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History of Newburyport, Mass., 1764–1905; Volume 1 PDF

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Designation: D7823−16 Standard Test Method for Determination of Low Level, Regulated Phthalates in Poly (Vinyl Chloride) Plastics by Thermal Desorption—Gas Chromatography/Mass Spectrometry1 ThisstandardisissuedunderthefixeddesignationD7823;thenumberimmediatelyfollowingthedesignationindicatestheyearof originaladoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.A superscriptepsilon(´)indicatesaneditorialchangesincethelastrevisionorreapproval. 1. Scope* E177Practice for Use of the Terms Precision and Bias in ASTM Test Methods 1.1 This test method provides a procedure to identify and E355PracticeforGasChromatographyTermsandRelation- quantify six phthalates by thermal desorption (TD) gas chro- ships matography(GC)massspectrometry(MS).Thephthalatesare E594Practice for Testing Flame Ionization Detectors Used BBP, DBP, DEHP, DNOP, DINPand DIDP. in Gas or Supercritical Fluid Chromatography NOTE1—Themethodcanbeextendedtoincludeotherphthalates. E691Practice for Conducting an Interlaboratory Study to 1.2 Withinthecontextofthismethod,“lowlevel”isdefined Determine the Precision of a Test Method as 1000 ppm. IEEE/ASTM SI{10Practice for Use of the International System of Units (SI), the Modernized Metric System 1.3 The values in SI units are to be regarded as standard. 2.2 ASTM Adjuncts: 1.4 This test method includes references, notes and foot- Adjunct to D7823 Vinyl Plasticizer Library—Total Ion notes that provide explanatory material. These notes and Chromatograms and Mass Spectra3 footnotes (excluding those in the tables and figures) shall not be considered as requirements of this method. 3. Terminology 1.5 This standard does not purport to address all of the 3.1 Definitions—For definition of plastic terms used in this safety concerns, if any, associated with its use. It is the test method, see Terminologies D883 and D1600. responsibility of the user of this standard to establish appro- 3.2 For units, symbols, and abbreviations used in this test priate safety and health practices and determine the applica- method refer to Practices E594, E355, or SI10. bility of regulatory limitations prior to use. 3.3 Compounds and Instrumentation: NOTE2—ThereisnoknownISOequivalenttothisstandard. 3.3.1 (DOA) Hexanedioic acid, 1,6{bis(2{ethylhexyl) ester 2. Referenced Documents CAS #103{23{1 3.3.2 (DINCH) 1,2{Cyclohexanedicarboxylic acid, dinonyl 2.1 ASTM Standards:2 ester, branched and linear CAS #474919{59{0 D883Terminology Relating to Plastics 3.3.3 (DBP) 1,2{Benzenedicarboxylicacid, 1,2{di{n{butyl D1600TerminologyforAbbreviatedTermsRelatingtoPlas- ester CAS #84{74{2 tics 3.3.4 (BBP) Benzyl butyl phthalate CAS #85{68{7 D3465TestMethodforPurityofMonomericPlasticizersby 3.3.5 (DEHP) Bis(2{Ethyhexyl) Phthalate CAS #117{81{7 Gas Chromatography 3.3.6 (DNOP) Di(n{octyl) phthalate CAS #117{84{0 D7083Practice for Determination of Monomeric Plasticiz- 3.3.7 (DINP) 1,2{Benzenedicarboxylicacid, ersinPoly(VinylChloride)(PVC)byGasChromatogra- di{C8{10{branched alkyl esters, C9{rich (Jayflex) CAS phy #68515{48{0 3.3.8 (DINP) 1,2{Benzenedicarboxylicacid, 1,2{diisononyl (Palatinol) CAS #28553{12{0 1ThistestmethodisunderthejurisdictionofASTMCommitteeD20onPlastics andisthedirectresponsibilityofSubcommitteeD20.70onAnalyticalMethods. 3.3.9 (DIDP) 1,2{Benzenedicarboxylicacid, Current edition approved May 1, 2016. Published May 2016. Originally di{C9{11{branched alkyl esters, C10{rich (Jayflex) CAS approved in 2013. Last previous edition approved in 2014 as D7823-14. DOI: #68515{49{1 10.1520/D7823-16. 2ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,or [email protected] Standardsvolumeinformation,refertothestandard’sDocumentSummarypageon 3Available from ASTM International Headquarters. Order Adjunct No. theASTMwebsite. ADJD7823S-EA.Originaladjunctproducedin2016. CPNrooop vryeidrpiegrodhCd tb uAoycS ptIiHToyMSnri gouInrhn tndteeer©ntrw aliAotcioreSknn--``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`---iTnasgleM pweIitnrhmt eAitrtSenTdaM twi oithnoaul,t l1ic0e0nsBe afrrormH IHaSrborDri*veA,PSOumBomxCa7r0y0,oWfeCshtCaonngsehsohsoecckteino,nPAa1LNp1ioc9pet4 nfeo2sar8e Rre-2e=ssI9raa5alne9tP,. 0atU6ph/en1eri4.tie/r2e d0n1S6d t0a6ote:f2s6t:1h8i MsDsTtandard D7823 − 16 3.3.10 (DIDP) 1,2{Benzenedicarboxylicacid, 1,2{diisodecyl identical retention times. The analyst shall take the necessary CAS #26761{40{0 steps to insure that adequate separation of the plasticizer 3.3.11 TD Thermal Desorption components is achieved and or the ions used to monitor for a 3.3.12 GC Gas Chromatography target phthalate are free of interference. This includes, but is 3.3.13 GC/MS Gas Chromatography/Mass Spectrometry not limited to changing the selectivity of the chromatographic 3.3.14 PVC Poly (Vinyl Chloride) column. Calibration by standard addition offers the advantage 3.3.15 THF GC grade or higher “Tetrahydrofuran” of minimizing interferences. 3.3.16 DCM GC grade or higher “Methylene Chloride” 6.2 WhenusingaTD{GC/MSmethod,caremustbetakento 3.3.17 EGA{MS Evolved Gas Analysis{mass spectrometry ensure that the sample cups are inert and clean. Any and all 3.3.18 FTIR Fourier Transform Infrared Spectroscopy solvents used to prepare standards and sample solutions must 3.3.19 TIC Total ion chromatogram be free of contamination. 3.3.20 DQO Data quality objectives 6.3 Thepresenceorabsenceofeachphthalateisbasedupon NOTE3—DINPandDIDP,whenusedinvariousPVCformulationsare threecriteria:(1)therelativeretentiontimeofthepeak(2)the technical mixtures. Take care, when preparing the phthalate calibration presence or absence of the quant ion and the two confirming standardtousethetechnicalgrade.HereisspecificinformationonDINP ions and (3) the ratio of the quant and the confirming ion one andDIDP.Formoreinformation,pleaserefertoAppendixX3. Jayflex DIDP: 1,2{Benzenedicarboxylicacid, di{C9{11{branched alkyl must satisfy the established guideline (see Table 1). esters,C10{rich:CAS#68515{49{1. 6.4 Calculatingthephthalateconcentrationsusingtheareas Jayflex DINP: 1,2{Benzenedicarboxylicacid, di{C8{10{branched alkyl eTMmn4sa.HtaSte4seSrF..ssd1u.--``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`---,Pms1Chq2p09tum0eh{a0rcµaiantclLrramthayt:.oegiCosfoQAnofatufhSrTa(e#etSnehi6sITtediM8tfiHe5PMnc1FVat5oiet{firCsito4oehf8nldsouu{a0dltbiml.isyospnbtclhaeaasenreiae)rdr—eraoensdtneaeiselntyshtoziTeoelavndabertldueiemsaii1nneo.sgf1aS0TantaDdmdn-etdLGhsaieCrogidf-r/ orf7aaetf.cidN7nicAlu.giOo1tcpTameEitpensGp5sai—oattrnhhsuateeOnetcrpurdh7aftspr5iesooirpdnmetaoenclcaoc3bitnefiou5vgcte0frrrr°sieaoCoicpomnonhmrs/abnmmnaeotngeanwndse{eds.teaesnsdtrpag:dneeVecdtteatancirlrtooe{dfmdmreaaepedntoaedGluriyCtnsci/idoMassnpa.SansbdAigldeenvaipoofitlfevcreoa.dpnTgethlariy-ss addition is the calibration method. analysis. NOTE4—Standardadditioncalibrationwillnegatematrixinterference. 7.2 Thermal desorption unit capable of heating the sample Italsotakesintoaccounttheoverallperformanceoftheinstrumentation from 100 to 350°C at 20°C/min. atthetimethesamplesareanalyzed. 