浸渍活性炭管采集溶剂解吸-气相色谱法同时测定空气中3种环氧化合物  

Simultaneous determination of three kinds of epoxy compounds in air adsorbed by dipped activated carbon tube with solvent desorption-gas chromatography

作　　者：戎伟丰[1,2] 黄汉林[2] 凌伟洁[3] 胡嘉雯 阮小林[2] 黄韬[2] 田东超 蒙瑞波[2] 吴邦华[2] 

机构地区：[1]中山大学公共卫生学院,广东广州510080 [2]广东省职业病防治院,广东省职业病防治重点实验室,510300 [3]广州市第十二人民医院,510620 [4]广东药学院公共卫生学院,510006 [5]深圳市职业病防治院,深圳518001

出　　处：《中国职业医学》2015年第1期59-65,共7页China Occupational Medicine

基　　金：广东省职业病防治重点实验室(2012A061400007);广东省医学科研基金(A2014072;B2013028)

摘　　要：目的研制用于捕集空气中环氧乙烷（EO）、环氧丙烷（PO）和环氧氯丙烷（ECH）的固体吸附剂管,并建立配套的气相色谱测定方法。方法基于EO、PO和ECH均能与氢溴酸发生开环反应的原理,以5%（V/V）氢溴酸-甲醇溶液为浸渍溶液制备固体吸附剂管,用于捕集空气中EO、PO和ECH。在捕集过程中各自生成相应的反应产物,经二甲基甲酰胺解吸后,毛细管色谱柱分离,电子捕获检测器测定。结果本方法 EO、PO和ECH的质量浓度分别在0.24～48.79、0.36～72.05和0.18～35.42 mg/L线性关系良好,相关系数均为0.999 97;最低检出浓度分别为0.01、0.01和0.02 mg/m3,最低定量浓度分别为0.02、0.02和0.05 mg/m3（以采集3.0 L空气计）;平均衍生效率分别为95.67%～97.38%、94.93%～98.27%和96.40%～98.24%;平均解吸效率分别为91.11%～94.78%、85.40%～88.03%和92.06%～95.32%;批内相对标准偏差分别为1.70%～2.87%、3.09%～3.42%和3.65%～4.47%,批间相对标准偏差分别为2.84%～5.48%、3.44%～3.88%和4.43%～5.65%;EO、PO和ECH样品在室温下至少可保存14 d。结论本方法研制的固体吸附剂管及其配套的浸渍活性炭管采集溶剂解吸-气相色谱法适用于工作场所空气、环境大气中EO、PO和ECH的采样以及检测。Objective To develop a new solid sorbent tube for simultaneously capturing ethylene oxide（ EO）,propylene oxide（ PO） and epichlorohydrin（ ECH） in air,and to establish a complete set of gas chromatography. Methods Based on the principle that EO,PO and ECH could all react with hydrobromic acid,the new solid sorbent tubes were developed with dipping solution of 5%（ V / V） hydrobromic acid-methanol solution,to capture EO,PO and ECH in air. The corresponding reaction products were generated in the process of capture,desorbed with dimethylformamide,separated through capillary chromatographic column separation,and then analyzed by gas chromatography-electron capture detector.Results The linear ranges of EO,PO and ECH were 0. 24-48. 79 mg / L,0. 36-72. 05 mg / L and 0. 18-35. 42 mg / L respectively,and the related coefficients were all 0. 999 97. The minimum detectable concentrations were 0. 01,0. 01 and0. 02 mg / m3 respectively and the minimum quantification concentrations were 0. 02,0. 02 and 0. 05 mg / m3respectively（ sample volume was 3. 0 L）. The average derivative efficiencies were 95. 67%-97. 38%, 94. 93%-98. 27%and 96. 40%-98. 24% respectively. The average desorption efficiencies were 91. 11%-94. 78%,85. 40%-88. 03% and92. 06%-95. 32% respectively. The relative standard deviations（ RSD） within the group were 1. 70%-2. 87%,3. 09%-3. 42% and 3. 65%-4. 47% respectively,and the RSD between the group were 2. 84%-5. 48%,3. 44%-3. 88% and4. 43%-5. 65% respectively. The samples could be stored at room temperature for at least 14 days. Conclusion The newly developedsolid sorbent tubes and its complete set of gas chromatography method could be used for sampling and quantitative detection of EO,PO and ECH in workplace air or ambient atmosphere.

关 键 词：固体吸附剂管 环氧乙烷 环氧丙烷 环氧氯丙烷 衍生反应 空气 气相色谱 

分 类 号：R134.4[医药卫生—劳动卫生]