ASTM_D_3893_-_03_2009.pdf

Designation:D389303(Reapproved 2009)Standard Test Method forPurity of Methyl Amyl Ketone and Methyl Isoamyl Ketone byGas Chromatography1This standard is issued under the fixed designation D3893;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()indicates an editorial change since the last revision or reapproval.1.Scope*1.1 This test method covers the determination of the purityof methyl amyl ketone and methyl isoamyl ketone.In addition,the method determines total ketones and various impuritieswhich may include acetone,isopropyl alcohol,methyl propylketone,methyl isobutyl ketone,methyl butyl ketone,methylisobutyl carbinol,mesityl oxide,methyl isoamyl ketone,methyl butyl carbinol,methyl amyl ketone,and diisobutylketone.1.2 Water and acid cannot be determined by this testmethod.They must be determined by other appropriate ASTMprocedures,and the results used to normalize the chromato-graphic data.1.3 For purposes of determining conformance of an ob-served or a calculated value using this test method to relevantspecifications,test result(s)shall be rounded“off to the nearestunit”in the last right-hand digit used in expressing thespecification limit,in accordance with the rounding-off methodof Practice E29.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.1.6 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.2.Referenced Documents2.1 ASTM Standards:2D1364 Test Method for Water in Volatile Solvents(KarlFischer Reagent Titration Method)D1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint,Varnish,Lacquer,and Related ProductsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals(Withdrawn 2009)33.Summary of Method3.1 A representative specimen is introduced onto a gas-liquid partition column.The separated components are mea-sured in the effluent by a detector and recorded as a chromato-gram.The chromatogram is interpreted by applying componentattenuation and detector response factors to the peak areas andrelative concentrations are determined by relating the indi-vidual peak responses to the total peak response.Water andacidity are measured by Test Methods D1364 and D1613,respectively,and the results are used to normalize the valuesobtained by gas chromatography.4.Significance and Use4.1 This procedure is designed to determine the purity of thetwo ketones,methyl isoamyl ketone and methyl amyl ketone,and to obtain the concentration of their various impurities,several of which are critical in the application of these solvents.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.35 on Solvents,Plasticizers,and Chemical Intermediates.Current edition approved Dec.1,2009.Published January 2010.Originallyapproved in 1980.Last previous edition approved in 2003 as D3893 03.DOI:10.1520/D3893-03R09.2For referenced 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.3The last approved version of this historical standard is referenced onwww.astm.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.Apparatus5.1 ChromatographAny gas-liquid chromatographic in-strument having either a thermal conductivity or flame ioniza-tion detector and sufficient sensitivity and stability to obtain for0.01%impurity in the specimen a recorder deflection of atleast 20 mm at a signal-to-noise ratio of at least 5 to 1.Arecording integrator or computer data processing system mayalso be used.5.1.1 The injection port of the chromatograph must have avolume of at least 1.2 mL to provide for proper vaporization ofthe specimen.The use of a smaller injection port or on-columninjection causes peak broadening and tailing.5.2 ColumnFour and one half m of 3.2-mm stainless steeltubing packed with 80 to 90-mesh acid-washed,base-washed,and silanized diatomaceous earth support coated with 10.0%20 000 molecular weight polyethylene glycol and a 8.33%phenyl methyl(50:50)silicone.A capillary column,capable ofthe requ