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采用在线螯合富集模式,将海水中被测元素富集在螯合柱上,通过净化后的缓冲溶液冲洗螯合柱,除去海水中盐分基质,然后经10%HNO3溶液洗脱,使待测物质随着洗脱液直接进入ICP-MS进行分析测定;从而建立了在线分离富集-ICPMS直接测定海水中Y,La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu等15种稀土元素含量的分析方法。在ICP-M S最优化条件下,15种稀土元素在1.0~500 pg/m L范围内,线性相关系数在0.999以上,方法检出限(S/N=3)为0.01~1.1 pg/m L,采用不同盐度海水添加回收率在95%~115%,相对标准偏差(RSD)小于5%。应用NRCC(加拿大国家科学研究委员会)的SLEW-3标样进行方法检验,结果与NRCC参考值接近。
The chelate enrichment mode is adopted to enrich the measured elements in the seawater on the chelating column, and the chelating column is washed by the purified buffer solution to remove the salt matrix in the seawater and then eluted with 10% HNO3 solution The analytes were directly analyzed by ICP-MS with the eluent. The on-line separation and enrichment-ICPMS was established for the direct determination of Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho in seawater , Er, Tm, Yb, Lu and other 15 kinds of rare earth elements analysis method. Under ICP-M S optimization conditions, the linear correlation coefficients of 15 rare earth elements in the range of 1.0-500 pg / m L were above 0.999, and the detection limits (S / N = 3) were 0.01-1.1 pg / m L, the recoveries of seawater with different salinity ranges from 95% to 115%, and the relative standard deviations (RSDs) are less than 5%. The method validation was performed using the SLEW-3 standard from the NRCC (National Science Council of Canada) and the results were close to the NRCC reference values.