7.3 Inert, reusable or disposable sample containers or cups. 5. Significance and Use 7.4 GCcapillarycolumn:5%diphenyl{95%poly(dimeth- 5.1 Identificationandquantitationofphthalates:DBP,BBP, ylsiloxane)stainlesssteel,30mby0.25mmIDwitha0.25µm DEHP, DNOP, DINP, and DIDP are required for regulated film thickness, or equivalent. articles. Regulations include: EU—Directive 2005/84/EC, 7.5 Integrator or data handling system, capable of measur- US—Consumer Product Safety Improvement Act of 2008— ing peak areas and retention times to four significant figures. section 108, Japan—Health, Labor and Welfare Ministry 7.6 Analyticalbalance,capableofweighingto60.000001g guideline No.336 (2010). This test method provides a proce- (1 µg). If using a balance capable of weighing to 60.00001 g dure to identify and quantify regulated phthalates in PVC. (10 µg), weight used in the sample and standard preparation 5.2 Other techniques successfully used to separate and mustbescaledaccordinglyinordertoensurethatthedataare identifyphthalatesinPVCincludeGC/MS,HPLC/UV,HPLC/ accurate to three significant figures. MS, FTIR, and GC/FID (flame ionization detector). 7.7 Pressure regulators, for all required gas cylinders. 6. Interferences 7.8 Flowmeter,orothermeansofmeasuringgasflowrates 6.1 Retention times for GC are dependent on several vari- 60.1 mL/min. ables and it is possible to have two or more components with 8. Reagents and Materials 8.1 Helium carrier gas, chromatographic grade. TABLE1IonsandIonRatiosUsedtoIdentifyEachPhthalate 8.2 Methylene chloride (DCM) or n{hexane for preparing DBP BBP DEHP DNOP DINP DIDP the phthalate standard solution (Solution #1, 10.2), spectral Quantion 223 206 279 279 293 307 Confirm 149 149 149 149 149 149 quality or chromatographic grade. ion1 8.3 Tetrahydrofuran(THF),orasolventsuitableforprepar- Arearatio <0.04 <0.23 <0.08 <0.06 <0.20 <0.12 (±10%) ing the PVC sample (Solution #2, 10.3), spectral quality or (Quant/ chromatographic grade. Confirm 1) 8.4 Standards of the appropriate phthalates for use when Confirm 167 167 167 167 167 167 constructinganexternalcalibrationcurveorpreparingSolution ion2 #3 (10.4) used for standard addition. See Note 3. Copyright ASTM International 2 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT D7823 − 16 9. Safety and Precautions toslightlycloudy.Place10µLofthesamplesolutioninaclean sample cup. Evaporate the solvent; the sample is ready to 9.1 Use THF and methylene chloride in a well{ventilated analyze. See Figs. 2 and 3 for example chromatograms. space. 10. Preparation of theAnalytical Samples (based upon NOTE6—Acriticalstepintheaccuratedeterminationofphthalatesis samplehomogeneity.ThisisdiscussedinmoredetailinAppendixX2. using a 1 µg balance) Weights must be scaled up if NOTE7—Itispossiblethatthesolutionwillcontaininorganicmaterial. using a 10-µg balance. Studieshaveshownthatthepresenceofinsolubleinorganicmaterialwill notaffecteithertheaccuracyorprecisionofthephthalatedetermination. 10.1 Three solutions must be prepared: (1) a stock solution of the target phthalate standards, (2) a solution of the sample 10.4 Solution #3—Place 10 µL of the sample solution (#2) and (3) the sample solution spiked with the standard stock into a clean sample cup.Add 10 µLof the phthalate standard solution. solution (#1). Evaporate the solvent. 10.2 Solution #1—Prepare a stock standard solution of the NOTE8—Toexpeditetheevaporationprocess,passasteadystreamof phthalatesbydissolving0.30mgofeachphthalatein10mLof ahighpurityinertgasusingclean,(plasticizer-andadditive-free)tubing methylene chloride (0.30 mg/10 mL). N{hexane has also been overthesamplecup. used with success. See Fig. 1 for a typical chromatogram. 