溶媒抽出-原子吸光法による銅,ニッケル,アルミニウムおよびウラン地金中の極微量カドミウムおよび亜鉛の定量

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An atomic absorption spectrophotometric method for the determination of cadmium and zinc in copper, nickel, aluminum and uranium metals has been presented. This method involves the extraction of cadmium and zinc with methyl iso-butylketone (MIBK) solution of tri-n-octylamine and the measurements of absorbances of the extract. Ten milligrams of Be2+, Bi3+, Co2+, Cr3+, Mg2+, Pb2+, Sn4+, and Zr4+, 1 mg of As(III), Fe3+, Ga3+, In3+, Mn2+ and V (V) and 6 N of SO42- do not interfere. More than 1 mg of Fe3+, 0.01 N of NO3- and 0.0001 N of CrO42- interfere. More than 1 mg of Zn2+ and Te(IV) interfere with the determination of cadmium, and more than 0.1 mg of Cd2+ and Te(IV) interfere with the determination of zinc. As little as 0.5 ppm of cadmium and zinc in copper, nickel, aluminum and uranium metals can be determined by this method. The recommended procedures are as follows. (1) Determination of Cd and Zn in copper and nickel metals: 1.0 g of sample is decomposed with 10.0 ml of HNO3(1+1). Ten milliliters of H2SO4 (1+1) is added and evaporated to fumes. It is transferred with 20 ml of HCl (1+1) into a separatory funnel and made up to 50 ml with water. It is shaken vigorously with 5.0 ml of 2 vol% tri-n-octylamine-MIBK solution for 5 minutes. The aqueous phase is transferred into another separatory funnel and shaken again with 5.0 ml of 2 vol% tri-n-octyl-amine-MIBK solution for 5 minutes. The two organic phases are combined and subjected to the atomic absorption spectrophotometry. The absorbances of Cd and Zn are measured, and the amounts of Cd and Zn are determined by referring to their calibration curves. (2) Determination of Cd and Zn in aluminum metal: 1.0 g of sample is decomposed with 20.0 ml of HCl (1+1), 7.0 ml of H2SO4 (1+1) and several ml of H2O2 (30%) {High purity aluminum metal is decomposed with 10.0 ml of NaOH solution (20%) and made acidic with 10.0 ml of H2SO4 (1+1) and 20.0 ml of HCl (1+1) }. It is transferred into a separatory funnel and made up to 50 ml with water, Cd and Zn are determined in accordance with above mentioned procedure (1). (3) Determination of Cd and Zn in uranium metal: 1.0 g of sample is decomposed with 12.0 ml of HCl (1+1), 3.0 ml of H2SO4 (1+1) and several ml of H2O2 (30%). It is transferred into a separatory funnel and made up to 50 ml with water. Cd and Zn are determined in accordance with above mentioned procedure (1) using 3 vol% solution in place of 2 vol% tri-n-octylamine-MIBK solution in the procedure (1).
社団法人日本分析化学会の論文

溶媒抽出-原子吸光法による銅,ニッケル,アルミニウムおよびウラン地金中の極微量カドミウムおよび亜鉛の定量

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