Feng Di, Yu Xingbei, Yan Meng, Du Hao
Occupational Hygiene Technology Services Co. , Ltd. , Nanhai West Oil Corporation, Zhanjiang 524057, China.
Wei Sheng Yan Jiu. 2021 Mar;50(2):310-314. doi: 10.19813/j.cnki.weishengyanjiu.2021.02.025.
To establish solvent desorption gas chromatograph method for o-toluidine determination in workplace air.
The o-toluidine vapour in workplace air was collected with silicone tube, and desorbed with absolute ethanol. Then the desorption solution was separated with polyethylene glycol HP-INNOWax capillary column(30 m×0. 32 mm, 0. 50 μm)and measured with flame ionization detector.
Detection limit of the method was 0. 18 μg/mL, quantification limit of the method was 0. 60 μg/mL, quantitative determination range of method was 0. 60-245. 37 μg/mL, and the minimum quantitative determination concentration was 0. 20 mg/m~3(based on 3. 0 L sample). The method had a good reproducibility, the relative standard deviation was 1. 0%-3. 5%, the average of desorption efficiency was 98. 7%, and the average of sampling efficiency was 93. 7%. The penetrating capacity of 200 mg alkaline silicone was over than 2. 1 mg, and the samples at room temperature could be preserved for 15 days at least. Methanol, toluene, chlorobenzene, acetoacetic ester, aniline, N-methylaniline, N, N-dimethylaniline, o-nitroaniline, p-toluidine or m-toluidine coexisted in the air did not interfere during the determination of o-toluidine.
The method with low determination concentration, high accuracy and precision, is feasible for determination of o-toluidine vapour in workplace air.
建立工作场所空气中邻甲苯胺的溶剂解吸气相色谱测定方法。
用硅胶管采集工作场所空气中的邻甲苯胺蒸气,用无水乙醇解吸。然后用聚乙二醇HP-INNOWax毛细管柱(30 m×0.32 mm,0.50μm)分离解吸液,用氢火焰离子化检测器测定。
该方法的检出限为0.18μg/mL,定量限为0.60μg/mL,定量测定范围为0.60 - 245.37μg/mL,最低定量测定浓度为0.20mg/m³(以3.0L样品计)。该方法具有良好的重现性,相对标准偏差为1.0% - 3.5%,解吸效率平均为98.7%,采样效率平均为93.7%。200mg碱性硅胶的穿透容量大于2.1mg,样品在室温下至少可保存15天。空气中共存的甲醇、甲苯、氯苯、乙酰乙酸乙酯、苯胺、N-甲基苯胺、N,N-二甲基苯胺、邻硝基苯胺、对甲苯胺或间甲苯胺在邻甲苯胺测定过程中不产生干扰。
该方法测定浓度低、准确度和精密度高,可用于工作场所空气中邻甲苯胺蒸气的测定。