11. Procedure 10.3 Solution#2—Dissolve200mgofthesamplein10mL THF(200mg/10mL).Shake(orsonicate)thesolutionforfive 11.1 Establish that the analytical system contains concen- minutes—seeNote6.Thesolutionislikelytorangefromclear trations of phthalate contamination that are lower than the FIG.1Solution#1—PhthalatesStandardMixture(see10.2) --``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`--- Copyright ASTM International 3 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT D7823 − 16 bDaactkagQroF--``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`---uIuGanl.idt2ycSOoonlbutjateimocntiinv#ae2ts—iobCnyharaocncmaelapyttzoaigbnrlgaem1ts0o(µTthLICe)oopffrToPHjVeFcC.twsipthecTihfirceeDifferentPlasticizers,TD-GC/MSAnalysis(see10.3and11.3) Copyright ASTM International 4 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT D7823 − 16 --``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`--- FIG.3Solution#2—ReproducibilityofPVC-DINCH(n=6)(see10.3and11.3) Copyright ASTM International 5 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT D7823 − 16 11.2 Establishtherelativeretentiontimeandmassspectrum ThermalDesorption(TD){GC/MSAnalysis of each phthalate using Solution #1—10.2: The following TDtemperature: 100{20°C/min{320°C(5minhold) Pyinterface: 320°C(Automode), conditions were used to obtain the example chromatograms GCinjector: 300°C shown in Figs. 1-4: FIG.4Solution#3—StandardAddition(see11.7) --``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`--- Copyright ASTM International 6 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT D7823 − 16 responsethatisonlyduetoDNOPandnotDOTPneedstotake GCoven: 80(1minhold)to200°C(at50°C/ min)to320°C(15°C/min,2minhold) into account principles of chromatographic peak shape and Solventdelay: 6min areas.4 Column: UA{5(5%Diphenyl{95%dimethyl polysiloxane)30mby0.25mmi.d, NOTE 10—Use the coefficient of determination, R2, to monitor the 0.25µmfilm)orequivalent qualityofthecalibration.TypicaltheR2valuesforalltargetphthalatesare ColumnHeflow: 1.2mL/min,Splitratio:1/20 0.99orbetter—seeFig.5. Massrange: 29{600m/z, Scanspeed: 2.57scans/sec, 12. Example calculations Threshold: 50 MSDTransferLineTemp.: 300°C 12.1 Atypicalsetofstandardadditioncurvesarepresented IonSource(EI)temp.: 230°C inFig.5.IncludedinFig.5isanexampleofhowtocalculate 11.2.1 Confirm the TD zone using Evolved Gas Analysis the concentration of the target phthalate and the analytical (EGA){MS. The total ion chromatogram of the sample (Solu- precision (n=6) of the method. tion#2,10.3)needstobesimilartothatpresentedinAppendix 13. Quality Control X1. 13.1 Perform the quality checks outlined in Table 2. 11.3 Analyze the sample (Solution #2, 10.3) using the TABLE2SystemPerformanceVerification conditionsoutlinedin11.2.Typicalchromatogramsareshown in Figs. 2 and 3.The precision of theTD method is shown in SampleDescription Frequency Rationale MethodBlank10µL Priortosampleanalysis Verifiesthatthe Fig. 3. trtTdahhenaataetd1beta1lqn,ec.utt4fioh1aounen.nlPfiltPetsrsihiamoocmtklnahieensnaiglldiesaiseoxstietntutoehrtrqnadiecfiusceiptcaneaanhdontTttiifhdoatiaaobntlttnlhsaiheoteecena1h.r.qiireUosoTunmsabhbenaeaaatststraheoeesidegadosrunuparmopeamnaotapisktnotirsoaotaehfrnlaeaebpsatboipreveoiteinhedfandekgttitrhhceeameeartrmeteaqqenadduiutsneiaaoeonniidnnsftt LSSbTaHaaebmmFf1oopp3rrall.eeet2o1#ra01yEnCµnaLolsnyoutfzrroielngthseamsypPa1a1sn0n0lrtieeddosssmraaaa.tmmffottPeeppisrrsrllaeeitthhmssofeerrpelaaetennoaaaonllyysafssaliiymsspsooihpsfftlheaaVtsspbltlehhayonheeveeslttlraueoheticpfietllwaiherymoolocarsntfsojhtoe.aipetmehcsnnhetbadtm’tshtatasohtaacDhmtgxlkeaaerQigbmatierasiOnplouitbthosaumyieicntcloiktdiofbtiynys --``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`--- ion can be used to accurately determine the amount of the of the system to perform properly shall be verified. phthalate. 