ASTM D5984-11(2017) Standard Test Method for Semi-Quantitative Field Test Method for Base Number in New and Used Lubricants by Color-Indicator Titration.pdf

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1、Designation: D5984 11 (Reapproved 2017)Standard Test Method forSemi-Quantitative Field Test Method for Base Number inNew and Used Lubricants by Color-Indicator Titration1This standard is issued under the fixed designation D5984; the number immediately following the designation indicates the year ofo

2、riginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure for determining thebasic

3、 constituents in petroleum products in the field or labora-tory using a pre-packaged test kit. The test uses a micro-titration resulting in a visual endpoint facilitated by a colorindicator.1.1.1 This test method covers base numbers from 0 to 20. Itcan be extended to higher ranges by diluting the sa

4、mple or byusing a smaller sample size; however, the precision data wereobtained for base numbers up to 20.1.2 This test method can be used to indicate relative changesthat occur in an oil during use under oxidizing conditions.Although the test is performed under closely specified condi-tions with st

5、andardized reagents, the test method does notmeasure an absolute basic property that can be used to predictperformance of an oil under service conditions. No generalrelationship between bearing corrosion and base number isknown.1.3 The values stated in SI units are to be regarded as thestandard.1.3.

6、1 ExceptionThe values given in parentheses are forinformation only.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the ap

7、plica-bility of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued

8、by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD2896 Test Method for Base Number of Petroleum Productsby Potentiometric Perchloric Acid TitrationD4057 Practice for Manual Sampling of Petroleum

9、 andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3. Terminology3.1 Definitions:3.1.1 base number, nthe quantity of a specified acid,expressed in terms of the equivalent number of milligrams ofpotassium hydroxide per gram of sample, required to titrate asa

10、mple in a specified solvent to a specified endpoint using aspecified detection system.3.1.1.1 DiscussionThis test method uses fixed amounts ofisooctane and alcoholic hydrochloric acid as the sample solventand the endpoint is defined as the amount of titrant required toreach a yellow endpoint with a

11、methyl red indicator solution.4. Summary of Test Method4.1 To determine the base number of an oil sample, thesample is dissolved in a fixed amount of iso octane andalcoholic hydrochloric acid. The solution is mixed well with7 mL of sodium chloride solution and the aqueous and organicphases are allow

12、ed to separate. The aqueous phase is thendecanted off and a small amount of methyl red indicator isadded. The solution is titrated with a solution of sodiumhydroxide contained in a calibrated 1 mL micro-burette. Whenthe solution changes from magenta to yellow, the titration isstopped and the base nu

13、mber is read off the side of the titrationburette.5. Significance and Use5.1 New and used petroleum products can contain basicconstituents that are present as additives or as degradation1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubrican

14、ts and is the direct responsibility ofSubcommittee D02.06 on Analysis of Liquid Fuels and Lubricants.Current edition approved May 1, 2017. Published July 2017. Originally approvedin 1996. Last previous edition approved in 2011 as D5984 11. DOI: 10.1520/D5984-11R17.2For referenced ASTM standards, vis

15、it 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29

16、59. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical

17、Barriers to Trade (TBT) Committee.1products formed during service. The amount of these additivesin an oil can be determined by titrating against an acid. Thebase number is a measure of the amount of basic substance inthe oil, always under the conditions of the test. A decrease inbase number is often

18、 used as a measure of lubricantdegradation, but any condemning limits must be empiricallyestablished.5.2 This test method uses reagents that are considered lesshazardous than most reagents used in alternate base numbermethods. It uses pre-packaged reagents to facilitate basenumber determinations in

19、the field where scientific equipmentis unavailable and quick results are at a premium.NOTE 1Results obtained by this test method3are similar to thoseobtained by Test Method D2896.6. Apparatus46.1 Sampling Syringe, fixed volume of 0.35 mL.6.2 Test Tubes (2), pliable, plastic with threaded tops ca-pab

20、le of holding at least 20 mL, one with a standard screw capand the second with a screw cap that is equipped with adispenser nozzle.6.3 Titrating Burette, disposable, 1.0 mL.6.4 Filter Funnel, capable of removing suspended oil drop-lets from aqueous solutions. Polypropylene wool has beenfound to work

21、 well for this purpose.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Pre-packaged, manufactured test kits shall useonly reagent grade chemicals.7.2 Purity of WaterAll water will be reagent water asspecified by Type III of Specification D1193.7.3 Hy

