1、Designation: D 2982 07An American National StandardStandard Test Methods forDetecting Glycol-Base Antifreeze in Used Lubricating Oils1This standard is issued under the fixed designation D 2982; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、 revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 These test methods cover the qualitative determinationof glycol-base antifreeze in used lubri
3、cating oils (mineral base)by two procedures, one using reagents in tablet form and theother using laboratory shelf reagents. Principally the testmethods detect ethylene glycol but will also detect other1,2-glycols that may be present.1.1.1 When a positive result is obtained and a sample of theunused
4、 oil is available, the unused oil is also tested and used asa reference.NOTE 1Since the inception of this test method (1971), there havebeen many changes in base stock technology and additive technology.Therefore, when available, the new, unused oil, or a sample of the sameused oil, known to not con
5、tain antifreeze, is tested as a reference.1.2 The tablet procedure (Procedure A) is sensitive to about100 mg/kg and the shelf reagent procedure (Procedure B) toabout 300 mg/kg of ethylene glycol.1.3 Glycol-based coolant leaks into crankcases may not bedetected or may result in a low bias using these
6、 test methods ifthe glycol has degraded or been thermally or otherwiseoxidized. The conditions in crankcases may be such thatcontaminant glycols are oxidized or degraded to a degree towhich the color indicator reaction does not occur or is biasedenough so as to not trigger the color change. Other te
7、stmethods for the detection of coolants or coolant additives inlubricating oils should be used if the results from these testmethods alone are inconclusive or questionable.1.4 Carbohydrates such as sugars and sugar-containingsubstances are sometimes used for sabotage purposes. If thepresence of thes
8、e substances is suspected, Procedure A con-tains a modification to remove these interferences.1.5 Both procedures are adaptable to field kit use, and briefdescriptions for converting to field kit form are given in AnnexA1.1.5.1 Commercial field testing kits are available.2,31.6 The results obtained
9、by this method are qualitativeexpressions. However, for the preparation of reagents and inthe procedures, acceptable SI units are to be regarded as thestandard.1.7 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the use
10、r of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:4D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD 1193 Specification for
11、Reagent WaterD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3. Terminology3.1 Definitions:3.1.1 glycol-base antifreeze, n in engi
12、ne coolants, ethyl-ene or propylene glycol commonly used in admixture withwater and additives to lower the coolant freezing point.3.1.2 used oil, nany oil that has been in a piece ofequipment (for example, an engine, gear box, transformer, orturbine) whether operated or not.3.1.2.1 DiscussionIn the
13、development of this test method,the used oil is a mineral lubricating oil from an enginecrankcase. D 41754. Summary of Test Methods4.1 The ethylene glycol is extracted from the sample with anacid solution and oxidized to formaldehyde with periodic acidwhich is detected colorimetrically with decolori
14、zed fuchsin.1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and are the direct responsibility of Subcommit-tee D02.06 on Analysis of Lubricants.Current edition approved Nov. 1, 2007. Published December 2007. Originallyapproved in 1971. Last pr
15、evious edition approved in 2004 as D 298298(2004).2The sole source of supply of the apparatus known to the committee at this timeis 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 PreventativeMaintenance Ltd., 11
16、2-5621, 11th St., N.E., Calgary, AB, Canada T2E 6Z7.3If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.4For referenc
17、ed ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyrig
18、ht ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 Leakage of glycol-base antifreeze into the crankcase isserious because the coolant tends to interfere with the lubricantand its ability to lubricate; it also promotes
19、 sludging. Ethyleneglycol present in the coolant can increase varnish depositformation in the crankcase as a result of glycol oxidation andthe interaction between glycol and lubricant. Furthermore,because glycol is a higher boiling material than water, it willtend to stay longer in the crankcase oil
