ASTM D2982-07(2013)
(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
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
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Designation: D2982 − 07 (Reapproved 2013)
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
ofglycol-baseantifreezeinusedlubricatingoils(mineralbase)
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 and health practices and determine the applica-
unused oil is available, the unused oil is also tested and used as
bility of regulatory limitations prior to use.
a reference.
NOTE1—Sincetheinceptionofthistestmethod(1971),therehavebeen
2. Referenced Documents
many changes in base stock technology and additive technology.
2.1 ASTM Standards:
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. D95 Test Method for Water in Petroleum Products and
Bituminous Materials by Distillation
1.2 The tablet procedure (ProcedureA) is sensitive to about
D1193 Specification for Reagent Water
100 mg/kg and the shelf reagent procedure (Procedure B) to
D4057 Practice for Manual Sampling of Petroleum and
about 300 mg/kg of ethylene glycol.
Petroleum Products
1.3 Glycol-based coolant leaks into crankcases may not be D4175 Terminology Relating to Petroleum, Petroleum
detected or may result in a low bias using these test methods if Products, and Lubricants
the glycol has degraded or been thermally or otherwise D4177 Practice for Automatic Sampling of Petroleum and
oxidized. The conditions in crankcases may be such that Petroleum Products
contaminant glycols are oxidized or degraded to a degree to
3. Terminology
which the color indicator reaction does not occur or is biased
enough so as to not trigger the color change. Other test
3.1 Definitions:
methods for the detection of coolants or coolant additives in
3.1.1 glycol-base antifreeze, n—in engine coolants,ethylene
lubricating oils should be used if the results from these test
or propylene glycol commonly used in admixture with water
methods alone are inconclusive or questionable.
and additives to lower the coolant freezing point.
1.4 Carbohydrates such as sugars and sugar-containing 3.1.2 used oil, n—any oil that has been in a piece of
equipment (for example, an engine, gear box, transformer, or
substances are sometimes used for sabotage purposes. If the
turbine) whether operated or not.
presence of these substances is suspected, Procedure A con-
3.1.2.1 Discussion—In the development of this test method,
tains 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
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 and Lubricants and are the direct responsibility of Subcommit- ation at a meeting of the responsible technical committee, which you may attend.
tee D02.06 on Analysis of Lubricants. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2013. Published August 2013. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1971. Last previous edition approved in 2007 as D2982 – 07. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D2982-07R13. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D2982 − 07 (2013)
the used oil is a mineral lubricating oil from an engine where such specifications are available. Other grades may be
crankcase. D4175 used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
4. Summary of Test Methods accuracy of the determination.
4.1 Theethyleneglycolisextractedfromthesamplewithan 7.2 Purity of Water—Unless otherwise indicated, references
acid solution and oxidized to formaldehyde with periodic acid to water shall be understood to mean distilled water conform-
which is detected colorimetrically with decolorized fuchsin. ing to Type III of Specification D1193.
8. Sampling
5. Significance and Use
5.1 Leakage of glycol-base antifreeze into the crankcase is 8.1 Ethylene glycol is immiscible with and heavier than
mineral lubricating oil; hence, it will tend to settle. Do not take
serious because the coolant tends to interfere with the lubricant
and its ability to lubricate; it also promotes sludging. Ethylene a sample that is too large to shake vigorously in the laboratory
because vigorous shaking is required before conducting the
glycol present in the coolant can increase varnish deposit
formation in the crankcase as a result of glycol oxidation and test.
the interaction between glycol and lubricant. Furthermore,
8.2 If the sample delivered is too large to be shaken
because glycol is a higher boiling material than water, it will
vigorously, then draw the sample to be tested from a low point
tend to stay longer in the crankcase oil than water. Lubricant
in the container.
displacement, sludging, and deposit formation all lead to
engine malfunction and possible seizure. 8.3 Under some circumstances ethylene glycol will emul-
sify with the oil to form a sludge. If the sample to be tested is
5.2 These tests are designed to detect glycol-base coolant
asludge,thendilutethesamplewithasolvent,suchasnaphtha
contamination even at low levels because early detection
or toluene. (Warning—These solvents are toxic and flam-
enables corrective measures to be taken to prevent leaking
mable.) Use a volume of solvent sufficient to provide a fluid
coolant from accumulating and seriously damaging the engine.
sample for the test.
