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目的建立工作场所空气中对苯二胺毛细管气相色谱测定方法。方法硅胶管采样,乙醇解吸,SE-54毛细管色谱柱分离,在最佳仪器条件下用气相色谱仪测定,按照《工作场所空气中化学物质的测定方法》的要求,进行实验室方法研究。结果对苯二胺在0～1 120μg/ml之间有良好的线性关系,相关系数0.999 6。方法的最低检出浓度为0.39μg/ml(进样1μl解吸液,以3倍噪音计算),样品最低检出浓度为0.13 mg/m3(采样体积以3 L计)。分别测定高、中、低3个浓度的样品,进行6次重复测定,相对标准偏差为0.0%～0.45%,解吸效率为95.2%～96.4%。工作场所空气中与苯二胺共存的苯、甲苯、二甲苯、丙酮、二苯胺、苯胺、邻苯二胺、间苯二胺、联苯、三乙胺等对测定无干扰。结论本法简单、快速、灵敏度高、检出限低、共存物不干扰测定,适用于工作场所空气中对苯二胺的检测。
Objective To establish a method for the determination of p-phenylenediamine in the air of workplace by capillary gas chromatography. Methods Silicone tube sampling, ethanol desorption, SE-54 capillary column separation were performed with gas chromatograph under the best instrument conditions. The laboratory method was studied in accordance with the requirements of “Determination method of chemical substances in workplace air”. Results There was a good linear relationship between p-phenylenediamine and 0-1 120 μg / ml with a correlation coefficient of 0.999 6. The minimum detectable concentration of the method was 0.39 μg / ml (1 μl of desorption solution was injected with 3 times the noise). The minimum detectable concentration was 0.13 mg / m3 (sample volume was 3 L). The determination of high, medium and low concentrations of three samples, respectively, repeated determination of 6 times, the relative standard deviation of 0.0% to 0.45%, desorption efficiency of 95.2% to 96.4%. Benzene, toluene, xylene, acetone, diphenylamine, aniline, o-phenylenediamine, m-phenylenediamine, biphenyl, triethylamine co-exist in the air with phenylenediamine in the workplace. Conclusion This method is simple, rapid, sensitive, low detection limit, coexistence does not interfere with the determination of phenylenediamine in the workplace for the detection of air.