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目的建立工作场所空气中二苯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《工作场所空气中毒物检测的研制规范》的要求,进行实验室方法研究。结果二苯胺在0～815.2μg/ml之间有良好的线性关系,相关系数0.999 7。方法的最低检出量为0.35μg/ml(进样1μl解吸液,以3倍噪音计算),最低检出浓度为0.12 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1.2%～4.3%,解吸效率为90.32%～102.07%。工作场所空气中与二苯胺共存的苯、甲苯、二甲苯、丙酮、异丙醇、苯胺、邻苯二胺、邻苯二甲酸二丁酯、联苯胺等对测定无干扰。结论本法各项指标已达到《工作场所空气中毒物检测的研制规范》的要求,适用于工作场所空气中二苯胺的检测。
Objective To establish a method for the determination of diphenylamine capillary gas chromatography in the air of workplace. Methods Silicone tube sampling, ethanol desorption, SE-54 capillary column separation were performed by gas chromatograph under the best instrument conditions. The laboratory method was studied in accordance with the requirements of “Development Specification of Air Toxics Detection in Workplace”. Results Diphenylamine had a good linearity between 0 and 815.2 μg / ml with a correlation coefficient of 0.999 7. The minimum detectable amount of this method is 0.35 μg / ml (1 μl of desorption solution is injected with 3 times noise) and the minimum detectable concentration is 0.12 mg / m3 (sampling volume is 3 L). The determination of high, medium and low concentration of three samples were repeated 6 times, the relative standard deviation of 1.2% to 4.3%, desorption efficiency of 90.32% ~ 102.07%. Benzene, toluene, xylene, acetone, isopropanol, aniline, o-phenylenediamine, dibutyl phthalate and benzidine in the air of the workplace coexisted with diphenylamine. Conclusions The indicators of this law have reached the requirements of “normative norms for the detection of airborne poison in the workplace” and are applicable to the detection of diphenylamine in the air of the workplace.