SPME/GC-MS分析废水中苯酚与五氯酚方法的比较研究

Ji-Young Kyung, Yo-yong Kim, S. Hwang, Wo-kyung Nam, K. Park, Tae-Hwa Kim
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引用次数: 1

摘要

现行水污染检验标准方法中用于分析苯酚和五氯酚的溶剂萃取法,由于使用的溶剂量大,预处理时间长,不易执行。因此,采用不需要萃取溶剂的固相微萃取(SPME)法作为预处理方法,研究其替代传统溶剂萃取法的适用性。对纤维吸附条件、NaCl浓度、吸附时间、搅拌速度和搅拌温度进行了优化。此外,我们评估了这些条件是否满足标准方法的QA/ q要求。并对出水进行回收试验,采用苯酚和五氯酚配对t检验对溶剂萃取法和SPME法的试验结果进行统计学比较。因此,两种方法对五氯酚的测定结果存在差异。结果表明,SPME法的定量限为0.948 μg/L,定量限为3.020 μg/L,精密度为1.8%,准确度为97.7%。验证试验表明,SPME法对出水苯酚的回收率可达95%以上。此外,由于配对t检验表明SPME法与溶剂萃取法没有差异,因此SPME法可以取代溶剂萃取法进行苯酚分析。
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Comparative Study of Phenol and Pentachlorophenol Analysis Methods in Wastewater by SPME/GC-MS
The solvent extraction method for the analysis of phenol and pentachlorophenol in the present standard methods for the examination of water pollution is not easy to perform due to the use of a large amount of solvent and long pretreatment time. Therefore, the solid phase microextraction (SPME) method, which does not require an extraction solvent, was used a pretreatment approach and its applicability as an alternative to the conventional solvent extraction method was studied. The SPME conditions of fiber adsorption, concentration of NaCl, adsorption time, stirring speed, and stirrer temperature were optimized.Moreover, we assessed whether these conditions satisfied the QA/QCrequirements of the standard methods. In addition, the recovery test was performed on the effluent, and the test results of the solvent extraction and SPME methods were statistically compared by the paired t-test for phenol and pentachlorophenol analyses. As a result, there was a difference in the results of the two methods for pentachlorophenol. Therefore, the SPME method was not adequate, but phenol was judged to be appropriate as it showed 0.948 μg/L of LOD, 3.020 μg/L of LOQ, 1.8% of precision and 97.7% of accuracy. In addition, the validation test indicated that the recovery of phenol in the effluent was better than 95% by SPME. Moreover, because the paired t-test showed that the SPME method was not different from the solvent extraction method, the SPME method can replace the solvent extraction method for phenol analysis.
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