工作场所空气中硫酸二甲酯测定的气质联用仪法

Determination of dimethyl sulfate in the air of workplace by GC-MS

目的 建立工作场所空气中硫酸二甲酯（DMS）的气质联用（GC-MS）仪测定方法.方法 工作场所空气中的DMS经硅胶管吸附,硅胶倒入解吸瓶后,加入1.0 ml丙酮,振摇1 min,放置30 min后,解吸液由GC-MS仪进行定性和定量测定.结果 该方法的线性范围为0.1-200.0μg/ml,方程为y=11810x-4943（r=0.999）;批内精密度为2.6%-4.7%,批间精密度为4.0%-9.0%;方法检出限为0.1μg/ml,最低检出浓度为0.02 mg/m^3（以采样4.5 L计）;平均解吸效率均大于90%.结论 该方法前处理简单,分析周期短,优化了线性范围、检测限等指标,适用于工作场所空气中DMS的测定.

Objective To establish a method to detect the concentrations of dimethyl sulfate in the air of workplace by GC-MS. Methods DMS in the air of workplace adsorpted by Silicone tube, then desorped by acetone, add 1.0 ml of acetone, shake 1 min, placed after 30 min, the desorption solution qualitative and quantitative determination by gas chromatography-mass. Results The calibration curves were liner in the range of 0.1-200.0μg/ml. The within-run and between-run precisions were 2.6%-4.7%and 4.0%-9.0%respectively. The method detection limit is 0.1μg/ml, the minimum detectable concentration is 0.02 mg/m3（in terms of sampling 4.5 L）. Add 1 ml of desorption liquid, place 30 min, the average desorption efficiency of more than 90%. Conclusion This method has simple pretreatment, short analysis period, and optimized linear rage and limit of detection, and is suitable for the determination of DMS in workplace air.