静态顶空-气相色谱法测定水中二硫化碳

摘要

采用气相色谱法静态顶空进样,HP-1柱分离,FPD检测器检测,测定水中CS2,并对测定条件进行了探讨。实验表明,当取样量为10.0 mL,气液比为12.3,在40℃平衡25 min时,能获得满意的灵敏度,且稳定性很好。二硫化碳在0.63μg/L～502μg/L之间呈线性,相关系数为0.999 2,相对标准偏差为1.3%～5.7%、加标回收率为88%～105%,检出限可达0.3μg/L。干扰试验表明硫化氢、甲硫醇、甲硫醚不干扰二硫化碳的测定。本方法操作简便,测定快速,完全能够满足快速分析水中二硫化碳的要求。%CS2 concentration in water was determined by gas chromatography with static head-space injection,HP-1 column separation and FPD detector.The detection conditions were discussed.Experiment results show that satisfactory sensitivity and good stability could be acquired when the sample volume was 10.0mL,gas-liquid ratio was 12.3,and balanced at 40 ℃ for 25 min.CS2 detection concentration was linear from 0.63μg/L to 502μg/L,with correlation coefficient of 0.9992,relative standard deviation of 1.3%-5.7%,labeling recovery rate of 88%-105%,and the detection limit of 0.3 μg/L.Interference experiment results show that hydrogen sulfide,methyl mercaptan,dimethyl sulfide do not interfere with the detection of CS2.The method proposed is simple and rapid,meeting the requirements of rapid determination of CS2 in water.