace
PROCEDURE A—USING TABLETS
reaction as the glycol derivatives are slowly destroyed under
conditions of use in the engine.
9. Apparatus
6.5 A modification is described in Procedure A for removing
9.1 Graduated Cylinder, glass-stoppered, 100 mL, with
interferences caused by carbohydrates such as sugars and
1-mL graduations (two required).
sugar-containing substances that are sometimes used for sabo-
9.2 Tablet Press—See 10.2.
tage purposes.
10. Reagents and Materials
7. Purity of Reagents
10.1 Acid Solution (12 volume %)—Add and mix slowly
7.1 Purity of Reagents—Reagent grade chemicals shall be
with caution 12 volumes of concentrated sulfuric acid (H SO ,
2 4
used in all tests. Unless otherwise indicated, it is intended that
relative density 1.84) into 88 volumes of water. (Warning—
all reagents shall conform to the specifications of the Commit-
See Note 4 and Note 5.)
tee on Analytical Reagents of the American Chemical Society,
where such specifications are available. Other grades may be
NOTE 4—Warning: Corrosive. Causes severe burns.
used, provided it is first ascertained that the reagent is of
NOTE 5—Precaution: Mixing sulfuric acid with water generates heat.
Always add the acid to the water and add it slowly. Never add the water
sufficiently high purity to permit its use without lessening the
to the acid.
accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, references
10.2 Potassium Periodate Tablet. (Warning—See Note
to water shall be understood to mean distilled water conform-
6.)
ing to Type III of Specification D 1193.
NOTE 6—Warning: Toxic. Hazardous.
8. Sampling
10.2.1 Composition of Tablet:
8.1 Ethylene glycol is immiscible with and heavier than
mineral lubricating oil; hence, it will tend to settle. Do not take
Ingredient Amount Function
a sample that is too large to shake vigorously in the laboratory
Potassium periodate (Caution—Toxic. 0.3 6 0.01 g oxidizing
because vigorous shaking is required before conducting the
Hazardous.) agent
test. Ammonium chloride 0.9 6 0.03 g diluent
Sodium bicarbonate 0.3 6 0.01 g diffusing agent
8.2 If the sample delivered is too large to be shaken
Polyvinylpyrrolidone (5 mass % 0.01 g binder
vigorously, then draw the sample to be tested from a low point 8
dissolved in isopropyl alcohol)
in the container.
8.3 Under some circumstances ethylene glycol will emul-
Total weight 1.5 6 0.05 g
sify with the oil to form a sludge. If the sample to be tested is
10.2.2 Preparation of Tablet—Bind chemicals into tablet
a sludge, then dilute the sample with a solvent, such as naphtha
form not to exceed 13 mm in diameter. The tablet should
or toluene. ( Warning—See Note 2.) Use a volume of solvent
withstand reasonable handling and be readily soluble in the
sufficient to provide a fluid sample for the test.
acid solution (Note 7). Store in amber glass bottles with a
NOTE 2—Warning: These solvents are toxic and flammable.
plastic cap at room temperature and out of direct rays of the
sun. In this way the tablet will remain stable for at least five
8.4 When drawing a sample directly from an engine or
years.
machine, ensure that the sample is representative by drawing it
6 7
Reagent Chemicals, American Chemical Society Specifications, American Suitable potassium periodate and sodium sulfite/pararosaniline hydrochloride
Chemical Society, Washington, DC. For suggestions on the testing of reagents not tablets are available from Accurate Manufacturing Chemicals Inc., PO Box 26, Cote
listed by the American Chemical Society, see Analar Standards for Laboratory St., Lue Station, Montreal, Quebec, Canada H4V 1H8 and from Technical Products
Chemicals, BDH Ltd., Poole, Dorset, U.K. and the United States Pharmacopeia and Inc., PO Box 11428, Baltimore, MD 21239.
National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, Polyvinylpyrrolidone is available as “Plasdone” from Antara Chemicals Divi-
MD. sion of General Aniline and Film Corp., New York, NY.