22、drochloric Acid, 0.114 mol L (60.001 mol L) HCl inpropan-2-ol (isopropyl alcohol). (WarningFlammable.)7.4 Methyl Red Indicator, 0.05 % (m/v) solution of methylred in anhydrous ethanol. (WarningFlammable.)7.5 Sodium Chloride Solution, 7.0 mL of 20 % (m/m) NaClin reagent grade, CO2free water.7.6 Sodiu

23、m Hydroxide Titrant, 1.0 mL of 0.0645 mol L(60.0005 mol L) NaOH sealed from the environment in aplastic titration burette which is indexed with base numberunits from 0 to 20. (WarningToxic and corrosive.)7.7 2,2,4-Trimethyl Pentane (iso octane)(WarningFlammable.)8. Procedure58.1 Obtain samples for a

24、nalysis by this test method inaccordance with instructions given in Practice D4057 orD4177.8.2 If a sample is to be taken directly from a hot engine,follow the manufacturers instructions for obtaining a repre-sentative sample. Allow the oil to cool to 50 C beforeproceeding further.8.3 It is essentia

25、l to ensure the sample is representative sinceany sediment can be acidic or basic or have adsorbed acidic orbasic material from the sample. When necessary, samples arewarmed to aid mixing. Used oils should be vigorously mixed toensure homogeneity before sampling.8.4 As used oils can change appreciab

26、ly in storage, samplesshall be tested as soon as possible after removal from thelubricating system.8.5 Prepare the oil sample by shaking well to disperse anyparticulates.8.6 Place the tip of the fixed volume sampling syringe intothe oil sample. Draw back the plunger of the sampling syringeuntil it s

27、tops. Remove the syringe from the oil sample and wipethe outside clean of any excess oil. Dispense the entire volumeof the syringe into the first test tube. Replace the cap on the testtube.8.7 Add 1.0 mL of 2,2,4-trimethyl pentane (isooctane) andshake the tube well to mix the oil with the diluent. A

28、dd 1.0 mLof 0.114 mol/L alcoholic HCl and shake the tube well for 30 s,allowing the acid to react with the diluted oil sample.8.8 Pour 7.0 mL 20 % NaCl solution into the oil mixture.Cap the tube and shake the mixture well for 30 s so that the twophases are completely dispersed. Stand the tube upside

29、-downon its cap and allow the aqueous and organic phases toseparate.8.9 Place the plastic filter into the top of the second testtube. Keeping the first test tube upside-down and vertical, openthe dispenser cap on the tube and dispense exactly 5 mL of theaqueous solution through the filter into the s

30、econd test tube.Stop dispensing as soon as 5 mL has been placed in the tube.8.10 Place the 1.0 mL micro-burette into the tube containingthe 5.0 mL of aqueous extract. Seal the burette into place byscrewing the threaded cap of the burette onto the test tube. Add0.5 mL of the methyl red indicator solu

31、tion and disperse theindicator throughout the solution by gently shaking. Startslowly dispensing the titrant into the solution and shake gently.As soon as the solution turns from magenta to yellow, stop the3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requ

32、esting Research Report RR:D02-1345. ContactASTM CustomerService at serviceastm.org.4A patent pending field test kit containing appropriate apparatus reagents, andmaterials is available from Dexsil Corp., Hamden, CT.5This procedure is covered by U.S. patent number 5,366,898, Dexsil Corp.,Hamden, CT.

33、If you are aware of alternative, 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.D5984 11 (2017)2titration and read the result, in base number units, off the

34、 sideof the burette barrel. The reading should be taken at the tip ofthe plunger.9. Precision and Bias9.1 The precision of this test method as determined by thestatistical examination of test results from 11 samples of newand used oils, covering base numbers between 0 and 20, run induplicate by nine

35、 different laboratories (Research ReportRR:D02-1345)3is as follows:9.1.1 RepeatabilityThe difference between successive re-sults obtained by the same operator with the same apparatusunder constant operating conditions on identical test materialwould, in the long run, in the normal and correct operat

36、ion ofthe test method, exceed the following value only in one case intwenty:r 5 0.94 base number units mg KOH/g sample! (1)9.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would

37、, inthe long run, in the normal and correct operation of the testmethod, exceed the following values only in one case intwenty:R 5 1.91 base number unitsmgKOH/g sample! (2)9.2 BiasThis procedure has no bias because the basenumber can be defined only in terms of the test method.10. Keywords10.1 base

38、number; color-indicator titration; lubricants; testkitASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent r

39、ights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either f

40、or revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair heari

41、ng you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard m

42、ay be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 11 (2017)3