ASTM_D_2072_-_92_1998e1.pdf

Designation:D 2072 92(Reapproved 1998)e1Standard Test Method forWater in Fatty Nitrogen Compounds1This standard is issued under the fixed designation D 2072;the number immediately following the designation indicates the year oforiginal adoption 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.This test method was prepared jointly by ASTM and the American Oil Chemists Society.e1NOTEFormer Footnote 4 was deleted editorially in May l998.1.Scope1.1 This test method covers the determination of water infatty nitrogen compounds by titration with a water-methanolsolution after addition of an excess of Karl Fischer reagent.1.2 The procedures appear in the following order:SectionsFatty Primary Amines,Diamines,and Amidoamines4-8Difatty Secondary Amines9-12Quaternary Ammonium Chlorides13-161.3 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 applica-bility of regulatory limitations prior to use.Specific hazardstatements are given in 5.3,6.1,and 11.2.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2D 1364 Test Method for Water in Volatile Solvents(FischerReagent Titration Method)33.Summary of Test Method3.1 An excess of Karl Fischer reagent is added to thespecimen dissolved in the prescribed solvent.After reactionwith the water in the specimen,the excess Karl Fischer reagentis back-titrated with water-methanol solution.The end point isbest detected electrometrically,but with practice it may besatisfactorily determined visually.FATTY PRIMARY AMINES,DIAMINES,ANDAMIDOAMINES4.Apparatus4.1 Buret and Bottle Assemblies(or other convenient ar-rangement),protected with silica gel so as to maintain KarlFischer reagent and water-methanol solutions free from con-tamination with moisture either through the atmosphere orotherwise(Note 1).The titration should be performed in aclosed system to avoid the absorption of water.The electrodeand buret shall be mounted through a close-fitting stopper,andprovision made for mechanical stirring by means of a magneticstirrer.NOTE1It is essential that the Karl Fischer reagent,water-methanolsolution,and anhydrous methanol be protected from atmospheric moistureat all times.In humid seasons or climates,the drying tubes used to protectthe reagents against moisture in the air must be watched closely.The silicagel must be changed as soon as there is evidence of color change in it.Care also must be taken to minimize the exposure of the sample andsolutions to atmospheric moisture during the determinations.4.2 Magnetic Stirrer,that can be used with the closedtitration beaker with inert plastic-coated stirring bar.4.3 Pipet,automatic,25-mL.4.4 Pipet,weighing,or equivalent for weighing water,forstandardization of reagent.4.5 Electrometric Titrator of the“dead stop”type,equipped with platinum electrodes.On operation a smallelectrical potential is imposed across the electrodes.At the endpoint there is a change in the flow of current due to the changein polarization of the electrodes.5.Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform 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 the determination.5.2 Purity of WaterUnless otherwise indicated,references1This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,andApplications,and is the direct responsibility ofSubcommittee D01.32 on Drying Oils.Current edition approved March 15,1992.Published May 1992.Originallypublished as D 2072 65 T.Last previous edition D 2072 66(1987)e1.2Annual Book of ASTM Standards,Vol 11.01.3Annual Book of ASTM Standards,Vol 06.04.4Reagent 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 United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTMto water shall be understood to mean reagent water conformingto Type II of Specification D 1193.5.3 Acetic Acid,Glacial(CH3COOH).Warning(see6.2).5.4 Karl Fischer ReagentSuitable reagent is availablefrom most chemical supply houses or see Test Method D 1364.5