ASTM D2982-98(2004)
(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
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.
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.
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 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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An American National Standard
Designation:D2982–98 (Reapproved 2004)
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 2. Referenced Documents
1.1 These test methods describe the qualitative determina- 2.1 ASTM Standards:
tion of glycol-base antifreeze in used lubricating oils (mineral D95 Test Method for Water in Petroleum Products and
base) by two procedures, one using reagents in tablet form and Bituminous Materials by Distillation
the other using laboratory shelf reagents. Principally the test D 1193 Specification for Reagent Water
methods detect ethylene glycol but will also detect other D 4057 Practice for Manual Sampling of Petroleum and
1,2-glycols that may be present. Petroleum Products
1.1.1 When a positive result is obtained and a sample of the D 4175 Terminology Relating to Petroleum, Petroleum
unused oil is available, the unused oil is also tested and used as Products, and Lubricants
a reference. D 4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
NOTE 1—Since the inception of this test method (1971), there have
been many changes in base stock technology and additive technology.
3. Terminology
Therefore, when available, the new, unused oil, or a sample of the same
3.1 Definitions:
used oil, known to not contain antifreeze, is tested as a reference.
3.1.1 glycol-base antifreeze, n— in engine coolants, ethyl-
1.2 The tablet procedure (ProcedureA) is sensitive to about
ene or propylene glycol commonly used in admixture with
100 mg/kg and the shelf reagent procedure (Procedure B) to
water and additives to lower the coolant freezing point.
about 300 mg/kg of ethylene glycol.
3.1.2 used oil, n—any oil that has been in a piece of
1.3 Carbohydrates such as sugars and sugar-containing
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.
the used oil is a mineral lubricating oil from an engine
1.4 Both procedures are adaptable to field kit use, and brief
crankcase. D4175
descriptions for converting to field kit form are given inAnnex
A1.
4. Summary of Test Methods
1.4.1 Commercial field testing kits are available.
4.1 Theethyleneglycolisextractedfromthesamplewithan
1.5 The results obtained by this method are qualitative
acid solution and oxidized to formaldehyde with periodic acid
expressions. However, for the preparation of reagents and in
which is detected colorimetrically with decolorized fuchsin.
the procedures, acceptable SI units are to be regarded as the
standard.
5. Significance and Use
1.6 This standard does not purport to address all of the
5.1 Leakage of glycol-base antifreeze into the crankcase is
safety concerns, if any, associated with its use. It is the
serious because the coolant tends to interfere with the lubricant
responsibility of the user of this standard to establish appro-
and its ability to lubricate; it also promotes sludging. Ethylene
priate safety and health practices and determine the applica-
glycol present in the coolant can increase varnish deposit
bility of regulatory limitations prior to use.
formation in the crankcase as a result of glycol oxidation and
the interaction between glycol and lubricant. Furthermore,
These test methods are under the jurisdiction of ASTM Committee D02 on
because glycol is a higher boiling material than water, it will
Petroleum Products and Lubricants and are the direct responsibility of Subcommit-
tend to stay longer in the crankcase oil than water. Lubricant
tee D02.06 on Analysis of Lubricants.
Current edition approved Dec. 1, 2004. Published December 2004. Originally
e1
approved in 1971. Last previous edition approved in 1998 as D 2982 – 98 .
2 3
The Gly-Tek Test Kit is available from the Nelco Co., 1047 McKnight Rd., S., For referenced ASTM standards, visit the ASTM website, www.astm.org, or
St. Paul, MN 55119, and in Canada, it is available from Metro Tech Preventative contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
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instructions are provided with the kit. the ASTM website.
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D2982–98 (2004)
displacement, sludging, and deposit formation all lead to asludge,thendilutethesamplewithasolvent,suchasnaphtha
engine malfunction and possible seizure. or toluene. (Warning—These solvents are toxic and flam-
5.2 These tests are designed to detect glycol-base coolant mable.) Use a volume of solvent sufficient to provide a fluid
contamination even at low levels because early detection sample for the test.
