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[目的]建立顶空气相色谱测定工作场所空气中苦味酸的方法。[方法]用微孔滤膜采集空气中苦味酸,纯水洗脱,次氯酸钠衍生顶空气相色谱电子捕获检测器检测。[结果]苦味酸浓度在0.01~1.00μg/m L范围内线性关系良好(r=0.999 7),本法检出限为0.000 06μg/m L(进样量为100μL),最低检出浓度为0.000 008 mg/m3(采样体积为75 L,解吸液体积为10 m L),相对标准偏差为1.42%~1.61%,平均回收率为97.9%~99.7%,平均洗脱效率为95.9%~97.3%,采样效率为95.1%~97.1%,微孔滤膜吸收10μg苦味酸,在室温条件下保存,至少可稳定15 d。[结论]该方法各项指标均符合GBZ/T 210.4—2008《职业卫生标准制定指南第4部分:工作场所空气中化学物质测定方法》的要求,适用于工作场所空气中苦味酸的检测。
[Objective] To establish a method for determination of picric acid in the air by headspace gas chromatography. [Method] Picric acid in air was collected with microporous membrane and pure water was eluted. Sodium hypochlorite derivatized headspace gas chromatography electron capture detector was used to detect. [Result] The linear relationship between picric acid concentration in the range of 0.01-1.00 μg / mL was good (r = 0.999 7). The detection limit of this method was 0.000 06 μg / mL (the injection volume was 100 μL). The lowest detection limit was The relative standard deviations were 1.42% ~ 1.61% with the average recovery of 97.9% ~ 99.7%. The average elution efficiency was 95.9% ~ 97.3 %, Sampling efficiency of 95.1% ~ 97.1%, microporous membrane absorption of picric acid 10μg, at room temperature, at least stable for 15 d. [Conclusion] The indexes of the method all met the requirements of GBZ / T 210.4-2008 Occupational Health Standard Setting Guide Part 4: Determination of Chemical Substances in the Air at Workplace, which is suitable for the detection of picric acid in the air of workplace.