工作场所空气中过氧化丁酮毛细管气相色谱测定方法研究

STUDY ON THE DETERMINATION OF METHYL ETHYL KETONE PEROXIDE IN THE AIR OF WORKPLACE BY CAPILLARY GAS CHROMATOGRAPHY

[目的]建立工作场所空气中过氧化丁酮毛细管气相色谱测定方法。[方法]活性碳管采样,甲醇解吸,FFAP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]过氧化丁酮在0-970μg/ml之间有良好的线性关系,相关系数0.9999。方法的最低检出量为2.57μg(进样1μl解吸液,以3倍噪音计算),最低检出浓度为1.7-mg/m3(采样体积以1.5L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0.5%-2.0%,解吸效率为90.40%-99.69%。工作场所空气中与过氧化丁酮共存的苯、甲苯、二甲苯、苯乙烯、丙酮、丁酮、乙醛、邻苯二甲酸二丁酯,对过氧化丁酮测定无干扰。[结论]本方法各项指标达到《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过氧化丁酮的检测。

[Objective] To establish a method to determine the methyl ethyl ketone peroxide in the air of workplace by capillary gas chromatography. [Methods] The methyl ethyl ketone peroxide in the air of workplace was sampled with activated carbon tube and eluted with methanol, separated by FFAP capillary column and determined by gas chromatography. The experimental study was conducted according to the requirements of Regulation of Studies on the Determination of Toxicants in the Air of Workplace. [Results] Methyl ethyl ketone peroxide showed good linearity at the range of 0-970ug/ml （r=0.9999） with the correlation coefficient of 0.999 9. The limit of detection was 2.57ug （S/N=3, injection volume： 1ul） and the limit of quantification was 1.71mg/m^3 per 1.5L of air. Samples of high, middle and low concentrations were re-determined for 6 times and the RSD was 0.5%-2.0% with the desorption efficiency at the range of 90.401% to 99.69%. Benzene, methylbenzene, xylene, acetone, Butanone, acetaldehyde and dibutylphthalate, which may coexist with methyl ethyl ketone peroxide in the air of workplace, had no interrupting influence on the determination of methyl ethyl ketone peroxide. [ Conclusion] Each index of the method can meet the requirements of Regulation of Studies on the Determination of Toxicants in the Air of Workplace, which is suitable to determine the methyl ethyl ketone peroxide in the air of workplace.