69理化测试NO.022023塑料科技PlasticsScienceandTechnology全蒸发顶空气相色谱法测定聚乙醇酸中的乙酸乙酯含量王睿,肖含,刘俊彦,张育红（中国石油化工股份有限公司上海石油化工研究院，上海201208）摘要：采用全蒸发顶空气相色谱法，建立了聚乙醇酸中残留溶剂乙酸乙酯含量的分析方法。在顶空平衡温度130℃，平衡时间90min的条件下，采用DB-FFAP毛细管色谱柱（30m×0.25mm×0.25μm）进行分离、氢火焰离子化检测器检测和外标法定量的分析方案，实现聚乙醇酸中残留溶剂乙酸乙酯的准确测定。标准曲线的线性相关系数（R2）为0.9978，加标回收率在98.1%~99.4%之间，6次重复测定结果的相对标准偏差<4%，最低检测限为0.47mg/kg，表明方法重复性和准确性良好，检测灵敏。本方法无需样品前处理，操作简便，结果准确可靠，适用于聚乙醇酸中残留乙酸乙酯的检测。关键词：聚乙醇酸；残留溶剂；乙酸乙酯；顶空气相色谱法中图分类号：O657.71文献标识码：A文章编号：1005-3360（2023）02-0069-04DOI：10.15925/j.cnki.issn1005-3360.2023.02.014Full-EvaporationHeadspaceGasChromatographyforDeterminationofEthylacetateContentinPolyglycolicAcidWANGRui,XIAOHan,LIUJun-yan,ZHANGYu-hong(SINOPECShanghaiResearchInstituteofPetrochemicalTechnology,Shanghai201208,China)Abstract：Amethodforthedeterminationofresidualsolventethylacetateinpolyglycolicacidbyfull-evaporationheadspacegaschromatographywasestablished.Undertheconditionsofheadspaceequilibriumtemperatureof130℃andequilibriumtimeof90min,theDB-FFAPcapillarycolumn(30m×0.25mm×0.25μm)wasusedforseparation,withhydrogenflameionizationdetectordetectionandexternalstandardmethodforquantitativeanalysistodeterminetheresidualsolventethylacetateinpolyglycolicacid.Thelinearcorrelationcoefficient(R2)ofthestandardcurveis0.9978,andtherecoverybystandardadditionmethodisintherangeof98.1%and99.4%.Therelativestandarddeviationof6repetitionsislessthan4%,andtheminimumdetectionlimitis0.47mg/kg.Therefore,themethodhasgoodrepeatabilityandaccuracy,andthedetectionissensitive.Thismethoddoesnotrequiresamplepretreatment,whichissimpletooperate,andthedeterminationresultsareaccurateandreliable.Itissuitableforthedetectionofresidualethylacetateinpolyg...
