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目的建立作业场所空气中硝基苯的快速定性、定量的便携式气质联用的检测方法。方法使用静态配气法配制一定浓度的硝基苯标准气,在实验室建立硝基苯浓度的回归方程,然后在工作场所使用便携式气质联用仪直接采样,对空气中硝基苯进行浓度定量与定性识别,同时使用国家标准方法对空气中的硝基苯浓度进行实验室分析,比较不同方法的检测结果,以确认所建立方法的准确度。结果空气中硝基苯浓度在0.753~30.120 mg/m~3时具有很好的线性;回归方程为Y=6×10~(-8)X+0.095 1,r=0.998;检出限0.038 mg/m~3;定量下限0.376 mg/m~3。高、中、低3个浓度下的精密度(RSD)在0.3%~4.7%之间;批间精密度(RSD)在2.5%~7.3%之间,测量准确度在102.1%~114.3%之间;与国家标准检测方法比较,GC-MS结果在标准方法结果的75.0%~94.3%之间。空气中苯、甲苯、苯乙烯等物质对测定不产生干扰。结论便携式GC-MS能直接检测空气中硝基苯浓度,方法准确、简便、快速,能反映空气中硝基苯的真实浓度,结果与实验室标准方法检测结果差异无统计学意义,适合于工作场所空气中硝基苯浓度的检测。
Objective To establish a rapid qualitative and quantitative method for the detection of nitrobenzene in workplace air by portable GC / MS. Methods A static gas distribution method was used to prepare nitrobenzene standard gas with a certain concentration. A regression equation of nitrobenzene concentration was established in the laboratory. Then, a sample of the nitrobenzene concentration in the air was directly sampled at the workplace. And qualitative identification, at the same time using the national standard method of nitrobenzene concentration in the air laboratory analysis, comparison of different methods of test results to confirm the accuracy of the established method. Results The concentration of nitrobenzene in the air was good at 0.753 ~ 30.120 mg / m ~ 3. The regression equation was Y = 6 × 10 -8 + X = 0.095 1, r = 0.998. The detection limit was 0.038 mg / m ~ 3; the lower limit of quantification is 0.376 mg / m ~ 3. The precision (RSD) was between 0.3% and 4.7% at three concentrations of high, medium and low, and the RSD was between 2.5% and 7.3% with the accuracy of 102.1% to 114.3% ; Compared with the national standard detection method, the GC-MS results are between 75.0% and 94.3% of the standard method results. Air benzene, toluene, styrene and other substances do not interfere with the determination. Conclusion Portable GC-MS can directly detect nitrobenzene concentration in the air. The method is accurate, simple and rapid and can reflect the true concentration of nitrobenzene in the air. The results are in good agreement with those of the laboratory standard method Nitrobenzene concentration in the air at the test site.