溶媒抽出-発光分光分析法による酸化セリウム中の微量非希土類元素の定量
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概要
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An emission-spectrographic method is described for the quantitative determination of traces of non-rare earth elements separated from cerium dioxide by means of solvent extraction.<BR>A 1.0 g sample of cerium dioxide is dissolved in a mixture of 5 m<I>l</I> of concentrated nitric acid and 5 m<I>l</I> of 30% hydrogen peroxide by heating on a water bath. The solution is evaporated to dryness. The residue is dissolved in 50 m<I>l</I> of 9<I>N</I> nitric acid containing 0.20 g of sodium bromate. The solution is extracted twice with 50 m<I>l</I> portions of tri-<I>n</I>-butyl phosphate. The aqueous layer is mixed with 0.10 g graphite powder, evaporated to dryness and finally heated at 500°C. To the residue thus obtained is added 10 ppm of gallium as an internal standard, and the whole is made up to 0.50 g by graphite powder. A weighed portion of this is placed on the sample electrode and packed lightly with a venting tool, and is discharged by d. c. arc.<BR>Spectrographic conditions were as follow : 3.4 m Ebert grating spectrometer GEM-340; excitation voltage 220 V; arc current 15 A; analytical gap 2 mm; exposure time 20 sec without prc-burn; and anode charge 30 mg.<BR>Recovery of impurity elements in the proposed analytical procedure was : 130% for Al and Mg; 90110% for Ag, Ca, Co, Cu, Mn, Ni, Pb and Sn; 5085% for Bi, Fe and Ti. Analytical values of impurities in the sample were corrected by the correction factor obtained from the recovery.<BR>The proposed method enables the determination of microquantities of 13 impurity elements in cerium dioxide down to 0.2<SUB>5</SUB> ppm for Mg and Mn; 0.5 ppm for Ag, Bi and Cu; 2.5 ppm for Al, Ca, Fe, Ni, Pb and Sn; 5.0 ppm for Co; 12.5 ppm for Ti. Coefficients of variation are less than 15%.
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