N-ベンゾイル-N-フェニルヒドロキシルアミンを用いるニッケル中の微量の高原子価元素の抽出-逆抽出による分離

抄録

The separation and determination of trace amounts of Ti, Zr, Mo, Sn and Hf in Ni were studied. After the sample was dissolved with nitric acid, Ti, Zr, Mo, Sn and Hf were separated from Ni by extracting into benzene with N-benzoyl-N-phenylhydroxylamine (BPA) and subsequently back-extracted into nitric acid for the determination by ICP-AES or ICP-MS. The recoveries of Ti, Zr, Mo, Sn and Hf were satisfactory throughout the extraction with 4.0×10⁻² mol·dm⁻³ BPA in benzene from 1.0 mol·dm⁻³ nitric acid-0.1 mol·dm⁻³ trichloroaceticacid solution and the back- extraction with 60%nitric acid. The separation factors (S_M=D_M⁄D_Ni, D=distribution ratios) of Ti, Zr, Mo, Sn and Hf from Ni were 9.9×10³ for Ti, 3.2×10⁴ for Zr, 3.2×10⁴ for Mo, 1.3×10³ for Sn and 4.0×10⁴ for Hf. The recoveries of Ti, Zr, Mo, Sn and Hf decreased somewhat with increasing the added amount of Ni. The detection limits by ICP-MS were found to be 0.031 μg·g⁻¹ for Ti, 0.046 μg·g⁻¹ for Zr, 0.014 μg·g⁻¹ for Mo, 0.7 μg·g⁻¹ for Sn and 0.006 μg·g⁻¹ for Hf using 0.5 g of Ni sample. The proposed method was applied to analysis of the real sample.