采用X射线荧光光谱仪测试了二甲基二氯硅烷水解物中有机氯含量,通过减压蒸馏排除无机氯的干扰,使用标准加入法除去基体的干扰,解决了标准样不易获取的难题.采用该方法时需要对样品进行前处理,较佳的样品量为5 mL.该方法具有操作简单、分析速度快的优点,适用于二甲基二氯硅烷水解物中有机氯含量的日常快捷测试.
The Lead content in the production of methyl chorosilanes contact mass was determined by ICP-MS,and the impact of the elements interfering elements copper was studied.Considered the effection of different sample preparation methods on the Measured results.after contradistinction,Taking the methode of whicht,first using Aqua Regia heated and dissolved the solid,then using concentrated sulfuric acid eluted could receive an exceptional result,Lead Content from Silicon Contact Mass Determined towards 1.156ppm,with RSD only 1.03 %.
Analysis conditions of trichlorosilane by gas chromatography were studied,and the optimum analysis conditions of gas chromatography with capillary column for trichlorosilane were comfirmed.The liner range of this analysis method was determined with the defined analysis conditions,and linear correlation was obtained,i.e.R=0.999 93.Parallel and repeated tests were also carried out and results showed the method had good parallelity and repeatability.The relative standard deviation(RSD) of the mass fraction of trichlorosilane was less than 0.02% and the result was satisfied.
