气相色谱法同时测定合成产物二甲基亚砜及其中杂质

Simultaneous determination of dimethyl sulfoxide and other components in synthetic product by gas chromatography

以工业废气硫化氢为原料制备精细化工产品二甲基亚砜,建立了气相色谱法同时测定合成产物二甲基亚砜及其中杂质的分析方法。采用150~180μm Porapak Q高分子微球填料的不锈钢填充柱分离样品,柱温采取程序升温,载气(H_(2))流量为48 mL/min,检测器为热导检测器(TCD),检测器温度为250℃,利用色谱峰面积归一化法进行定量分析。水、二甲基硫醚、二甲基亚砜、二甲基砜测定值的相对标准偏差均小于1.5%(n=6),加标回收率为96.0%~101.5%,满足定量分析的要求。该方法简单高效、快速,可为石油化工、有机合成、医药与医疗等行业高质量二甲基亚砜生产提供反馈和技术支撑。

Hydrogen sulfide(H2S) derived from petrochemical waste gas was used to prepare dimethyl sulfoxide(DMSO),a gas chromatography method was developed for the determination of dimethyl sulfoxide and other components in DMSO synthetic product.A stainless steel column packed with 150-180 μm Porapak Q polymer microspheres was used to analyse DMSO products,the column temperature was programmed and a thermal conductivity detector(TCD) was selected,the flow rate of carrier gas(H_2) was 48 mL/min,the detection temperature was 250 ℃,and the area normalization method was used for quantitative analysis.The relative standard deviations of the detect results of the components such as water,dimethyl sulfide,dimethyl sulfoxide and dimethyl sulfone were less than 1.5%(n=6),and the recoveries were in the ranges of 96.0%-101.5%,which met the detection requirement.This method is simple and efficient,and it can be effectively used in petrochemical,organic synthesis,medicine and medical production industries,and provided important feedback and technical support for the high quality production and high efficiency detection of dimethyl sulfoxide.