ASTM_D_7090_-_04_2010.pdf

Designation:D709004(Reapproved 2010)Standard Test Method forPurity of Isophorone by Capillary Gas Chromatography1This standard is issued under the fixed designation D7090;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.Scope1.1 This test method covers the determination of the purityof isophorone.This method also determines the impurities ofthe material in concentration level less than 0.5 mass%,whichmay include mesityl oxide(MSO),mesityl oxide-isomer,mesitylene,trimethyl cyclohexenone(TMCH),phorone,phorone-isomer,xylitone,and tetralone.1.2 Water cannot be determined by this test method andshall be measured by other appropriate ASTM procedure.Theresult is used to normalize the chromatographic data deter-mined by this test method.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 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 to determine theapplicability of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D1364 Test Method for Water in Volatile Solvents(KarlFischer Reagent Titration Method)E29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE300 Practice for Sampling Industrial Chemicals3.Summary of Test Method3.1 A representative specimen is introduced into a gaschromatograph with a bonded polyethylene glycol capillarycolumn using temperature programming and a flame ionizationdetector.The concentrations of the sample components arecalculated from the integrated component peaks using internalstandardization technique with response factors.Water ismeasured in accordance with Test Method D1364 and theresult is used to normalize the values obtained by gas chroma-tography.4.Significance and Use4.1 This test method determines the purity of isophorone,aswell as the concentration of various potential impurities,several of which are critical in the application of these solvents.5.Apparatus5.1 ChromatographAny gas chromatograph utilizing acapillary column and has the following characteristics(seeTable 1 for typical GC parameters):5.1.1 DetectorA flame ionization detector(FID)capableof continuous operation at a temperature equivalent to themaximum column temperature employed.The detector shallhave sufficient sensitivity to detect 0.001 mass%of impurity inthe specimen at a peak height 3 times the noise level.5.1.2 Columnfused silica capillary column with bondedpolyethylene(see Table 1 for details).5.1.3 Column Temperature ProgrammingThe chromato-graph shall be capable of reproducible linear temperatureprogramming.5.1.4 Sample Inlet SystemThe sample inlet system shallbe capable of split injection,typically at a 100:1 split ratio.NOTE1An autoinjector is recommended.Manual injection with asyringe is acceptable,however the observed precision may not apply.5.1.5 IntegratorMeans shall be provided for determiningthe area of the observed chromatographic peaks.This can bedone by means of an electronic integrator or a computer basedchromatography data system.The integrator/computer systemshall have standard chromatographic software for determiningthe retention times and quantification of eluting peaks.5.1.6 Flow ControllerThe chromatograph shall beequipped with a constant flow device capable of maintainingthe carrier gas at a constant flow rate throughout the tempera-ture program.5.1.7 MicrosyringeA microsyringe of appropriate capac-ity is required for injection of the specimen into the chromato-graph.Typically,a 5 L syringe is used.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.1,2010.Published December 2010.Originallyapproved in 2004.Last previous edition approved in 2004 as D7090-04.DOI:10.1520/D7090-04R10.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in the preparation of the calibration mixture.6.2 Calibra