13.3 The run{to{run precision for all phthalates shall be 11.5 If using selected ion monitoring (SIM), peak identifi- better than 5 % RSD. Report the precision. cation is based solely on the presence or absence of the quant ion and the two confirming ions at a predetermined retention 14. Report time. Quantitation is based on the area of the quant ion. 14.1 The amount of each target phthalate in ppm. 11.6 WhenDINPandDIDParebothpresentinasampleor 14.1.1 Analyze10%ofthesamplesintriplicate,reportthe standard,usem/z127asaqualifyingionforDINPandm/z289 standard deviation for each target compound. If the sample for DIDP. This is because DINP and DIDP partially co{elute batch is less than 10 samples, then analyze one sample in and both produce m/z 149 and 167. If 149 qualifier ion ratios triplicate and report the standard deviation. aresetwhenDINPandDIDPareatequalconcentrations,then 14.1.2 If a sample batch is analyzed over more than two any samples with different ratios will produce substantially days, the percent difference between the first and last Labora- different149/167ratios,potentiallyleadingtoafalsenegative. tory control sample must be less the 10. NOTE 9—Atypical total ion chromatogram obtained using the condi- 14.2 Reporttheconcentration(ppm)ofeachtargetphthalate tionsspecifiedin11.2isshowninFig.1.Becausetheabsoluteretention in the method blank. timesaredependentupontheentiretyoftheGCsystem;relativeretention times can be used to identify each phthalate. The choice of the base 14.3 Report the chromatographic conditions and note any phthalateislefttothelaboratory. deviations from those specified in 11.2. 11.7 Quantitation is done using standard addition.Analyze 14.4 Report the Coefficient of Determination for the cali- Solution#3.AtypicaltotalionchromatogramisshowninFig. bration line for each target phthalate. 4.Analyticalprecisionispresentedinthetableatthebottomof Fig. 4. Standard addition is very useful when it is difficult to 15. Precision and Bias eliminate interferences from the sample matrix. This is often 15.1 The precision of this test method is based on an the case when analyzing PVC where DINCH, Mesamoll or interlaboratory study of Test Method D7823, conducted in both are present. 2013. As many as four laboratories tested a single PVC 11.8 Payattentiontothechromatographicpeakshapeofthe materialforlowlevelphthalates.Every“testresult”represents DNOP as partial co{elution with di{octylterephthalate (which produces all the same ions in different ratios) has been 4Agoodoverviewofstandardadditioncanbefoundonpage476,LCGCNorth observed. Careful integration of quantifying ion (m/z 279) America,Vikyne27,number6,June2009 Copyright ASTM International 7 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT D7823 − 16 --``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`--- FIG.5QuantitativeResultsUsingStandardAddition(see12.1) anindividualdetermination,andallparticipantswereaskedto 15.1.1 Repeatability (r)—The difference between repetitive report four replicate test results. Except for the inclusion of results obtained by the same operator in a given laboratory only one test material, Practice E691 was followed for the applying the same test method with the same apparatus under designandanalysisofthedata;thedetailsaregiveninASTM constant operating conditions on identical test material within Research Report No. D20-1263.5 shortintervalsoftimewouldinthelongrun,inthenormaland correct operation of the test method, exceed the following 5SupportingdatahavebeenfiledatASTMInternationalHeadquartersandmay values only in one case in 20. beobtainedbyrequestingResearchReportRR:D20-1263.ContactASTMCustomer [email protected]. Copyright ASTM International 8 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT D7823 − 16 15.1.1.1 Repeatability can be interpreted as maximum dif- run, in the normal and correct operation of the test method, ference between two results, obtained under repeatability exceed the following values only in one case in 20. conditions, that is accepted asplausible due to random causes 