摘要
建立了高效液相色谱(HPLC)分离-氢化物发生(HG)-动态反应池(DRC)-电感耦合等离子体质谱仪(ICP-MS)联用分析电子企业废水中砷形态的方法。在样品送入DRC-ICP-MS检测器之前,先以HPLC将不同的砷物种分离,以分别得到各砷物种信号。使用HG技术来提升As信号,以增加灵敏度;采用L-半胱氨酸(L-cys)来消除废水中其它金属离子基底干扰;结合动态反应池(DRC)来消除75ArCl+对75As+造成的光谱干扰。实验探讨了HPLC洗脱液的最佳组成、氢化物生成的最佳试剂条件以及DRC最佳化相关参数。结果表明:以pH6.0的甲醇(φ=5%)-3mmol/L四丁基磷酸铵-8mmol/LNH4Ac作为HPLC流动相,5g/LNaBH4作为HG系统的氢气发生剂,以5g/LL-cys作为掩蔽和增敏剂,控制反应气流速为1.5mL/min时,4种As物种都有最佳的分离和检测效果。结果表明:该分析方法对上述4种砷形态的检出限均在0.01ng/L以下,在0.01～3000ng/L范围内线性关系良好,对实际样品检测回收率为86%～104%,样品中的Cl-对测定没有影响。所建立的HPLC-HG-DRC-ICP-MS分析方法适用于快速、批量测定电子企业废水中砷形态。
A method for the simultaneous determination of arsenic species in electronic factory waste water was established by high performance liquid chromatography（HPLC）-hydride generation（HG）- dynamic reaction cell（DRC）-inductively coupled plasma mass spectrometry （ICP-MS）. In order to get the species signals, different arsenic species were separated hy HPLC before introduced into the DRC- ICP-MS detector. In further experiment, hydride generation technology was employed for the enrichment of As in samples to enhance their sensitivity; L-cysteine was chosen to mask the interference of other ion matrix; dynamic reaction cell （DRC） was used to overcome the spectral interference of ^75ArCl^＋ on ^75As. Besides, the optimum composition of eluent for HPLC, the dosage of reagents in hydride generation and the optimized parameters of DRC were also discussed. The four species of As could be completely separated with methanol （φ=5 %）-3 mmol/L TBAP-8 mmol/L NH4Ac as HPLC flow phase at pH 6.0. A good separation and determination result was achieved when 5 g/L NaBH4 was used for hydride generation, 5 g/L L-cys was used as mask and enhanced sensitivity reagent, and the flow rate of reaction gas was controlled at 1. 5 mL/min. The detection limits of the proposed method for the four arsenic species were all below 0.01 ng/L. The linear relationship was good in the content range of 0.01-3 000 ng/L. The recoveries for actual samples were 86 %- 104 %. Cl^- in sample matrix did not interfere in the determination. Thus, the HPLC-HG-DRC-ICP-MS could be applied to the rapid and batch determination of arsenic species in waste water of electronic factory.
出处
《冶金分析》
CAS
CSCD
北大核心
2009年第4期14-19,共6页
Metallurgical Analysis
基金
浙江省自然科学基金(Y4080023&Y4080017)
宁波市自然科学基金(No.2008A610043&2008A610072&2008C50014)
宁波大学王宽城基金资助项目
关键词
氢化物发生
动态反应池
电感耦合等离子体质谱
电子废水
砷
形态分析
hydride generation
dynamic reaction cell
inductively coupled plasma mass spectrometry
electronic waste water
arsenic
species analysis
