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-1-UNITEDSTATES美国CONSUMERPRODUCTSAFETYCOMMISSION消费品安全委员会DIRECTORATEFORLABORATORYSCIENCES实验室科学理事会DIVISIONOFCHEMISTRY化学部10901DARNESTOWNRDDARNESTOWN路10901号GAITHERSBURG,MD20878马里兰GAITHERSBURG城20878TestMethod:CPSC-CH-C1001-09.3测试方法：CPSC-CH-C1001-09.3StandardOperatingProcedureforDeterminationofPhthalates邻苯二甲酸酯测定的标准操作程序April1st,20102010年4月1日ThisdocumentprovidesdetailedinformationontestmethodsthatwillbeusedbytheU.S.ConsumerProductSafetyCommission’s(CPSC)testinglaboratory(LSC)fortheanalysisofphthalatecontentinchildren’stoysandchildcarearticlescoveredbythestandardsetforthintheConsumerProductSafetyImprovementActSection108.这篇文章详细描述了美国消费品安全委员会（CPSC）测试室（LSC）所涵盖的消费者产品安全改进法案第108中规定的儿童玩具和护理品中邻苯二甲酸酯的测试方法。IthasbeenconcludedthatinordertoprotectchildrenfromthehazardtheActintendedtoaddress,that“concentrationsofmorethan0.1percent”mustapplyperplasticizedcomponentpartofachildren’stoyorchildcarearticle1.它决议出为保护儿童危害行为地方，每一个儿童的玩具或儿童护理品1的部位每种增塑剂“浓度超过0.1%”。1StatementofPolicy:TestingofComponentPartswithrespecttoSection108oftheCPSIA,August7,2009()1法律声明：测试部件遵守消费者产品安全改进法案第108款，8月1日，2009-2-CPSCstaffhasdeterminedthatusinganappropriatecombinationofmethodsofextractionandanalysispresentedhereinissufficienttodeterminetheconcentrationofthesixregulatedphthalatesinmostconsumerproducts.Adjustmentsmaybenecessaryforproductsmadefromcertainmaterials,andshouldbebasedonsoundchemistryandmaterialsscienceknowledgeaswellasappropriatesolventsforthematerials.Thegeneralapproachistodissolvethesamplecompletelyintetrahydrofuran,precipitateanyPVCpolymerwithhexanes,filterandthendilutethesolutionwithcyclohexane,andanalyzebyGasChromatography-MassSpectrometry(GC-MS).CPSC确定用一个合适的组合方法能够测定大多数消费品中六种受限制的邻苯二甲酸酯浓度。某些特定的材料产品可能需要调整和基于健康的化学和材料科学知识也要有对材料合适的溶剂。一般通过在四氢呋喃完全溶解它，用正己烷沉淀聚氯乙烯，过滤，然后用环己烷稀释溶液，并用气相色谱质谱联用仪（GC-MS）分析。Definitions定义1.Sample–Anindividualconsumerproductoragroupofidenticalconsumerproductsfromabatchtobetested.样品-从一批货中调出用于检测的个别消费品或一组同样的消费品。2.ComponentPart–Individualsub-unitwithinaproduct.组成部件-产品内部的子单位。3.LaboratoryReagentBlank(LRB)–Analiquotofsolventsthatistreatedexactlyasasampleincludingexposuretoglassware,apparatusandconditionsusedforaparticulartest,butwithnoaddedsample.LRBdataareusedtoassesscontaminationfromthelaboratoryenvironment.空白实验试剂（LRB）-一种没有添加样品，同样品一样经过玻璃器皿、设备和条件下测试的一定量溶剂。LRB数据是用于评估从实验环境下受污染的程度。4.StockStandard–Phthalate(s)purchasedfromreputablecommercialsourceatthehighestavailablepurity,usedtopreparecalibrationstandards.Replacebeforeexpirationdate.