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目的建立工作场所空气中1-溴丙烷(1-Bromopropane,1-BP)的毛细管柱气相色谱测定法。方法利用活性炭管采集工作场所中的1-溴丙烷,经二硫化碳(CS2)溶剂解吸,用FFAP毛细管柱分离,气相色谱-氢火焰离子化检测器检测。结果该方法线性范围在1.34μg/ml~535μg/ml,标准曲线的回归方程为y=1013.8775x-1170.2034,相关系数r2=0.9999,检出限为0.25μg/ml。以采集3.0 L空气样本计,空气中1-溴丙烷最低检出浓度为0.085 mg/m3。活性炭管中分别加入含2.66μg、13.3μg、66.5μg 1-BP的标准溶液过夜稳定后测定,加标回收率为95.6%~96.5%,批内、批间相对标准偏差分别为0.93%~2.41%、1.04%~2.08%,解吸效率为90.4%~92.3%。采样后的活性炭管在4℃条件下存放5 d,1-BP下降率为9.70%,20℃条件下下降率为46.7%。结论利用活性炭管采样,4℃保存,采用毛细管柱气相色谱测定,该方法操作简便,灵敏度高、精密度好、准确度好,稳定性好,适用于工作场所空气中1-溴丙烷浓度的测定。
Objective To establish a capillary gas chromatographic method for the determination of 1-Bromopropane (1-BP) in workplace air. Methods 1 - bromopropane in the workplace was collected by activated charcoal tube, desorbed by CS2 solvent, separated by FFAP capillary column and detected by gas chromatography - hydrogen flame ionization detector. Results The linear range of this method was 1.34μg / ml ~ 535μg / ml. The regression equation of the standard curve was y = 1013.8775x-1170.2034. The correlation coefficient r2 was 0.9999. The detection limit was 0.25μg / ml. To collect 3.0 L air samples, the minimum detectable concentration of 1-bromopropane in the air was 0.085 mg / m3. The standard solutions containing 2.66μg, 13.3μg and 66.5μg of 1-BP were added into the activated carbon tube and stabilized overnight. The recoveries were 95.6% -96.5%. The relative standard deviations (RSDs) were 0.93% ~ 2.41 %, 1.04% ~ 2.08%, desorption efficiency of 90.4% ~ 92.3%. The sampled activated carbon tube was stored at 4 ℃ for 5 days. The rate of decline of 1-BP was 9.70%, and the rate of decrease was 46.7% at 20 ℃. Conclusion The method is simple, sensitive, accurate, accurate and stable, and is suitable for the determination of 1-bromopropane concentration in the air of the workplace by using activated carbon tube sampling and storage at 4 ℃. .