溶解-沉淀-GC/MS法测定聚氯乙烯塑料中的邻苯二甲酸酯类增塑剂  

Determination of Phthalates in PVC Plastic through Solution-precipitation-GC/MS Method

作　　者：李丹[1] 周明辉[1] 刘莹峰[1] 郑建国[1] 翟翠萍[1] 

机构地区：[1]广东出入境检验检疫局,广东广州510623

出　　处：《塑料科技》2010年第3期92-96,共5页Plastics Science and Technology

基　　金："十一五"科技支撑项目"人体安全重要技术标准研制"(2006BAK04A10)

摘　　要：建立了用溶解-沉淀-GC/MS法同时测定聚氯乙烯(PVC)塑料中15种邻苯二甲酸酯类增塑剂的分析方法。选择四氢呋喃作溶剂将PVC树脂溶解,然后用甲醇作为沉淀剂将高聚物进行沉淀,使增塑剂与高聚物进行分离而增塑剂继续留在溶液中,取清液进行气相色谱-质谱分析。本实验选择了适当的溶剂与沉淀剂,考察了聚合物分子沉淀对目标化合物的吸附作用,在优化的色谱-质谱条件下实现了15种邻苯二甲酸酯的成功分离与检测,方法平均回收率为82.7%～112.4%,测定结果的相对标准偏差为2.15%～5.77%,测定下限(S/N=10)为25～50mg/kg。该方法操作简便,精密度高,准确性好,实用性强,与国家标准GB/T22048—2008相比,检测结果基本一致,而效率大大提高。应用此方法对两种PVC塑料实际样品中的邻苯二甲酸酯进行测定,获得满意结果。A method was established for the determination of phthalate plasticizer in PVC material by solution-precipitation pretreatment and GC/MS method.The sample was dissolved by tetrahydrofuran （THF） first,and then phthalates were separated from PVC polymer after methanol was added in drops into the solution which lead to the precipitation of polymer molecular while phthalates still remained in the supernatant.The proper solvent and precipitant were selected through performance tests,and the absorption of phthalates by the precipitated polymer was studied as well.Under the optimum separation and detection condition,the supernatant was analyzed by GC-MS and 15 phthalates were qualified and quantified at the same time.The recoveries ranged from 82.7% to 112.4%,with the RSD ranged from 2.15% to 5.77%,and the lower limit of determination could get to the level of 25～50mg/kg.This method was accurate,precise,easy to operate,and was time-saving comparing with GB/T 22048-2008.It was used to determinate the content of phthalates in 2 PVC products with satisfactory results.

关 键 词：聚氯乙烯 增塑剂 溶解-沉淀 气相色谱-质谱 

分 类 号：TQ325.3[化学工程—合成树脂塑料工业]