20、 than water. Lubricantdisplacement, sludging, and deposit formation all lead toengine malfunction and possible seizure.5.2 These tests are designed to detect glycol-base coolantcontamination even at low levels because early detectionenables corrective measures to be taken to prevent leakingcoolant f
21、rom accumulating and seriously damaging the engine.5.3 These test methods are also significant because thereagents can be packaged as a field kit, and the procedure canbe followed at the site where there is a concern.6. Interferences6.1 The reactions are not specific to ethylene glycol; other1,2-gly
22、cols and many carbohydrates will give a positive test.6.2 Hexylene glycol and methoxy glycol, which are oftenused as gasoline anti-icing additives, do not interfere whenpresent in gasoline-diluted used oils.6.3 Oil oxidation products present do not interfere with thetest.6.4 Some new oils can contai
23、n small amounts of glycolderivatives as part of their makeup and thus give a positive test.These oils, after use, invariably give a negative or tracereaction as the glycol derivatives are slowly destroyed underconditions of use in the engine.6.5 Amodification is described in ProcedureAfor removingin
24、terferences caused by carbohydrates such as sugars andsugar-containing substances that are sometimes used for sabo-tage purposes.7. Purity of Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to
25、the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.5Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determ
26、ination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean distilled water conform-ing to Type III of Specification D 1193.8. Sampling8.1 Ethylene glycol is immiscible with and heavier thanmineral lubricating oil; hence, it will tend to settle. Do not takea
27、 sample that is too large to shake vigorously in the laboratorybecause vigorous shaking is required before conducting thetest.8.2 If the sample delivered is too large to be shakenvigorously, then draw the sample to be tested from a low pointin the container.8.3 Under some circumstances ethylene glyc
28、ol will emul-sify with the oil to form a sludge. If the sample to be tested isa sludge, then dilute the sample with a solvent, such as naphthaor toluene. (WarningThese solvents are toxic and flam-mable.) Use a volume of solvent sufficient to provide a fluidsample for the test.8.4 When drawing a samp
29、le directly from an engine ormachine, ensure that the sample is representative by drawing itjust after the engine or machine has been shut down. If theengine or machine has seized, or it has not seized but is not tobe turned over, draw the sample from a low point so as tosample the settled glycol if
30、 present. (WarningAvoid a top ordipstick sample because the glycol portion, if present, can bemissed.)8.5 Where applicable, Practice D 4057 (manual sampling)and Practice D 4177 (automatic sampling) will provide usefuldirection for obtaining consistent and representative samples.Consistent and repres
31、entative sampling is especially importantwhen the lubricant is in equipment which is still operationaland other tests on the sample are also required.PROCEDURE AUSING TABLETS9. Apparatus9.1 Graduated Cylinder, glass-stoppered, 100 mL, with1-mL graduations (two required).9.2 Tablet PressSee 10.2.10.
32、Reagents and Materials10.1 Acid Solution (12 volume %)Add and mix slowlywith caution 12 volumes of concentrated sulfuric acid (H2SO4,relative density 1.84) into 88 volumes of water. (WarningCorrosive. Causes severe burns. Mixing sulfuric acid withwater generates heat. Always add the acid to the wate
33、r and addit slowly. Never add the water to the acid.)10.2 Potassium Periodate Tablet.3,6(WarningToxic.Hazardous.)10.2.1 Composition of Tablet:Ingredient Amount FunctionPotassium periodate (WarningToxic.Hazardous.)0.3 6 0.01 g oxidizingagentAmmonium chloride 0.9 6 0.03 g diluentSodium bicarbonate 0.3
34、 6 0.01 g diffusing agent5Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K. and the
35、 United States Pharmacopeia andNational Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.6The sole source of supply of the apparatus known to the committee at this timeis potassium periodate and sodium sulfite/pararosaniline hydrochloride tabletsavailable from Accurate Manufactur
