气相色谱法对水中硝基氯苯类化合物的测定

Determination of Nitrochlorobenzene Compounds in Water by Gas Chromatography

目的分析气相色谱法对水中硝基氯苯类化合物的测定效果,从而建立一种操作简便、灵敏度高的水中硝基氯苯测定方法。方法采集水样后,使用环己烷对水中的硝基氯苯类化合物进行液液萃取,经无水硫酸钠干燥后,使用环己烷将其定容至2 mL,使用50 mg的PSA对其进行净化,离心取上清液后对其进行气相色谱测定。结果在设定的色谱条件下,三种硝基氯苯均得到较好的分离,在1.00~50.00μg/L浓度范围内,三种硝基氯苯均具有良好线性关系,检出限在0.02μg/L以内,其相关系数均高于0.999。通过对其进行0.1、0.25、1.0μg/L三个加标水平的回收率和精密度测试,三种硝基氯苯的精密度在0.98%~2.96%,回收率在91%~97%,能够满足相关检测标准。经实际水样分析,结果满意。结论该测定方法具有操作简便,准确度高,回收率稳定及检出限低等优势,在基层实验室也能够推广应用。

Objective To establish a simple and highly sensitive method for the determination of nitrochlorobenzene in water by analyzing the effect of gas chromatography on the determination of nitrochlorobenzene compounds in water.Methods After collecting water samples,nitrochlorobenzene in water was extracted by liquid-liquid extraction with cyclohexane.After being dried by anhydrous sodium sulfate,it was diluted to 2 mL with cyclohexane,purified with 50 mg PSA,and centrifuged for determination by gas chromatography.Results Under the set chromatographic conditions,the three kinds of nitrochlorobenzene were well separated.In the concentration range of 1.00-50.00μg/L,the three kinds of nitrochlorobenzene had a good linear relationship,and the detection limit was within 0.02μg/L,and the correlation coefficients were all higher than 0.999.The precisions of nitrochlorobenzene were in the range of 0.98%-2.96%,and the recoveries were in the range of 91%-97%,which could meet the relevant detection standards.Through analysis of actual water sample,the results were satisfactory.Conclusion This determination method has the advantages of simple operation,high accuracy,stable recovery rate and low detection limit.It can also be popularized and applied in basic laboratories.