Simultaneous Determination of Volatile Organic Pollutants in Water by Headspace Gas Chromatographic Analysis with Dual Detection

H. Ohno, T. Aoyama, H. Kishimoto
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引用次数: 3

Abstract

Headspace gas chromatographic analysis using a semi-wide bore capillary column and a dual detection system with a flame ionzation detector (FID) and an electron capture detector (ECD) was carried out for the simple and rapid simultaneous determination of 13 kinds of volatile organic pollutants : benzene (1), toluene (2), ethyl benzene (3), o-, m-and p-xylenes (4-6), monochlorobenzene (7), o-, m-and p-dichlorobenzenes (8-10), 1, 1, 1-trichloroethane (11), trichloroethylene (12) and tetrachloroethylene (13) in drinking water at low ppb (10-9g/ml) level. The effects of the headspace and syringe temperatures as well as the equilibration time and injection volume of headspace gas on the sensitivity and reproducibility of analysis were examined to find the optimal conditions. The capillary column permitted satisfactory separation of the target compounds except m-and p-xylenes (5 and 6) without interference by trihalomethanes in drinking water. FID was sensitive to all aromatic hydrocarbons (1-6) and monochlorobenzene (7) at 0.3-0.5 ppb, while ECD was poorly sensitive to them. By contrast, ECD was highly sensitive to chlorinated hydrocarbons (11-13) and aromatic chlorinated hydrocarbons except monochlorobenzene (8-10) with detection limits of 0.005-0.02 and 0.2-0.6 ppb, respectively, while FID was poorly sensitive to them. The coefficients of variation (n=4) in the simultaneous analysis using FID and ECD for sample water containing 0.1-20 ppb of the target compounds were 3.4-7.4% with good precision and reproducibility.
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双检测顶空气相色谱法同时测定水中挥发性有机污染物
采用半宽口径毛细管柱和火焰电离检测器(FID)和电子捕获检测器(ECD)双检测系统进行顶空气相色谱分析,对13种挥发性有机污染物进行了简单快速的同时测定:低PPB (10-9g/ml)饮用水中苯(1)、甲苯(2)、乙苯(3)、邻、间和对二甲苯(4-6)、一氯苯(7)、邻、间和对二氯苯(8-10)、1,1,1 -三氯乙烷(11)、三氯乙烯(12)和四氯乙烯(13)含量。考察了顶空温度、注射器温度、顶空气体平衡时间和进样量对分析灵敏度和重现性的影响,以确定最佳条件。毛细管柱对饮用水中除间二甲苯和对二甲苯(5和6)外的目标化合物进行了满意的分离,不受三卤甲烷的干扰。在0.3 ~ 0.5 ppb范围内,FID对所有芳烃(1 ~ 6)和一氯苯(7)敏感,而ECD对它们的敏感性较差。相比之下,ECD对氯代烃(11-13)和除一氯苯(8-10)外的芳香族氯代烃(8-10)高度敏感,检出限分别为0.005-0.02和0.2-0.6 ppb,而FID对它们的灵敏度较低。FID和ECD同时分析的变异系数(n=4)为3.4 ~ 7.4%,具有良好的精密度和重现性。
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