5.3 These test methods are also significant because the
8.4 When drawing a sample directly from an engine or
reagents can be packaged as a field kit, and the procedure can
machine, ensure that the sample is representative by drawing it
be followed at the site where there is a concern.
just after the engine or machine has been shut down. If the
engine or machine has seized, or it has not seized but is not to
6. Interferences
be turned over, draw the sample from a low point so as to
6.1 The reactions are not specific to ethylene glycol; other sample the settled glycol if present. (Warning—Avoid a top or
1,2-glycols and many carbohydrates will give a positive test. dipstick sample because the glycol portion, if present, can be
missed.)
6.2 Hexylene glycol and methoxy glycol, which are often
used as gasoline anti-icing additives, do not interfere when 8.5 Where applicable, Practice D4057 (manual sampling)
present in gasoline-diluted used oils. and Practice D4177 (automatic sampling) will provide useful
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
and other tests on the sample are also required.
6.4 Some new oils can contain small amounts of glycol
derivativesaspartoftheirmakeupandthusgiveapositivetest.
PROCEDURE A—USING TABLETS
These oils, after use, invariably give a negative or trace
reaction as the glycol derivatives are slowly destroyed under
9. Apparatus
conditions of use in the engine.
9.1 Graduated Cylinder, glass-stoppered, 100 mL, with
6.5 AmodificationisdescribedinProcedureAforremoving
1-mL graduations (two required).
interferences caused by carbohydrates such as sugars and
sugar-containing substances that are sometimes used for sabo-
9.2 Tablet Press—See 10.2.
tage purposes.
7. Purity of Reagents
Reagent Chemicals, American Chemical Society Specifications , American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
7.1 Purity of Reagents—Reagent grade chemicals shall be
listed by the American Chemical Society, see Analar Standards for Laboratory
used in all tests. Unless otherwise indicated, it is intended that
Chemicals,BDHLtd.,Poole,Dorset,U.K.andthe United States Pharmacopeia and
all reagents shall conform to the specifications of the Commit-
National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
tee onAnalytical Reagents of theAmerican Chemical Society, MD.
D2982 − 07 (2013)
10. Reagents and Materials soluble in the acid solution (Note 2). Store in an amber glass
bottle with plastic cap at room temperature or lower and out of
10.1 Acid Solution (12 volume %)—Add and mix slowly
the direct rays of the sun. In this way, the tablets will remain
with caution 12 volumes of concentrated sulfuric acid (H SO ,
2 4
stable for at least five years.
relative density 1.84) into 88 volumes of water. (Warning—
Corrosive. Causes severe burns. Mixing sulfuric acid with 10.4 Toluene—(Warning—Toxic. Flammable.)
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.)
6,3
11.1 Rinsethecylinderfirstwithtoluenetoremovetheused
10.2 Potassium Periodate Tablet —(Warning—Toxic.
oil/toluene mixture and then with hot water. Dry.
Hazardous.)
10.2.1 Composition of Tablet:
11.2 Warning—Do not use soaps or detergents for cleaning
Ingredient Amount Function
because they can leave residues that can interfere with the
separation of the aqueous layer.
Potassium periodate (Warning—Toxic. 0.3 ± 0.01 g oxidizing
Hazardous.) agent
Ammonium chloride 0.9 ± 0.03 g diluent 12. Procedure
Sodium bicarbonate 0.3 ± 0.01 g diffusing agent
12.1 Bring the sample to room temperature and shake well
Polyvinylpyrrolidone (5 mass % 0.01 g binder
7,3
dissolved in isopropyl alcohol)
toensureevendistributionofanyglycolthroughoutthesample
(Section 8). Use only reagents at room temperature (above
Total weight 1.5 ± 0.05 g
18°C).