D 2982
NOTE 7—Exercise care in the preparation of the tablets to assure that
about 1 min and then disappears.
they are not so brittle that they will crumble in handling or not so compact
12.5 After the disappearance of the brown color, observe the
that they will not readily dissolve in the acid solution.
formation of color in the aqueous layer.
10.3 Sodium Sulfite/Pararosaniline Hydrochloride Tablet
13. Observations and Interpretations
(Warning See Note 6.)
10.3.1 Composition of Tablet:
13.1 Regard a yellow or pale green coloration that persists
for at least 30 min as a negative test result.
Ingredient Amount Function
13.2 Regard a pale, dirty green color that gradually turns to
purple in 30 min as a trace test result. This trace quantity is in
Sodium sulfite (Caution—Toxic. 1.05 6 0.03 g reducing agent
the range of 100 to 300 mg/kg.
Hazardous.)
Pararosaniline hydrochloride (Caution— 0.01 6 0.001 g indicator 13.3 Regard a purple color, which may intensify upon
Toxic. Hazardous.)
standing for 30 min, as a positive test result. When the purple
Sodium bicarbonate 0.42 6 0.01 g diffusing agent
color appears within a few minutes, more than 1 % glycol is
Magnesium stearate 0.01 g lubricant
Polyvinylpyrrolidone (5 mass % 0.01 g binder
present.
dissolved in isopropyl alcohol)
13.4 When the test result is positive or trace, and sugar or
sugar-containing materials are suspected of being present,
Total weight 1.50 6 0.04 g
instead of performing the test directly on the toluene/oil
10.3.2 Preparation of Tablet—Mix and grind together the
mixture (12.2), do a water test (Test Method D 95 first on the
sodium sulfite, sodium bicarbonate, and the pararosaniline
100 mL of this mixture, transfer the condensed trap contents to
hydrochloride. Pass the mixture through a 180-μm (80-mesh) the acid/periodate solution in the glass-stoppered cylinder
sieve, dampen with the polyvinylpyrrolidone in alcohol, and
(12.3), and carry out the rest of the antifreeze test. Discard the
pass through a 425-μm (40-mesh) sieve. Dry for4hat 380°C oil/solvent residue from the water test that would contain any
and overnight at room temperature. Pass through a 500-μm
sugar. The presence or absence of interfering compounds from
(30-mesh) sieve. Sprinkle with magnesium stearate and mix.
manufacture can be confirmed by carrying out the test on new
Press into tablet form not to exceed 13 mm in diameter. The
or preferably on the used oil known not to be contaminated by
tablet should withstand reasonable handling and be readily
glycol-base antifreeze as the concentration of these compounds
soluble in the acid solution (Note 7). Store in an amber glass
tends to diminish in use. Allow for such interference when
bottle with plastic cap at room temperature or lower and out of
reporting results.
the direct rays of the sun. In this way, the tablets will remain
13.5 When a positive test result is obtained, perform the test
stable for at least five years.
on the same oil, unused, or the same oil, used and known to
10.4 Toluene—(Warning—See Note 8.)
contain no antifreeze. A difference in the color formation,
especially a bluish tint, between the blank and the used oil
NOTE 8—Warning: Toxic. Flammable.
indicates a positive result. A positive result cannot be con-
11. Preparation of Apparatus
firmed if there is no difference between the color formation of
the blank and used oil.
11.1 Rinse the cylinder first with toluene to remove the used
13.6 A light red (13.2) or a deep red (13.3) may also be an
oil/toluene mixture and then with hot water. Dry.
indication of a positive test. However this can be confirmed by
11.2 Caution—Do not use soaps or detergents for cleaning
testing the color formation in the same oil, unused, or on the
because they can leave residues that can interfere with the
same used oil which is known to contain no antifreeze. A
separation of the aqueous layer.
difference in the color formation, especially a bluish tint,
12. Procedure
between the blank and the used oil indicates a positive result.
12.1 Bring the sample to room temperature and shake well
A positive result cannot be confirmed if there is no difference
to ensure even distribution of any glycol throughout the sample
between the color formation of the blank and used oil.
(Section 8). Use only reagents at room te
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