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目的建立工作场所空气中正丁基硫醇的气相色谱测定方法。方法 工作场所空气中的正丁基硫醇用Tenax采样管采集,样品经甲醇解吸,毛细管气相色谱柱分离(30.00 m×0.32 mm×3.00μm),火焰离子化检测器检测,以保留时间定性,峰面积定量。结果 本法正丁基硫醇质量浓度在1.70~100.40 mg/L呈线性关系,相关系数为0.999 96,最低检出浓度为0.10 mg/m3(以采集3.0 L空气样品计),精密度相对标准偏差为2.0%~2.8%,采样效率为98.7%~100.0%,平均解吸效率为91.9%,样品在-10℃冰箱中至少可保存7 d。结论 本方法灵敏度高,精密度和准确度好、操作简便、易普及,可作为工作场所空气中正丁基硫醇的标准检测方法。
Objective To establish a gas chromatographic method for the determination of n-butyl mercaptan in workplace air. Methods The n-butyl mercaptan in the air of the workplace was collected with a Tenax sampling tube. The sample was separated by methanol, separated by capillary gas chromatography (30.00 m × 0.32 mm × 3.00 μm) and detected by flame ionization detector. The retention time was qualitative, Peak area quantitative. Results The linear n-butyl mercaptan concentration ranged from 1.70 to 100.40 mg / L with a correlation coefficient of 0.999 96 and a minimum detectable concentration of 0.10 mg / m3 (with an air volume of 3.0 L), the relative standard precision The deviation was 2.0% -2.8%, the sampling efficiency was 98.7% -100.0%, and the average desorption efficiency was 91.9%. The samples could be stored in -10 ℃ refrigerator for at least 7 days. Conclusion The method has high sensitivity, precision and accuracy, easy to operate and easy to popularize. It can be used as the standard method for the detection of n-butyl mercaptan in the air of workplace.