储备标准-从规范的供应商购买的用于配制校准标准纯邻苯二甲酸酯。在产品有效期前替换掉它。-3-5.CalibrationStandard–Solutionscontainingthephthalate(s)ofinterestincyclohexane.Eachstandardshouldcontain20µg/mlinternalstandardwhenrunninga20:1splitinjection,or1µg/mlforsplitlessinjection.Aminimumoffourcalibrationstandardsareused.Calibrationstandardsshouldbepreparedasneedfromthestocksolutionandmaybestoredatroomtemperature.Recordweightofsolutionsbeforeandafterusetomonitorforsolventevaporation.Standardsshouldbereplacedwhenexperimentaldatademonstratesadecreaseinqualityorsignificantlossinsolventweight.校准标准-在环己烷中含目标邻苯二甲酸酯浓度的溶液。当运行20:1分流进样时，每一个标准溶液必须包含20µg/mL的内标物或使用1µg/mL不分流进样。昀少要用四个校准标准。校准标准如果需要，从储备溶液中重新配制并在室温下保存，记录前后溶剂的重量以监控溶剂蒸发。当超过有效期，证明质量或溶剂质量大的流失，需要替换标准溶液。6.QualityControlSample(QCS)–Solutionscontainingknownamountsofphthalatesthatareusedtoevaluatetheperformanceoftheanalyticalinstrumentsystem.QCSsareobtainedfromasourceexternaltothelaboratoryandarenotmadefromtheStockStandardsolutions.Forexample,certifiedreferencematerials(CRMs)areavailablefromtheNationalInstituteofStandardsandTechnology(NIST),suchasthoselistedintheEquipmentandSuppliessectionbelow.质量控制样（QCS）-含有用于评价分析仪器性能的已知一定量的邻苯二甲酸酯溶液。质量控制样是从本实验室外部获得的，并非是从标准储备溶液配制得来。例如，标准物质（CRM）能从美国标准物质技术研究院得到，例如这些信息在下列仪器和供应品一节中列出。EquipmentandSupplies仪器和供应品Thematerialsusedforsamplingandanalysesareasfollows:下列这些材料用于制样和分析：1.Tetrahydrofuran(C4H8O,THF),GCgradeorhigher四氢呋喃（C4H8O,THF），色谱纯或更高2.Hexane(C6H12),GCgradeorhigher正己烷(C6H12)，色谱纯或更高3.Cyclohexane(C6H12),GCgradeorhigher环己烷(C6H12)，色谱纯或更高4.SealableglassvialswithPTFEorsiliconelinere,size20mlorlarger.用聚四氟乙烯或硅树脂衬垫密封的20mL玻璃瓶；或更大的。-4-5.Cryogenic-mill(orsuitablealternativetogrindsamplestopowder)低温研磨机（或合适可用于研磨样品至粉末的）6.PTFEfilters,0.45µm.0.45µm聚四氟乙烯滤器7.GasChromatograph-MassSpectrometer(GC-MS)withanauto-sampler,split/splitlessinlet,programmableGCoven,andcapableofselectiveionmonitoring.带自动进样器的气相色谱-质谱联用仪（GC-MS），分流/不分流进样，可编程的柱箱和可以进行离子选择监测。8.CRMscontainingphthalates(suchasNISTSRM3074)含邻苯二甲酸酯的标准物质（例如NISTSRM3074）9.BenzylBenzoate(C14H12O2,BB),analyticalgradeorhigher.苯甲酸苄酯(C14H12O2,BB)，分析级或更高10.DibutylPhthalate(C16H22O4,DBP),CASNo.84-74-2.analyticalgradeorhigher.邻苯二甲酸二丁酯(C16H22O4,DBP)，美国文摘登记号为84-74-2。分析级或更高。11.Di-(2-ethylhexyl)phthalate(C24H38O4,DEHP),CASNo.117-81-7.analyticalgradeorhigher.邻苯二甲酸二（2-乙基）己酯(C24H38O4,DEHP),CASNo.117-81-7.分析级或更高。12.BenzylButylPhthalate(C19H20O4,BBP),CASNo.85-68-7.analyticalgradeorhigher.邻苯二甲酸丁苄(C19H20O4,BBP),CASNo.85-68-7.分析级或更高13.Di-n-octylphthalate(C24H38O4,DnOP),CASNo.117-84-0.Analyticalgrade邻苯二甲酸二正辛酯(C24H38O4,DnOP),CASNo.11