enables corrective measures to be taken to prevent leaking 8.4 When drawing a sample directly from an engine or
coolant from accumulating and seriously damaging the engine. machine, ensure that the sample is representative by drawing it
5.3 These test methods are also significant because the just after the engine or machine has been shut down. If the
reagents can be packaged as a field kit, and the procedure can engine or machine has seized, or it has not seized but is not to
be followed at the site where there is a concern. be turned over, draw the sample from a low point so as to
sample the settled glycol if present. (Warning—Avoid a top or
6. Interferences
dipstick sample because the glycol portion, if present, can be
6.1 The reactions are not specific to ethylene glycol; other missed.)
1,2-glycols and many carbohydrates will give a positive test. 8.5 Where applicable, Practice D 4057 (manual sampling)
6.2 Hexylene glycol and methoxy glycol, which are often and Practice D 4177 (automatic sampling) will provide useful
used as gasoline anti-icing additives, do not interfere when direction for obtaining consistent and representative samples.
Consistent and representative sampling is especially important
present in gasoline-diluted used oils.
6.3 Oil oxidation products present do not interfere with the when the lubricant is in equipment which is still operational
and other tests on the sample are also required.
test.
6.4 Some new oils can contain small amounts of glycol
PROCEDURE A—USING TABLETS
derivativesaspartoftheirmakeupandthusgiveapositivetest.
These oils, after use, invariably give a negative or trace
9. Apparatus
reaction as the glycol derivatives are slowly destroyed under
9.1 Graduated Cylinder, glass-stoppered, 100 mL, with
conditions of use in the engine.
1-mL graduations (two required).
6.5 AmodificationisdescribedinProcedureAforremoving
9.2 Tablet Press—See 10.2.
interferences caused by carbohydrates such as sugars and
sugar-containing substances that are sometimes used for sabo-
10. Reagents and Materials
tage purposes.
10.1 Acid Solution (12 volume %)—Add and mix slowly
7. Purity of Reagents with caution 12 volumes of concentrated sulfuric acid (H SO ,
2 4
relative density 1.84) into 88 volumes of water. (Warning—
7.1 Purity of Reagents—Reagent grade chemicals shall be
Corrosive. Causes severe burns. Mixing sulfuric acid with
used in all tests. Unless otherwise indicated, it is intended that
water generates heat.Always add the acid to the water and add
all reagents shall conform to the specifications of the Commit-
it slowly. Never add the water to the acid.)
tee onAnalytical Reagents of theAmerican Chemical Society,
10.2 Potassium Periodate Tablet. (Warning—Toxic. Haz-
where such specifications are available. Other grades may be
ardous.)
used, provided it is first ascertained that the reagent is of
10.2.1 Composition of Tablet:
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
Ingredient Amount Function
7.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean distilled water conform-
Potassium periodate (Caution—Toxic. 0.3 6 0.01 g oxidizing
ing to Type III of Specification D 1193.
Hazardous.) agent
Ammonium chloride 0.9 6 0.03 g diluent
Sodium bicarbonate 0.3 6 0.01 g diffusing agent
8. Sampling
Polyvinylpyrrolidone (5 mass % 0.01 g binder
8.1 Ethylene glycol is immiscible with and heavier than dissolved in isopropyl alcohol)
mineral lubricating oil; hence, it will tend to settle. Do not take
Total weight 1.5 6 0.05 g
a sample that is too large to shake vigorously in the laboratory
because vigorous shaking is required before conducting the
10.2.2 Preparation of Tablet—Bind chemicals into tablet
test.
form not to exceed 13 mm in diameter. The tablet should
8.2 If the sample delivered is too large to be shaken
vigorously, then draw the sample to be tested from a low point
in the container.
Suitable potassium periodate and sodium sulfite/pararosaniline hydrochloride
tabletsareavailablefromAccurateManufacturingChemicalsInc.,POBox26,Cote
8.3 Under some circumstances ethylene glycol will emul-
St., Lue Station, Montreal, Quebec, Canada H4V 1H8 and from Technical Products
sify with the oil to form a sludge. If the sample to be tested is
Inc.,POBox11428,Baltimore,MD21239.Ifyouareawareofalternativesuppliers,
please provide this information to ASTM International Headquarters. Your com-
ments will receive careful consideration at a meeting of the responsible technical
Reagent Chemicals, American Chemical Society Specifications, American committee , which you may attend.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not Polyvinylpyrrolidone is available as “Plasdone” from Antara Chemicals Divi-
listed by the American Chemical Society, see Analar Standards for Laboratory sion of General Aniline and Film Corp., New York, NY. If you are aware of
Chemicals,BDHLtd.,Poole,Dorset,U.K.andthe United States Pharmacopeia and alternative suppliers, please provide this information to ASTM International
National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, Headquarters.Your comments will receive careful consideration at a meeting of the
MD. responsible technical committee , which you may attend.
