分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2014年
5期
753-758
,共6页
常燕%瞿建国%张瑞峰%张经
常燕%瞿建國%張瑞峰%張經
상연%구건국%장서봉%장경
氢化物发生%扇形磁场电感耦合等离子体质谱%天然水%硒%价态
氫化物髮生%扇形磁場電感耦閤等離子體質譜%天然水%硒%價態
경화물발생%선형자장전감우합등리자체질보%천연수%서%개태
Hydride generation%Inductively coupled plasma mass spectrometry%Natural water%Selenium%Speciation
通过对仪器参数、质谱干扰、Se同位素选择、NaBH4浓度、样品酸度、Se(Ⅵ)还原条件及氢化反应干扰的评估和优化,建立了自制连续流动氢化物发生装置与扇形磁场电感耦合等离子体质谱联用测定天然水中无机硒价态的分析方法,克服了天然水中多种元素对氢化反应的干扰,解决了不同介质样品中Se(Ⅵ)还原率保持95%以上时间短的问题。方法检出限为0.002μg/L,灵敏度为215378 cps/(μg/L),优于同类方法,测定河水和海水中Se(Ⅵ)和Se(Ⅵ)精密度小于4%,加标回收率在97%~103%之间,可应用于准确测定海水、河口区半咸水、河水等天然水中Se(Ⅵ)和Se(Ⅵ)浓度。
通過對儀器參數、質譜榦擾、Se同位素選擇、NaBH4濃度、樣品痠度、Se(Ⅵ)還原條件及氫化反應榦擾的評估和優化,建立瞭自製連續流動氫化物髮生裝置與扇形磁場電感耦閤等離子體質譜聯用測定天然水中無機硒價態的分析方法,剋服瞭天然水中多種元素對氫化反應的榦擾,解決瞭不同介質樣品中Se(Ⅵ)還原率保持95%以上時間短的問題。方法檢齣限為0.002μg/L,靈敏度為215378 cps/(μg/L),優于同類方法,測定河水和海水中Se(Ⅵ)和Se(Ⅵ)精密度小于4%,加標迴收率在97%~103%之間,可應用于準確測定海水、河口區半鹹水、河水等天然水中Se(Ⅵ)和Se(Ⅵ)濃度。
통과대의기삼수、질보간우、Se동위소선택、NaBH4농도、양품산도、Se(Ⅵ)환원조건급경화반응간우적평고화우화,건립료자제련속류동경화물발생장치여선형자장전감우합등리자체질보련용측정천연수중무궤서개태적분석방법,극복료천연수중다충원소대경화반응적간우,해결료불동개질양품중Se(Ⅵ)환원솔보지95%이상시간단적문제。방법검출한위0.002μg/L,령민도위215378 cps/(μg/L),우우동류방법,측정하수화해수중Se(Ⅵ)화Se(Ⅵ)정밀도소우4%,가표회수솔재97%~103%지간,가응용우준학측정해수、하구구반함수、하수등천연수중Se(Ⅵ)화Se(Ⅵ)농도。
By evaluating and optimizing instrument parameters, mass spectral interferences, selection of selenium isotopes, the concentration of NaBH4 , the acidity of samples, Se(Ⅵ) reduction conditions and the hydride generation interferences, a method was developed for measuring inorganic selenium speciation in natural water by sector field inductively coupled plasma mass spectrometry combined with laboratory made continuous-flow hydride generation, which overcame the hydride generation interference from various elements in the natural water and resolved the problem that Se(Ⅵ)reduction behavior was various in different matrix and the time of remaining stable reduction recovery was short. The detection limit was 0. 002 μg/L and the sensitivity was 215378 cps/(μg/L) which were superior to that of other similar methods. The precision of Se(Ⅵ) and Se(Ⅵ) in river water and seawater was lower than 4%, and the spiked recovery ranged from 97% -103%. Thus, the proposed procedure was a suitable method for determining the Se(Ⅵ)and Se(Ⅵ)concentration in natural water including seawater, saline water, river water and so on.