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

14 Pages·2016·1.024 MB·English

by  John J (John James) Currier, 1834–1912

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.
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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.
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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)
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D7823 − 16
bDaactkagQroF--``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`---uIuGanl.idt2ycSOoonlbutjateimocntiinv#ae2ts—iobCnyharaocncmaelapyttzoaigbnrlgaem1ts0o(µTthLICe)oopffrToPHjVeFcC.twsipthecTihfirceeDifferentPlasticizers,TD-GC/MSAnalysis(see10.3and11.3)
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D7823 − 16
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FIG.3Solution#2—ReproducibilityofPVC-DINCH(n=6)(see10.3and11.3)
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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)
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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
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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].
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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.
--``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`---
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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.
--``,``,,,,`,,`,`,,``,``,````,,`-`-`,,`,,`,`,,`---
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