化学結合型シリカゲルを固相抽出剤に用いた固相抽出/ICP-MSによる高純度鉄中微量元素の定量

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We attempted a simple pretreating method consisting of solid phase extraction using bonded silica with benzenesulfonic acid (SCX) as the solid phase sorbent to determine trace elements in pure iron samples by means of inductively coupled plasma mass spectrometry (ICP-MS). The isotope dilution method was used along with the method mentioned above to ensure precise determination of Zn. We dissolved the sample of 1.00g by nitric acid, subsequently adding citric acid as masking agent. The analytes could be separated by 1-10 phenanthroline as chelate from the matrix by solid phase extraction after adjusting the pH and adding 1-10 phenanthroline. The optimum condition for iron separation was 0.01 kmol・m^<-3> 1-10 phenanthroline, 10cm^3; citric acid (10w/v%), 10cm^3; pH, 5.5; SCX, 0.5g as the solid phase sorbent; and nitric acid, 2 cm^3 as eluate. In this method, some trace elements such as Ni, Cu, Cd and Zn were determined by ICP-MS using the eluate. The limits of detection in ng/g were Ni 0.29, Cu 0.10, Cd 0.20 and Zn 0.15. We precisely determined the Zn content byjointly using the isotope dilution method.
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