1、Designation: D 2982 98 (Reapproved 2004)An 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
2、or, in the case of 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. Scope1.1 These test methods describe the qualitative determina-tion of glycol-base an
3、tifreeze in used lubricating oils (mineralbase) by two procedures, one using reagents in tablet form andthe other 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
4、 a sample of theunused 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
5、 oil, known to not contain 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 Carbohydrates such as sugars and sugar-containingsubstances are sometimes used
6、for sabotage purposes. If thepresence of these substances is suspected, Procedure A con-tains a modification to remove these interferences.1.4 Both procedures are adaptable to field kit use, and briefdescriptions for converting to field kit form are given in AnnexA1.1.4.1 Commercial field testing ki
7、ts are available.21.5 The results obtained by this method are qualitativeexpressions. However, for the preparation of reagents and inthe procedures, acceptable SI units are to be regarded as thestandard.1.6 This standard does not purport to address all of thesafety concerns, if any, associated with
8、its use. It is theresponsibility of the user 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:3D95 Test Method for Water in Petroleum Products andBituminous Materia
9、ls by DistillationD 1193 Specification for 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 Definiti
10、ons:3.1.1 glycol-base antifreeze, n in engine 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) whethe
11、r operated or not.3.1.2.1 DiscussionIn the 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
12、 is detected colorimetrically with decolorized fuchsin.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 sludging. Ethyleneglycol present in the coolant can
13、 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 than water. Lubricant1These test methods are under
14、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 Dec. 1, 2004. Published December 2004. Originallyapproved in 1971. Last previous edition approved in 1998 as D 2982
15、98e1.2The 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 PreventativeMaintenance Ltd., 112-5621, 11th St., N.E., Calgary, AB, Canada T2E 6Z7. Testinstructions are provided with the kit.3For referenced ASTM st
16、andards, 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken
17、, PA 19428-2959, United States.displacement, 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 leaking
18、coolant from 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; oth
19、er1,2-glycols 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 c
20、an contain 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 r
21、emovinginterferences 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 co
22、nform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of t
23、he determination.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
24、not takea 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 ethy
25、lene glycol 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 drawi
26、ng a sample 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
27、glycol if 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 a
28、nd representative 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
29、10.2.10. 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
30、 the water and addit slowly. Never add the water to the acid.)10.2 Potassium Periodate Tablet.5(WarningToxic. Haz-ardous.)10.2.1 Composition of Tablet:Ingredient Amount FunctionPotassium periodate (CautionToxic.Hazardous.)0.3 6 0.01 g oxidizingagentAmmonium chloride 0.9 6 0.03 g diluentSodium bicarb
31、onate 0.3 6 0.01 g diffusing agentPolyvinylpyrrolidone (5 mass %dissolved in isopropyl alcohol)60.01 g binderTotal weight 1.5 6 0.05 g10.2.2 Preparation of TabletBind chemicals into tabletform not to exceed 13 mm in diameter. The tablet should4Reagent Chemicals, American Chemical Society Specificati
32、ons, 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 United States Pharmacopeia andNational Formulary, U.S. Pharmaceutical Convention,
33、Inc. (USPC), Rockville,MD.5Suitable potassium periodate and sodium sulfite/pararosaniline hydrochloridetablets are available fromAccurate Manufacturing Chemicals Inc., PO Box 26, CoteSt., Lue Station, Montreal, Quebec, Canada H4V 1H8 and from Technical ProductsInc., PO Box 11428, Baltimore, MD 21239
34、. If you are aware of alternative suppliers,please provide this information to ASTM International Headquarters. Your com-ments will receive careful consideration at a meeting of the responsible technicalcommittee1, which you may attend.6Polyvinylpyrrolidone is available as “Plasdone” from Antara Che
35、micals Divi-sion of General Aniline and Film Corp., New York, NY. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee1, which you may attend.D
36、2982 98 (2004)2withstand 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 for at least fiveyears.NOTE 2Exercise care in the preparati
37、on 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 Tablet5(WarningToxic. Hazardous.)10.3.1 Composition of Tablet:Ingredient Amount Functi
38、onSodium sulfite (CautionToxic.Hazardous.)1.05 6 0.03 g reducing agentPararosaniline hydrochloride (CautionToxic. Hazardous.)0.01 6 0.001 g indicatorSodium bicarbonate 0.42 6 0.01 g diffusing agentMagnesium stearate 0.01 g lubricantPolyvinylpyrrolidone (5 mass %dissolved in isopropyl alcohol)60.01 g
39、 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 polyvinylpyrrolidone in alcohol, andpass through a 425-m (40-mesh) sieve. D
40、ry 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 readilysoluble in the acid solution (Note 2). Store in an amber
41、 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 Rinse the cylinder first with toluene to remove the usedoil/tolue
42、ne mixture and then with hot water. Dry.11.2 CautionDo 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 temperature and shake wellto ensure even distribution of any glycol thr
43、oughout 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.12.3 Pour acid solution into another 100-mL glass-stoppered cyl
44、inder 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 avoid leakage of liquid from around thestopper. Remove the sto
45、pper 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 disappears.12.5 After the disappearance of the brown color, o
46、bserve 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 gradually turns topurple in 30 min as a trace test result. This tr
47、ace 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 When the test result is positive or trace, and sugar orsugar-cont
48、aining 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
49、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 confirmed by carrying out the test on newor preferably on the used oil known not to be contaminated byglycol-base antifreeze as the concentration of these compoundstends to diminish in use. Allow for such interference whenreporting results.13.5 When a positive test result is obtained, perform the teston the same oil, unused, or the same oil, used and known tocontai
