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气相色谱-质谱法测定轮胎橡胶中6种邻苯二甲酸酯类化合物
Determination of 6 Phthalate Acid Esters in Tire Rubber by GC-MS
【Author】 Peng Shao1,,Shuang Lang1,Xiaojing Fan1,Jinghua Zhang1,Jinming Lin2 1.Beijing Center for Physical and Chemical Analysis,Beijing 100089 2.Department of Chemistry,Tsinghua University,Beijing 100084
【机构】 北京市理化分析测试中心; 清华大学化学系;
【摘要】 对轮胎橡胶以二氯甲烷为提取溶剂,通过自动索氏提取,提取液经硅胶固相萃取小柱富集净化,用气相色谱-质谱法(GC-MS)对样品中6种邻苯二甲酸酯(PAEs)进行检测。该方法具有良好线性,相关系数R在0.9986~0.9999之间,检测限为31.4~718.2μg/kg,6种PAEs的平均回收率为82.6%~112.4%,相对标准偏差(RSD)范围为2.8%~8.6%。检测实际加标样品结果为DBP:223 mg/kg,BBP:245 mg/kg,DEHP:225 mg/kg,DNOP:225 mg/kg,DINP:1161 mg/kg,DIDP:822 mg/kg。该方法具有操作简单、灵敏度高、重现性好等特点,满足了国内外在轮胎橡塑中邻苯二甲酸酯的检测需求,为国家标准的制定提供了技术参考。
【Abstract】 Tire rubbers were extracted by automated soxhlet extractor with diethyl ether(Optima grade) as the solvent,and the extracts were enriched and purified by silica gel solid phase extraction,the determination of 6 phthalate acid esters(PAEs) in tire rubbers by gas chromatography-mass spectrometry(GC-MS) was developed.The correlation coefficients(R) of 6 PAEs were ranged from 0.9986 to 0.9999,and detection limits from 31.43 μg/kg to 718 μg/kg.The average recoveries of 6 PAEs in tire rubbers were ranged from 82.6% to 112.4%.In addition,the relative standard deviations(RSDs) were ranged from 2.8% to 8.6%.The determination results of added PAEs tire rubber sample were DBP: 223 mg/kg,BBP: 245 mg /kg,DEHP: 225 mg /kg,DNOP: 225 mg /kg,DINP: 1161 mg /kg,DIDP: 822 mg /kg.The method had the advantage of simplicity,sensitivity and repeatability,and met the request for testing of PAEs in tire rubbers at home and abroad,and provided the technical reference for formulation of a national standard.
【Key words】 Tire Rubber; Phthalate Acid Esters; GC-MS; Automated Soxhlet Extraction;
- 【会议录名称】 中国化学会第28届学术年会第9分会场摘要集
- 【会议名称】中国化学会第28届学术年会
- 【会议时间】2012-04-13
- 【会议地点】中国四川成都
- 【分类号】TQ336.1;O657.63
- 【主办单位】中国化学会