FI-HG-AFS for Determination of Trace Amount of Cadmium in Natural Water
摘 要
基于编结反应器,提出了流动注射-氢化物发生-原子荧光光谱法测定水中痕量镉含量的方法.样品与氨水-氯化铵缓冲溶液在线混合,产生的沉淀收集到编结反应器内壁,引入空气除去编结反应器内残留的溶液,泵入盐酸(3+97)溶液溶解沉淀,与硼氢化钾合并后用原子荧光光谱仪测定.在优化的试验条件下,当样品消耗15.6 mL时,富集倍数为14倍,方法检出限(3S/N)为2.9 ng·L-1,相对标准偏差(n=11)为3.4%.方法用于国家标准物质和天然水样中痕量镉的测定,测定值与标准值相符,天然水样的回收率在91.5%~107.5%之间.
Abstract
FI-HG-AFS by using knotted reactors (KR) was applied to the determination of trace amount of cadmium in natural water.The sample was on-line mixed with ammonia(aq.)-ammonium chloride buffer solution,and the precipitate of cadmium was collected on the inner walls of the knotted reactor.The removal of the residual solution from KR was achieved by introduction of air flow,and the precipitate was dissolved by HCl (3+97) solution.The solution obtained was mixed with KBH4 solution and used for HG-AFS detection.Under the optimal experimental conditions,an enrichment factor of 14 was obtained with sample consumption of 15.6 mL.The detection limit (3S/N)of the method found was 2.9 ng·L-1 and RSD (n=11) found was 3.4%.The proposed method was used for analysis of standard reference materials and natural water samples,the results of determination obtained was in agreement with the standard values,and values of recovery of Cd in natural water samples were ranged from 91.5% to 107.5%.
中图分类号 O657.31
所属栏目 试验与研究
基金项目 江苏省高校自然科学基金(07KJB150112),江苏省自然科学基金(BK2008121)
收稿日期 2009/1/2
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备注吴萍兰(1968-),女,江苏靖江人,兽医师,主要从事环境分析方法研究.
引用该论文: WU Ping-lan,CHEN Rong-shun,ZHANG Ya-jie,WU Hong. FI-HG-AFS for Determination of Trace Amount of Cadmium in Natural Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2010, 46(3): 217~219
吴萍兰,陈荣顺,张雅洁,吴宏. 流动注射-氢化物发生-原子荧光光谱法测定天然水中痕量镉[J]. 理化检验-化学分册, 2010, 46(3): 217~219
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参考文献
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【2】YEBRA M C,ENRIQUEZ M F,CESPON R M.Preconcentration and flame atomic absorption spectrometry determination of cadmium in mussels by an on-line continuous precipitation dissolution flow system[J].Talanta,2000,52(4):631-636.
【3】WANG Yang,CHEN Ming-li,WANG Jian-hua.Sequential/bead injection lab-on-valve incorporating a renewable microcolumn for coprecipitate preconcentration of cadmium coupled to hydride generation atomic fluorescence spectrometry[J].J Anal At Spectrom,2006,21(5):535-538.
【4】ANTHEMIDIS A N,ZACHARIADIS G A,STRATIS J A.Development of an on-line solvent extraction system for electrothermal atomic absorption spectrometry utilizing a new gravitational phase separator.Determination of cadmium in natural waters and urine samples[J].J Anal At Spectrom,2003,18(11):1400-1403.
【5】FANG Guo-zhen,TAN Jin,YAN Xiu-ping.An ion-imprinted functionalized silica gel sorbent prepared by a surface imprinting technique combined with a sol-gel process for selective solid phase extraction of cadmium(Ⅱ)[J].Anal Chem,2005,77(6):1734-1739.
【6】姚波,徐淑坤,方肇伦.流动注射在线吸着分离预浓集冷蒸气原子吸收法测定痕量镉[J].高等学校化学学报,2001,22(8):1301-1304.
【7】吴宏,金焰,毕树平.流动注射编结反应器在线富集新进展[J].分析化学,2007,35(6):905-911.
【8】WU Hong,FANG Chao,DU Bai-xiang.Flow injection on-line preconcentration coupled with hydride generation atomic fluorescence spectrometry for ultra-trace amounts of cadmium determination in seawater[J].Microchim Acta,2008,160(1):173-178.
【9】SUN Han-wen,SUO Ran.Enhancement reagents for simultaneous vapor generation of zinc and cadmium with intermittent flow system coupled to atomic fluorescence spectrometry[J].Anal Chim Acta,2004,509(1):71-76.
【10】王义壮,邱海鸥,汤志勇,等.流动注射在线离子交换分离-蒸气发生原子荧光测定沉积物中的镉[J].光谱学与光谱分析,2007,27(12):2581-2584.
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