塑料成品及其稳定剂中三甲基氯化锡的气相色谱-质谱联用测定法

Application of Gas Chromatography-mass Spectrometer in Determining Trimethyl Stannic Chloride in Plastic Products and Stabilizing Agents

目的 建立塑料稳定剂及塑料成品中三甲基氯化锡的测定方法。方法 按照有关检测方法的研制规范的要求,研究了色谱条件的选择、样品的处理方法、回收率试验、萃取效率试验、方法的线性范围及检出限、方法的精密度等指标。结果 采用HP -5MS弹性毛细管石英柱(3 0m×0 .3 2mm×0 .2 5 μm)能将三甲基氯化锡和其他可能共存的有机锡完全分离。三甲基氯化锡含量在0 .0 5～2 40mg/kg范围内呈线性关系,相关系数为0 .9987,方法的最低检出浓度为0 .0 5mg/kg。对浓度为0 .4、4.0、40 .0 μg/ml配制样,方法的相对标准偏差(RSD )为4.0 %～8.2 %。方法的回收率为90 .5 %～97.5 %。塑料成品的萃取效率可达到90 %以上,样品在密封容器内至少可保存14d。结论 该方法各项指标均达到有关检测方法的研制规范的要求。

[Objective] To establish a method for detecting trimethyl stannic chloride in plastic products and stabilizing agents. [Methods] Study was carried out on such indexes as chromatography condition, sample disposal, recovery rate test, extraction efficiency test, linear range, detection limit and accuracy of the method. [Results] Trimethyl stannic chloride could be separated from other possibly existing organotin with HP-5 MS elastic capillary quartzose pillar (30 m×0.32 mm×0.25 μm). The content of trimethyl stannic chloride showed a linear relation within the range of 0.05～240 mg/kg. The lowest detection concentration was 0.05mg/kg; the recovery rate was 90.5%～97.5%; the extraction efficiency reached above 90%. [Conclusion] All the indexes of this method meet relevant standards; gas chromatography-mass spectrometer is applicable in detecting trimethyl stannic chloride in plastic products and stabilizing agents.