ASTM_D_3421_-_75_scan.pdf

qlDesignation:D3421-75StandardRecommendedPracticeforEXTRACTION AND DETERMINATION OF PLASTICIZER.oMIXTURES FROM VINYL CHLORIDE PLASTICSlThis Standard is issueilunder.the fixed designation D3421:the number immediatel);followiilg the designation indicatesthe yearoforiginal adoption or.inthe caseorrevision.the yearoflast revision.numberin parentheses indicates theyearoflastreapproval.1.Scope1.1This recommendedprcticecoversthe isolation and determinationofthe mono-meric and polymeric constituents,ofplasti-cizerD)itunsused in,pply(vinyl chloride)compositions;it pr9videsmeans fortheanaly-sisofcompositions containing dioctyl phthal-ate with oneormore homogeneous polyesterplasticizers,and may beetendedto analysisofplasticizer mixtures containing simplephthalate esters other than diQctyl phthalate.NOTEI-Thevalues stated in SI units are to beregarded as the standard.2.Appiicable Documents2.IASTMStandards:D494Testfor Acetone ExtractionofPhe-nolic MoldedorLaminated Products2E260Recommended Practice for GeneralGas ChromatographyP;ocedues33.SigItificance3;1Separation and identificationofthecomponentsusedin thermoplastics com-pounds is,often required in efforts to relateperformance properties to constitution,andin the designoffabrication control,proce-dures.,:;,3.2Themethodobviates,difficultiescaused by incomplete reprecipitationofhighpolymeric materialfromcompositions com-pletely dissolved in solvents such as tetrahy-drofuran.4.Apparatus,4.1Forsmall samples(approximately(g),seniimicro Soxhlet extractors4are adequate;these.may be.used with paper thimbles,orwith gIass shells.5TheWiley-Richardsonap-paratus(Method D 494)suseful and gives.shortened extraction times dueto.full iinmer-,sionofthe saJIlple holder in solvent vapors;this typeofapparatus must bemodifi,toeliminate contact between solvent vapors andmetal parts.All-glass extractors having anouterjacket permitting solvent vapors,tosur-round the barrel are available.6s.Reagents5.1Carbqn,Tetrachloride,ACS,reagentgrade.5.2Chloroform.ACS,reagent grade.NOTE2:Caution-Bothcarbon tetrachlorideand chloroform are highly toxic,and should be.han:dled.withetfemecare,preferably within anefficienthood;inhalationofvaporsistobeavoided.;.,5.3Mthanol,ACS,reagentgrade.,.I6.SamplePreparation6.1Grindthe sample in a Wiley polymermill toZQ-meshparticle size.Ifa Wiley mill isunavailable,5 by 5-mm squares cut fromsheetingof0.6 to 2-mm thickness givesatis-factory results.IThis recommended practice isunder the jurisdictionofASTM Committee0-20on Plastics.and is the directresponsibilityofSubcommittee D20.70 on AnalyticalMethods.,.,.Currenteditiori approved June 30.191.5.PublishedAu-gust1975.Annual BookofASTMStandards.Part35.,aAnnualBookofASTMStandards.,Part42.For example.Scientific Glass Apparatus Co.CatalogNo.JR-5700A.Sargent S-31247A.5Sargent 5-31709.31710.Scientific Glass Apparatus Catalog No.JM-5120.NOTICE:This standard has either been superseded and replaced by a new version or discontinued.Contact ASTM International(www.astm.org)for the latest information.6.2 When sufficient materialisavailable,the preferred sample weightisapproximately5g.7.Procedure7.1 Place 1to 5gofthe prepared sample ina preweighed(to0.0001 g)paper thimbleor,glass/ceramic extractor cup,and weigh theassembly toO.OOOlg.Place the assemblyinthe extractorbarreL;.,.,7.2 Attach acondeDertotheexttorbarreldextractthesampl16h with a2+1(by volume)mixtureofcarbon tetrachlorideandmethanol.7.3Cool theextractand filter through aflutedpaperinto a tared flask,rinsing thepaperwith small portionsofthe solvent mix-ture.7.4 Evaporate thesolventtoconstant re-sidual weightona steam bath;weigh theresidue to the nearest 0.0001g.7.5 Determinethedioctyl phthalate con-tentbygas chromatography(see Recom-mended PracticeE 260).7.5.1 A general descriptionofconditionsappropriate for determinationofthe mono-meric content when the monomeric consistsofDOPfollows.7Isothermalandpro-grammed-temperature modes have been em-ployed.CoIu:1.8 m by 3.18niin(6ftby II.in.)10%SE-306n:ChromosorbWorDiatopott&Temperatures:265to280C(isothermal;26SCgavebetterresolutionofpeaks)50to3300CprogrammedatIOOClmin.Sample size:1p.1.Carrier:heliumat3:45MPa(50psi)gage;flowrate60tlll/minDetector:flame ionizationdetector,Detectortemperature:3200CIliectionporttem-3S00Cperature:Internal standard:dibutyl phthalate 7.5.2 Quantitatively transfer the residue(7.4)into a 100-mlvolumetric flask usingchlo-roform as a solvent.Weigh 1.5 gofdibutylphthalate(99%+purity)to the nearest0.0001 g,and place in the flask.Dilute tovolume with chloroform and mix thoroughly.Obtain a chromatogramofthis solution usingthe parameters given in 7.5.1.8.Calibration8.1 CalibrationFactorforDioctyl Phthal-03421ate-Intoa100-011volumetric flask contain-ing approximately50mlofchloroform,weigh1.5gofdioctyl phthalateofknown purity and1.5gofdibutyl phthalateofknown purity.(Make all weighings to the nearest0.0001g.)Dilute to volume with chloroform and mixthorol;lghly.Obtain a chromatogramofthisolutionusing the pafametersyenin 7.5.1