固相萃取-高效液相色谱法测定废水中4种氯苯类有机污染物

[目的]采用固相萃取-高效液相色谱法测定废水中4种氯苯类有机污染物。[方法]利用固相萃取技术,结合高效液相色谱法(PDA检测器)分析废水中4种氯苯类有机污染物,比较了ODS-C18、Sep-Park Vac Silica、Bond Elut CARBON、Bond Elut SI和Bond ElutPLEXA 5种SPE小柱对4种氯苯类的萃取效率,并系统研究了最佳萃取条件。[结果]氯苯、1,4-二氯苯和1,2,4-三氯苯的紫外检测波长为210 nm,而1,2-二氯苯的检测波长为224 nm;通过比较5种SPE小柱的萃取效率,发现ODS-C18小柱有很好的回收率。甲醇的最佳洗脱体积为4.0 ml;除氯苯外,其他氯苯类化合物的穿透体积都在1.0 L以上,而氯苯的穿透体积为250 ml,表明ODS-C18小柱对二氯苯和三氯苯具有很强的吸附性。在最佳萃取和测定条件下,该方法线性范围为0.005～0.100 mg/L,检出限为0.076～0.105μg/L,完全满足日常环境监测分析要求。[结论]该研究为氯苯类环境监测分析提供了参考。

Determination of Four Chlorobenzene Compounds in Waste Water by SPE-HPLC

[ Objective] The study aims to determine four chlorobenzene compounds in waste water by SPE-HPLC. [ Method] A method for determination of four chlorobenzene compounds in waste water by solid phase extraction with HPLC-PAD detection was investigated, then the extraction efficiency of four ehlorobenzene compounds by five SPE columns （ODS-C18, Sep-Park Vac Silica, Bond Elut CARBON, Bond Elut SI and Bond Elut PLEXA） was compared, finally the optimal extraction conditions were discussed. [ Result ] The UV detection wavelength of chlorobenzene, 1,4-DCB and 1,2,4-TCB was 210 nm, but that of 1,2-DCB was 224 nm. Among the five SPE columns, ODS-C18 column has the best recovery. 4.0 ml methanol is as eluting solvent; the breakthrough volume of most compounds is above 1.0 L, but that of chloroben- zene is 250 ml, showing that ODS-C18 column has a strong adsorption to dichlorobenzene and trichlorobenzene. Under the optimized condi- tions, the linear range was O. 005 - 0. 100 mg/L, and the detection limit was 0.076 - 0. 105 μg/L, which fully meets the requirements of dai- ly environmental monitoring and analysis. [ Conclusion] The research can provide references for monitoring and analysis of ehlorobenzene eom- oouuds.