污水处理厂中氯贝酸分析检测方法的建立和优化

目的]建立并优化污水处理系统中氯贝酸的分析检测方法。方法]以上海市两个污水处理厂的污水为样品,对样品的固相萃取和衍生化方法进行了优化,GC/MS检测时采用选择离子扫描(SIM)模式定性定量检测样品。结果]固相萃取过程中,氯贝酸的最优萃取条件为:HLB小柱,使用3 ml乙酸乙酯,3 ml甲醇和3 ml去离子水(pH=2～3)活化和8ml乙酸乙酯洗脱。衍生化条件为:衍生化试剂150μl,在70℃反应60 min。方法的检出限和定量检出限分别为0.31和1.03μg/L,回收率96.2%,相对标准偏差为6.61%(n=6)。结论]用优化后的方法检测上海市东区污水厂和曲阳污水处理厂进水氯贝酸的含量分别为66.3和20.3 ng/L,出水浓度分别为49.9和17.5 ng/L。

Establishment and Optimization of Determination Method for Clofibric Acid in Sewage Treatment Plant

Objective] The study aimed to establish and optimize the determination method for the clofibric acid in the sewage treatment system.Method] With the sewage from the 2 sewage treatment plants in Shanghai City as the samples,the solid phase extraction and derivatization conditions for the samples were optimized.In the GC/MS test,the selecting ion scan(SIM) model was used in the qualitative and quantitative determination on the samples.Result] In the solid phase extraction,the optimum extracting conditions for the clofibric acid was as follows: HLB small column,activated with 3 ml ethyl acetate,3 ml methanol and 3 ml de-ionized water at pH of 2-3,and then eluted with 8 ml ethyl acetate.The optimized derivatization condition was as follows: 150 μl derivatization reagent,reaction for 60 min at 70 ℃.The method detection limit and quantitative detection limit were 0.31 μg/L and 1.03 μg/L,resp.The recovery rate and the relative standard deviation were 96.2 % and 6.61 %(n=6) resp.Conclusion] When the optimized method was applied to investigate the occurrence of clofibric acid in Shanghai East Sewage Plant and Quyang Sewage Plant,the contents of clofibric acid in the influent were 66.3 and 20.3 ng/L,resp.and that in the effluent were 49.9 and 17.5 ng/L resp.