D2982–98 (2004)
withstand reasonable handling and be readily soluble in the periodate tablet into the acid solution and allow it to dissolve.
acid solution (Note 2). Store in amber glass bottles with a Bring to the 80-mL mark with the well-mixed toluene/oil
plastic cap at room temperature and out of direct rays of the mixture from the other cylinder. Shake vigorously for 1 min,
sun. In this way the tablet will remain stable for at least five being careful to avoid leakage of liquid from around the
years. stopper. Remove the stopper and let the cylinder stand for 10
min.
NOTE 2—Exercise care in the preparation of the tablets to assure that
12.4 Drop in a sulfite/pararosaniline tablet and wait for 30
they are not so brittle that they will crumble in handling or not so compact
min. Upon addition of the tablet, effervescence commences,
that they will not readily dissolve in the acid solution.
and a deep brownish color develops in the aqueous layer in
10.3 Sodium Sulfite/Pararosaniline Hydrochloride Tablet
about 1 min and then disappears.
(Warning—Toxic. Hazardous.)
12.5 Afterthedisappearanceofthebrowncolor,observethe
10.3.1 Composition of Tablet:
formation of color in the aqueous layer.
Ingredient Amount Function
13. Observations and Interpretations
13.1 Regard a yellow or pale green coloration that persists
Sodium sulfite (Caution—Toxic. 1.05 6 0.03 g reducing agent
Hazardous.)
for at least 30 min as a negative test result.
Pararosaniline hydrochloride (Caution— 0.01 6 0.001 g indicator
13.2 Regard a pale, dirty green color that gradually turns to
Toxic. Hazardous.)
Sodium bicarbonate 0.42 6 0.01 g diffusing agent purple in 30 min as a trace test result. This trace quantity is in
Magnesium stearate 0.01 g lubricant
the range of 100 to 300 mg/kg.
Polyvinylpyrrolidone (5 mass % 0.01 g binder
6 13.3 Regard a purple color, which may intensify upon
dissolved in isopropyl alcohol)
standing for 30 min, as a positive test result. When the purple
color appears within a few minutes, more than 1 % glycol is
Total weight 1.50 6 0.04 g
present.
10.3.2 Preparation of Tablet—Mix and grind together the
13.4 When the test result is positive or trace, and sugar or
sodium sulfite, sodium bicarbonate, and the pararosaniline
sugar-containing materials are suspected of being present,
hydrochloride. Pass the mixture through a 180-µm (80-mesh)
instead of performing the test directly on the toluene/oil
sieve, dampen with the polyvinylpyrrolidone in alcohol, and
mixture (12.2), do a water test (Test MethodD95 first on the
pass through a 425-µm (40-mesh) sieve. Dry for4hat 380°C
100 mLof this mixture, transfer the condensed trap contents to
and overnight at room temperature. Pass through a 500-µm
the acid/periodate solution in the glass-stoppered cylinder
(30-mesh) sieve. Sprinkle with magnesium stearate and mix.
(12.3), and carry out the rest of the antifreeze test. Discard the
Press into tablet form not to exceed 13 mm in diameter. The
oil/solvent residue from the water test that would contain any
tablet should withstand reasonable handling and be readily
sugar. The presence or absence of interfering compounds from
soluble in the acid solution (Note 2). Store in an amber glass
manufacture can be confirmed by carrying out the test on new
bottle with plastic cap at room temperature or lower and out of
or preferably on the used oil known not to be contaminated by
the direct rays of the sun. In this way, the tablets will remain
glycol-baseantifreezeastheconcentrationofthesecompounds
stable for at least five years.
tends to diminish in use. Allow for such interference when
10.4 Toluene—(Warning—Toxic. Flammable.)
reporting results.
13.5 When a positive test result is obtained, perform the test
11. Preparation of Apparatus
on the same oil, unused, or the same oil, used and known to
11.1 Rinsethecylinderfirstwithtoluenetoremovetheused
contain no antifreeze. A difference in the color formation,
oil/toluene mixture and then with hot water. Dry.
especially a bluish tint, between the blank and the used oil
11.2 Caution—Do
...
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