固相萃取光谱法结合多元校正同时测定水中痕量金属离子
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- 英文论文题名：Simultaneous Detection of Trace Metal Ions in Water by Solid Phase Extraction Spectroscopy Combined with Multivariate Calibration
- 论文作者：杜一平 ; 王蕾
- 英文论文作者：Yiping Du ; Lei Wang ; Research Center of Analysis and Test ; East China University of Science and Technology
- 年：2016
- 作者机构：华东理工大学分析测试中心;
- 论文关键词：固相萃取光谱 ; 多元校正 ; 同时测定 ; 金属离子
- 会议召开时间：2016-07-01
- 会议录名称：中国化学会第30届学术年会摘要集-第二十五分会：化学信息学与化学计量学
- 语种：中文
- 分类号：O657.3;X832
- 学会代码：ZGHY
- 会议名称：中国化学会第30届学术年会-第二十五分会 ; 化学信息学与化学计量学
- 会议地点：中国辽宁大连
- 主办单位：中国化学会
- 学会名称：中国化学会
- 页数：1
- 文件大小：304k
- 原文格式：D
- 会议级别：全国
摘要
传统可见光谱法测定金属离子往往灵敏度不高,检出限大致在mg/L水平,不适合痕量重金属离子的检测。本文提出一种将紫外可见光谱法与膜富集技术相结合的方法,将金属离子与螯合剂显色而生成的有机络合物富集到滤膜上后直接测量膜的漫反射光谱,并利用多元校正方法对光谱数据进行处理,实现溶液中多种重金属离子的同时测定。本方法操作便捷,检出限低。同时,通过将表面活性剂Brij-30先富集到膜上,对滤膜进行前期改性,结果表明Brij-30能够明显的降低检出限、提高灵敏度和稳定性。对影响实验过程的因素例如pH值、显色剂(PAN)用量、反应时间及抽滤真空度等进行优化。配制30个含有双金属Co~(2+)和Zn~(2+)的混合样品溶液,在最佳实验条件下测定可见光谱。用24个混合离子样本作为校正集建立模型,6个样本作为独立预测集对建立的模型进行评价。采用去一交互检验的方法确定多元校正模型的PLS因子数,使用该模型对预测集样本进行预测。Co~(2+)和Zn~(2+)的检出限分别达到0.066μg/L和0.104μg/L,明显低于传统可见光谱方法的检出限。对于矿物质水样品,Co~(2+)和Zn~(2+)的相对预测误差分别为6.65%和4.47%。
It is important to simultaneously detect trace concentration of heavy metals in real water samples.Traditional uv-vis transmission spectroscopy can't be applied on this detection because of high limit of detection.Solid phase extraction spectroscopy couple with multivariate calibration was proposed for simultaneous determination.The analytical conditions including pH,reaction time,sample volume,the amount of PAN,and flow rates were optimized.Nonionic surfactant Brij-30 was absorbed on themembranes prior to SPES to modify the membranes for improving the enrichment and spectrum measurement.Under optimal experiment conditions,leave-oneout cross-validation was utilized to choose the number of latent variables.24 samples were used as calibration set to build PLS model,while other 6 samples were used as independent prediction set to evaluate the built PLS model.Detection limits of Co~(2+) and Zn~(2+) estimated being 0.066 μg/L and0.104 μg/L,respectively were more lower than those of the traditional uv-vis method.For cobalt(Ⅱ) and zinc(Ⅱ),the relative errors of the prediction set were 6.65%and 4.47%.
It is important to simultaneously detect trace concentration of heavy metals in real water samples.Traditional uv-vis transmission spectroscopy can't be applied on this detection because of high limit of detection.Solid phase extraction spectroscopy couple with multivariate calibration was proposed for simultaneous determination.The analytical conditions including pH,reaction time,sample volume,the amount of PAN,and flow rates were optimized.Nonionic surfactant Brij-30 was absorbed on themembranes prior to SPES to modify the membranes for improving the enrichment and spectrum measurement.Under optimal experiment conditions,leave-oneout cross-validation was utilized to choose the number of latent variables.24 samples were used as calibration set to build PLS model,while other 6 samples were used as independent prediction set to evaluate the built PLS model.Detection limits of Co~(2+) and Zn~(2+) estimated being 0.066 μg/L and0.104 μg/L,respectively were more lower than those of the traditional uv-vis method.For cobalt(Ⅱ) and zinc(Ⅱ),the relative errors of the prediction set were 6.65%and 4.47%.
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