电子电气产品中氯化有机锡化合物的GC-MS分析法

Determination of Organotin Chloride Compounds in Electrical and Electronic Products by Gas Chromatography-mass Spectrometer

本文实验采用气相色谱-质谱法快速有效地测定了电子电气产品中常见的材料中可能含有的四种氯化有机锡化合物(氯化三丁基锡,二氯二丁基锡,三氯单丁基锡和氯化三苯基锡)。使用了甲醇作为萃取剂,利用超声萃取样品,然后调节提取液的p H值至4. 5,用四乙基硼酸钠进行衍生化,最后采用GC-MS进行定性定量分析。文章对样品的萃取条件和衍生化条件进行了优化,并优化了仪器条件。方法回收率在78. 2%～105. 3%;水平的变异系数在2. 33%～5. 72%,准确度和方法的精密度都符合要求。通过实践证明,可以有效的检测出电子电气产品中的四种有机锡,能达到低限度的要求,检测结果可以防止假阳性的影响,最终获得比较全面而准确的结果。

A rapid and effective method has been developed to determine organotin compounds in the electricaland electronic products with GC - MS, mainly for four types of chloride （ butyltintrichloride, di - n -butyltindichloride, tri - n - butyltin chloride and triphenyltin chloride）. The sample was ultrasonic extracted withmethanol. Then the target compounds were derivatized with sodium tetraethyl borate when the pH value is 4. 5.Subsequently the qualitative and quantitative analyses were carried out by GC - MS. In this paper, the extraction andderivatization conditions were optimized. And the average recoveries of the four kinds of chlorinated organotincompounds are 78. 2% ~ 105. 3% with the level of variation at 2. 33% ~ 5. 72%. The established method is accurateand sufficient for determination of organotin compounds in electrical and electronic products.