Simultaneous Determination of Ultra-trace Level of As,Sb,Bi,Ge,Sn and Hg in Coastal and Estuarine Seawater by Chemical Vapor Generation and Inductively Coupled Plasma Mass Spectrometry
建立了化学蒸汽发生(CVg)电感耦合等离子体质谱(ICP MS)同时测定近岸及河口海水中超痕量AS、Sb、bI、gE、Sn和Hg元素的方法。研究了CVg过程中kbH4、盐酸和硫脲的浓度以及样品流速、载气流速、海水样品盐度等对方法分析性能的影响。结果表明,在0.70%盐酸、0.10 g/l硫脲、11.0 g/l硼氢化钾、载气0.40 l/MIn条件下,6种待测元素的信噪比最高。优化实验条件下,AS、Sb、bI、gE、Sn和Hg的质量浓度在0.1~5.0μg/l内呈良好线性,相关系数不低于0.996 6;方法对0.1μg/l加标样品的相对标准偏差(rSd,n=5)为3.9%~8.9%,实际海水样品的加标回收率为89%~112%;方法的流程空白为0.012~0.036μg/l,定量下限(lOQS,10σ)在0.006 7~0.026μg/l之间,可满足近岸及河口海水样品中超痕量元素测定的需要。A chemical vapor generation(CVG) and inductively coupled plasma mass spectrometric(ICP MS) method was proposed for the simultaneous determination of ultra-trace level of As,Sb,Bi,Ge,Sn,and Hg in coastal and estuarine seawater.Effects of operating parameters,including concentrations of KBH4,HCl and thiourea,pump flow rate and carrier gas flow rate on analytical performance were studied.The results showed that good signal to noise(S/N) ratios for all the analysed elements were obtained when 0.70% HCl,0.10 g/L thiourea,11.0 g/L KBH4,and 0.40 L/min carrier gas were used in the CVG procedure.The relative standard deviations(RSDs,n=5) for 0.10 μg/L spiked sample were in the range of 3.9%-8.9%.The spiked recoveries for the seawater samples were between 89% and 112%.The method blanks were in the range of 0.012-0.036 μg/L.The limits of quantitation(LOQs,10σ) for the developed method were obtained between 0.006 7 μg/L and 0.026 μg/L.The method could be applied in the simultaneous determination of As,Sb,Bi,Ge,Sn and Hg in coastal and estuarine seawater.近海海洋环境科学国家重点实验室自主创新项目(MELRI0703
