气相色谱-表面发射火焰光度法测定电子电气产品中的氯化有机锡化合物

Determination of Organotin Chloride Compounds in Electrical and Electronic Products by Gas Chromatography with Flame Photometric Detector

本文实验采用气相色谱-表面发射火焰光度法（GC-FPD）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-FPD进行定性定量分析。文章对样品的萃取方法、萃取溶剂、萃取时间、萃取温度和衍生化条件进行了优化,并优化了仪器条件,主要是对工作气流量的优化,最后进行了线性关系、回收率、精密度和检测限的考察.结果表明,四种有机锡化合物能被很好的分离,方法的线性范围为0.01-1.0 mg/L,线性相关系数（R）为：0.999-0.9997。四种氯化有机锡化合物的回收率为78.2%-109.3%,相对标准偏差（n=7）均小于10%,方法具有较好的准确性和精密度。

A rapid and effective method has been developed to determine organotin compounds in the electrical and electronic products with GC- FPD（ gas chromatography with flame photometric detector）,mainly for four types of chloride（ butyltintrichloride,di- n- butyltindichloride,tri- n- butyltin chloride and triphenyltin chloride）. The sample was ultrasonic extracted with methanol. 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- FPD.In this paper,the extraction and derivatization conditions,such as method of extraction,extractive solvent and extraction temperature were optimized. Simultaneously the instrument conditions,mainly the working gas flow rate were optimized. Our results show that the linear ranges are 0. 01 - 1. 0 mg / L,the linear correlation coefficients（ R） of the four compounds are： 0. 999 - 0. 9997,and the average recoveries of the four kinds of chlorinated organotin compounds are 78. 2% - 109. 3% with the relative standard deviations（ n = 7） less than 10%. The established method is accurate and sufficient for determination of organotin compounds in electrical and electronic products.