金属络合效应对草酸HPLC分析的影响及消除.docVIP

收稿日期：2017-06-27 作者简介：吴雨涵（1993-），女，江苏人，硕士生，研究方向为电镀络合物。 通信联系人：孙贤波，E-mail：xbsun@ecust.edu.cn DOI:10.14135/j.cnki.1006-3080.20170614001 金属络合效应对草酸HPLC分析的影响及消除 吴雨涵，孙贤波，徐宏勇 （华东理工大学资源与环境工程学院，国家环境保护化工过程环境风险评价与控制重点实验室，上海 200237） 摘要：电镀废水中“金属-络合剂”带来的络合效应可能会降低高效液相色谱（HPLC）对络合剂分析的准确度。本文以镍-草酸作为模式化合物，考察了络合效应对于络合剂草酸HPLC分析的影响，发现200 mg/L的镍离子对草酸定性分析的影响较小，保留时间的变化幅度为1.0%；200 mg/L的镍离子对草酸定量分析的影响较大，峰面积的分析误差为33.7%。采用氢氧化物沉淀法来消除络合效应，使得峰面积的变化幅度降为1.7%，提高了电镀废水中草酸HPLC分析的准确度。 关键词：络合效应；草酸；HPLC；破络 中图分类号：X832.1 文献标志码：A Influence and Elimination of Complexation Effect on HPLC Analysis of Oxalic Acid WU Yu-han, SUN Xian-bo, XU Hong-yong (State Environmental Protection Key Laboratory of Environmental Risk Assessment and Control on Chemical Process, East China University of Science and Technology, Shanghai 200237, China) Abstract: The article is mainly about the complexation effect and the useful method to eliminate this effect. The discussion of the experiment result is about the high performance liquid chromatography (HPLC) analysis of nickel-oxalic acid and hydroxide precipitation pretreatment. It is known that the complexation effect is caused by metal ions and complexing agents and it will promote the formation of metal-complexing agents under the different conditions. The complexation effect brought by metal-complexing agents may reduce the analytical accuracy of complexing agents by HPLC. Since there are various kinds of metal-complexing agents in the electroplating wastewater, nickel-oxalic acid is chosen to be the typical metal-complexing agent in this paper. The research on the analysis of oxalic acid by HPLC that can be influenced by the complexation effect has been studied further. The UV-visible wavelength scanning is assisted to verify that the complexation effect has made a big impact on the HPLC analysis of oxalic acid. The HPLC analysis of oxalic acid is divided into the qualitative analysis and the quantitative analysis. The qualitative analysis is from the data of