顶空-气相色谱-质谱法测定水中1,3-丁二烯和1-溴丙烷

Determination of 1,3-butadiene and 1-bromopropane in water by headspace-gas chromatography mass spectrometry

建立顶空-气相色谱-质谱法测定水中1,3-丁二烯和1-溴丙烷。对平衡温度、平衡时间和盐析效应进行了优化。在顶空瓶中预先加入3.0 g氯化钠,加入10.00 mL水样,在65℃条件下平衡30 min,使用TG-624色谱柱分离,选择离子扫描方式进行分析。1,3-丁二烯和1-溴丙烷的质量浓度在2~100μg/L内与色谱峰面积线性关系良好,相关系数分别为0.996和0.998;方法检出限分别为0.6、0.8μg/L;样品加标平均回收率为101%~113%,相对标准偏差为4.5%~8.2%(n=6)。该方法环境友好,重复性好,准确度高,适合水中1,3-丁二烯和1-溴丙烷的痕量分析。

A method was established by headspace gas chromatography mass spectrometry for the determination of 1,3-butadiene and 1-bromopropane in water.Equilibrium temperature,equilibrium time and salting out effect were optimized.3.0 g of sodium chloride was added to the headspace bottle,10.00 mL of water sample was added,equilibrated at 65°C for 30 min,separated by TG-624 chromatographic column,and analyzed by ion scanning mode.The calibration curves of 1,3-butadiene and 1-bromopropane were linear in the range of 2-100μg/L with correlation coefficients of 0.996 and 0.998,respectively.The detection limits of 1,3-butadiene and 1-bromopropane were 0.6 and 0.8μg/L,respectively.The average recoveries were 101%-113%.The relative standard deviations were 4.5%-8.2%(n=6).The method is environmentally friendly,repeatable and accurate,which is suitable for the trace analysis of 1,3-butadiene and 1-bromopropane in water.