15.1.2.1 Reproducibility can be interpreted as maximum under normal and correct operation of the test method. difference between two results, obtained under reproducibility 15.1.1.2 Repeatability limits are listed in Table 3. conditions, that is accepted as plausible due to random causes 15.1.2 Reproducibility (R)—The difference between two under normal and correct operation of the test method. single and independent results obtained by different operators 15.1.2.2 Reproducibility limits are listed in Table 3. applying the same test method in different laboratories using 15.1.3 The above terms (repeatability limit and reproduc- differentapparatusonidenticaltestmaterialwould,inthelong ibility limit) are used as specified in Practice E177. 15.1.4 Any judgment in accordance with statements 15.1.1 and 15.1.2 would have an approximate 95% probability of TABLE3PhthalatesinPVC(ppb) being correct. Repeatability Reproducibility 15.2 Bias—At the time of the study, there was no accepted Repeatability Reproducibility AverageA Standard Standard referencematerialsuitablefordeterminingthebiasforthistest Limit Limit Deviation Deviation method, therefore no statement on bias is being made. x¯ S S r R r R DIDP 961.695 21.078 62.601 59.018 175.284 15.3 The precision statement was determined through sta- DINP 1086.519 29.608 64.733 82.903 181.252 tistical examination of 68 test results, reported by four DnOP 1050.138 50.234 102.574 140.656 287.207 DOP 895.161 21.289 38.545 59.609 107.927 laboratories, on one material. BBP 808.738 35.820 80.857 100.295 226.400 15.4 To judge the equivalency of two test results, it is DBP 972.310 49.406 74.857 138.338 209.600 recommended to choose the material closest in characteristics ATheaverageofthelaboratories’calculatedaverages. to the test material. APPENDIXES (NonmandatoryInformation) X1. VERIFICATIONOFTHEEGATHERMALDESORPTIONZONE(SEENOTE9) X1.1 Thethermaldesorptionzoneforphthalatesascitedin NOTEX1.1—ForadiscussiononEGA{MS,Yuzawaetal.,Ana.Sci,25, 11.1 appears to be independent of the plasticizer used in the 1057(2009). PVC formulation. If it becomes necessary to confirm the X1.1.1 AtypicalEGAthermogramofPVCispresentedFig. thermal zone, EGA{MS is the method of choice. Thermo X1.1. gravimetric (TGA) analysis is an alternative. The thermal desorption zone is easily determined using evolved gas analy- sis. --``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`--- Copyright ASTM International 9 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT D7823 − 16 FIG.X1.1TypicalEGAThermogramofPVC X2. SAMPLEPREPARATION(SEENote6) X2.1 The biggest challenge when working with multi{ X2.3 When working with a heterogeneous sample, sample componentsamplesistoensurethatarepresentativesampleis aliquots should be randomly selected in order to ensure that a inhand.Fig.X2.1illustratestheneedforsamplehomogeneity. representative sample is being analyzed. In the sample shown One technique used for this is cryo milling (to <45 µm) inFig.X2.2,3mmdiskswerepunchedoutofthePVCsheet. although other techniques have proven to be just as effective. Thediskswerecombinedinaglassvial,solventwasaddedand The resulting small particles are well mixed before an aliquot the resulting solution was analyzed. is removed for analysis. X2.2 Solution #2 should be made using milligrams of sample. The more accurately the weight of the analytical sample is known, the more accurate is the phthalate determi- nation. --``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`--- Copyright ASTM International 10 Provided by IHS under license with ASTM Licensee=IranPaper.ir No reproduction or networking permitted without license from IHS Not for Resale, 06/14/2016 06:26:18 MDT

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