36、ing Chemicals Inc., PO Box 26, Cote St., LueStation, Montreal, Quebec, Canada H4V 1H8 and from Technical Products Inc., POBox 11428, Baltimore, MD 21239.D2982072Polyvinylpyrrolidone (5 mass %dissolved in isopropyl alcohol)3,70.01 g binderTotal weight 1.5 6 0.05 g10.2.2 Preparation of TabletBind chem
37、icals into tabletform not to exceed 13 mm in diameter. The tablet shouldwithstand reasonable handling and be readily soluble in theacid solution (Note 2). Store in amber glass bottles with aplastic cap at room temperature and out of direct rays of thesun. In this way the tablet will remain stable fo
38、r at least fiveyears.NOTE 2Exercise care in the preparation of the tablets to assure thatthey are not so brittle that they will crumble in handling or not so compactthat they will not readily dissolve in the acid solution.10.3 Sodium Sulfite/Pararosaniline Hydrochloride Tab-let3,6(WarningToxic. Haza
39、rdous.)10.3.1 Composition of Tablet:Ingredient Amount FunctionSodium sulfite (WarningToxic.Hazardous.)1.05 6 0.03 g reducing agentPararosaniline hydrochloride (WarningToxic. Hazardous.)0.01 6 0.001 g indicatorSodium bicarbonate 0.42 6 0.01 g diffusing agentMagnesium stearate 0.01 g lubricantPolyviny
40、lpyrrolidone (5 mass %dissolved in isopropyl alcohol)3,70.01 g binderTotal weight 1.50 6 0.04 g10.3.2 Preparation of TabletMix and grind together thesodium sulfite, sodium bicarbonate, and the pararosanilinehydrochloride. Pass the mixture through a 180-m (80-mesh)sieve, dampen with the polyvinylpyrr
41、olidone in alcohol, andpass through a 425-m (40-mesh) sieve. Dry for4hat380Cand overnight at room temperature. Pass through a 500-m(30-mesh) sieve. Sprinkle with magnesium stearate and mix.Press into tablet form not to exceed 13 mm in diameter. Thetablet should withstand reasonable handling and be r
42、eadilysoluble in the acid solution (Note 2). Store in an amber glassbottle with plastic cap at room temperature or lower and out ofthe direct rays of the sun. In this way, the tablets will remainstable for at least five years.10.4 Toluene(WarningToxic. Flammable.)11. Preparation of Apparatus11.1 Rin
43、se the cylinder first with toluene to remove the usedoil/toluene mixture and then with hot water. Dry.11.2 WarningDo not use soaps or detergents for cleaningbecause they can leave residues that can interfere with theseparation of the aqueous layer.12. Procedure12.1 Bring the sample to room temperatu
44、re and shake wellto ensure even distribution of any glycol throughout the sample(Section 8). Use only reagents at room temperature (above18C).12.2 Pour toluene into a 100-mL glass-stoppered cylinder tothe 80-mL mark.Add the well-mixed oil sample to the 100-mLmark. Stopper the cylinder and mix well.1
45、2.3 Pour acid solution into another 100-mL glass-stoppered cylinder to the 60-mL mark. Drop a potassiumperiodate tablet into the acid solution and allow it to dissolve.Bring to the 80-mL mark with the well-mixed toluene/oilmixture from the other cylinder. Shake vigorously for 1 min,being careful to
46、avoid leakage of liquid from around thestopper. Remove the stopper and let the cylinder stand for 10min.12.4 Drop in a sulfite/pararosaniline tablet and wait for 30min. Upon addition of the tablet, effervescence commences,and a deep brownish color develops in the aqueous layer inabout 1 min and then
47、 disappears.12.5 After the disappearance of the brown color, observe theformation of color in the aqueous layer.13. Observations and Interpretations13.1 Regard a yellow or pale green coloration that persistsfor at least 30 min as a negative test result.13.2 Regard a pale, dirty green color that grad
48、ually turns topurple in 30 min as a trace test result. This trace quantity is inthe range of 100 to 300 mg/kg.13.3 Regard a purple color, which may intensify uponstanding for 30 min, as a positive test result. When the purplecolor appears within a few minutes, more than 1 % glycol ispresent.13.4 Whe
49、n the test result is positive or trace, and sugar orsugar-containing materials are suspected of being present,instead of performing the test directly on the toluene/oilmixture (12.2), do a water test (Test Method D95first on the100 mL of this mixture, transfer the condensed trap contents tothe acid/periodate solution in the glass-stoppered cylinder(12.3), and carry out the rest of the antifreeze test. Discard theoil/solvent residue from the water test that would contain anysugar. The presence or absence of interfering compounds frommanufacture can be confirm
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