采用聚苯胺改性四氧化三铁负载磁性纳米固相萃取材料建立了磁性固相萃取-电感耦合等离子体质谱方法,并将其用于制革废水中微量重金属钴、镉、铜、镍及锌的检测分析.经固相萃取条件优化,在萃取pH值为8和最优洗脱液为5 mL 2 mol/L的硝酸溶液时,各重金属的萃取回收率均高于95％,该方法可以耐受较高浓度的共存离子影响.各重金属元素的标准曲线线性关系良好(r＞0.999),检出限＜0.07μg/L.方法日内精密度、日间精密度分别为2.62％～6.77％和2.75％～6.76％,方法加标回收率为95.55％～107.3％,方法具有优异的精密度和准确度,可应用于制革废水的重金属元素分析.在不同工艺段的实际制革废水重金属检测应用中,废水收集箱、沉淀池、生化处理出水池和氧化出水池等不同工艺段的制革废水重金属均有所检出.
Simultaneous Determination of Heavy Metals in Tannery Wastewater by Magnetic Solid Phase Extraction and I CP-MS
A magnetic solid-phase extraction inductively coupled plasma mass spectrometry method was established using polyaniline modified ferric oxide loaded magnetic nano solid-phase extraction material,and it was used for the detection and analysis of trace heavy metals such as cobalt,cadmium,copper,nickel and zinc in tannery wastewater.After optimization of solid-phase extraction conditions,the extraction recovery rates of various heavy metals were higher than 95％in a nitric acid solution with an extraction pH of 8 and an optimal eluent of 5 mL 2mol/L.This method can tolerate the influence of coexisting ions at higher concentrations.The standard curves of various heavy metal elements have a good linear relationship(r＞0.999),and the detection limit is less than 0.07 µ g/L.The intra day precision and inter day precision of the method are 2.62％～6.77％and 2.75％～6.76％,respectively.The recovery rate of the method with added standard is 95.55％～107.3％.The method has excellent precision and accuracy and can be applied to the analysis of heavy metal elements in tannery wastewater.In the application of heavy metal detection in actual tannery wastewater in different process stages,including wastewater collection tanks,sedimentation tanks,biochemical treatment effluent tanks and oxidation effluent tanks,heavy metals in tannery wastewater were detected.
tanning wastewaterheavy metalsmagnetic solid-phase extractioninductively coupled plasma mass spectrometry
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