HG-AFS Determination of Selenium in Water with Field-Enanced Stacking
摘 要
采用场强放大堆积-氢化物发生-原子荧光光谱法测定水中硒的含量。设计了场强放大堆积装置,在电场作用下,硒阴离子可以从水样中迁移到高电导率的富集液中而实现硒的富集。优化的试验条件如下:①电极距离为4 cm;②富集腔体积为3.0 mL;③富集液为磷酸盐缓冲溶液;④场电流为80 mA;⑤富集时间为8 min。硒的质量浓度在3.0~200 ng·L-1内与其对应的荧光强度呈线性关系,检出限(3σ)为1.8 ng·L-1。在20 ng·L-1浓度水平进行加标回收试验,回收率为98.0%~106%。方法应用于国家标准样品GSBZ 50031-94的分析,测定值与认定值相符,测定值的相对标准偏差(n=5)为1.2%。
Abstract
HG-AFS was applied to the determination of selenium in water with field-enanced stacking. A field-enhanced stacking equipment was developed. Under application of electric field, selenium anion was migrated from water sample solution to enrichment solution of higher conductivity and concentrated. The optimized conditions found were as follows: ① electrode distance was 4 cm; ② volume of enrichment cavity was 3.0 mL; ③ enrichment solution was PBS; ④ field current was 80 mA; ⑤ enrichment time was 8 min. Linear relationship between values of fluorescence intensity and mass concentration of selenium was kept in the range of 3.0-200 ng·L-1, with detection limit (3σ) of 1.8 ng·L-1. Tests for recovery were made by standard addition method at the concentration level of 20 ng·L-1, giving values of recovery in the range of 98.0%-106%. The proposed method was applied to the analysis of national standard sample GSBZ 50031-94, giving result in consistency with the certified value with RSD (n=5) of 1.2%.
中图分类号 O657.31 DOI 10.11973/lhjy-hx201802009
所属栏目 工作简报
基金项目 安徽中烟工业有限责任公司联合实验室科技项目(2015124)
收稿日期 2017/2/23
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备注林作敏(1992-),女,河南商城人,硕士研究生,研究方向为仪器联用技术
引用该论文: LIN Zuomin,HUANG Miao,XU Zhiqiang,GAN Wuer. HG-AFS Determination of Selenium in Water with Field-Enanced Stacking[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(2): 167~171
林作敏,黄淼,徐志强,淦五二. 场强放大堆积-氢化物发生-原子荧光光谱法测定水中硒[J]. 理化检验-化学分册, 2018, 54(2): 167~171
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【3】王欣,幸苑娜,陈泽勇,等.高效液相色谱-电感耦合等离子体质谱法检测富硒食品中6种硒形态[J].分析化学, 2013,41(11):1669-1674.
【4】李春盈,张玉英.植物类中药材及饮片中18种重金属及有害元素研究[J].分析测试学报, 2016,35(1):1634-1638.
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【6】SANCHEZ-RODAS D, MELLANO F, MORALES E, et al. A simplified method for inorganic selenium and selenoaminoacids speciation based on HPLC-TR-HG-AFS[J]. Talanta, 2013,106(15):298-304.
【7】KARLSSON S, SJOBERG V, OGAR A. Comparison of MP AES and ICP-MS for analysis of principal and selected trace elements in nitric acid digests of sunflower (Helianthus annuus)[J]. Talanta, 2015,135:124-132.
【8】林立,孙海波,孙继红.离子色谱-电感耦合等离子体质谱法测定奶粉中的硒形态[J].理化检验-化学分册, 2015,51(9):1227-1231.
【9】鲁丹,俞琰垒.顺序注射-氢化物发生-原子荧光光谱法测定海产品中无机硒和有机硒[J].理化检验-化学分册, 2016,52(6):639-642.
【10】ZHANG W B, GAN W E, SHAO L J, et al. Flow-injection online reduction atomic fluorescence spectrometrydetermination of Se(IV) and Se(VI) with electrochemical hydride generation[J]. Spectroscopy Letters, 2006,39(6):533-545.
【11】EVANS E H, DAY J A, PALMER C D, et al. Atomic spectrometry update. Advances in atomic emission,absorption, and fluorescence spectrometry, and related techniques[J]. Journal of Analytical Atomic Spectrometry, 2008,23(6):889-918.
【12】MENTASTI E, NICOLOTTI A, PORTA N, et al. Comparison of different pre-concentration methods for the determination of trace levels of arsenic, cadmium, copper, mercury, lead and selenium[J]. Analyst, 1989,114(9):1113-1117.
【13】BIDARI A, JAHROMI E Z, ASSADI Y, et al. Monitoring of selenium in water samples using dispersive liquid-liquid microextraction followed by iridium-modified tube graphite furnace atomic absorption spectrometry[J]. Microchemical Journal, 2007,87(1):6-12.
【14】VOLKAN M, ATAMAN O Y, HOWARD A. Pre-concentration of some trace metals from sea water on a mercapto-modified silica gel[J]. Analyst, 1987,112(10):1409-1412.
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