10.2.2 Preparation of Tablet—Bind chemicals into tablet
12.2 Pour toluene into a 100-mLglass-stoppered cylinder to
form not to exceed 13 mm in diameter. The tablet should
the 80-mLmark.Add the well-mixed oil sample to the 100-mL
withstand reasonable handling and be readily soluble in the
mark. Stopper the cylinder and mix well.
acid solution (Note 2). Store in amber glass bottles with a
plastic cap at room temperature and out of direct rays of the
12.3 Pour acid solution into another 100-mL glass-
sun. In this way the tablet will remain stable for at least five
stoppered cylinder to the 60-mL mark. Drop a potassium
years.
periodate tablet into the acid solution and allow it to dissolve.
Bring to the 80-mL mark with the well-mixed toluene/oil
NOTE 2—Exercise care in the preparation of the tablets to assure that
mixture from the other cylinder. Shake vigorously for 1 min,
they are not so brittle that they will crumble in handling or not so compact
that they will not readily dissolve in the acid solution. being careful to avoid leakage of liquid from around the
stopper. Remove the stopper and let the cylinder stand for 10
10.3 Sodium Sulfite/Pararosaniline Hydrochloride
6,3
min.
Tablet —(Warning—Toxic. Hazardous.)
10.3.1 Composition of Tablet:
12.4 Drop in a sulfite/pararosaniline tablet and wait for 30
min. Upon addition of the tablet, effervescence commences,
Ingredient Amount Function
and a deep brownish color develops in the aqueous layer in
Sodium sulfite (Warning—Toxic. 1.05 ± 0.03 g reducing agent
about 1 min and then disappears.
Hazardous.)
Pararosaniline hydrochloride (Warning— 0.01 ± 0.001 g indicator
12.5 Afterthedisappearanceofthebrowncolor,observethe
Toxic. Hazardous.)
formation of color in the aqueous layer.
Sodium bicarbonate 0.42 ± 0.01 g diffusing agent
Magnesium stearate 0.01 g lubricant
Polyvinylpyrrolidone (5 mass % 0.01 g binder
13. Observations and Interpretations
7,3
dissolved in isopropyl alcohol)
13.1 Regard a yellow or pale green coloration that persists
Total weight 1.50 ± 0.04 g
for at least 30 min as a negative test result.
10.3.2 Preparation of Tablet—Mix and grind together the
13.2 Regard a pale, dirty green color that gradually turns to
sodium sulfite, sodium bicarbonate, and the pararosaniline
purple in 30 min as a trace test result. This trace quantity is in
hydrochloride. Pass the mixture through a 180-µm (80-mesh)
the range of 100 to 300 mg/kg.
sieve, dampen with the polyvinylpyrrolidone in alcohol, and
13.3 Regard a purple color, which may intensify upon
pass through a 425-µm (40-mesh) sieve. Dry for4hat 380°C
standing for 30 min, as a positive test result. When the purple
and overnight at room temperature. Pass through a 500-µm
color appears within a few minutes, more than 1 % glycol is
(30-mesh) sieve. Sprinkle with magnesium stearate and mix.
present.
Press into tablet form not to exceed 13 mm in diameter. The
tablet should withstand reasonable handling and be readily
13.4 When the test result is positive or trace, and sugar or
sugar-containing materials are suspected of being present,
instead of performing the test directly on the toluene/oil
The sole source of supply of the apparatus known to the committee at this time
mixture (12.2), do a water test (Test Method D95 first on the
is potassium periodate and sodium sulfite/pararosaniline hydrochloride tablets
100 mLof this mixture, transfer the condensed trap contents to
available from Accurate Manufacturing C
...
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