沈殿分離濃縮法による銅及び銀地金中の微量ビスマスのけい光X線分析

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Bismuth (<100μg) was coprecipitated with iron(III) hydroxide (100μg as iron) from 20 to 500 ml of aqueous solutions in the pH range of 8-11. As the X-ray intensity of bismuth decreased gradually with aging of the precipitate, filtration should be made immediately after precipitation. A linear calibration curve was obtained over (1〜100) μg of bismuth. The coefficient of variation was 1.8% with 10μg of bismuth in five runs. Sensitivity was 20 (counts/s) / μg Bi. The following amounts of foreign ions were tolerated in the determination of 100 μg of bismuth: Zn and Cd I g, Ni 250mg. Co 25 mg. Se(IV) 2 mg, Mn(II) and Sn(IV) 200μg, As(III) 100μg, P(V) and Cr(III) 50μg, Pb(II) 25μg. The procedure is as follows: Dissolve 2 g of copper or silver in 20 ml of 6.5 M nitric acid. Add 100μg of iron(III), adjust pH to 9-10 with aqueous ammonia, and collect the precipitate on a membrane filter (25 mm, 0.3μm). Wash the precipitate with a dilute solution of ammonia (pH 9). Measure the intensity of BiLa line (2e=33.0°) and that of background (26=32.6°), respectively, in a vacuum for 40s by using a molybdenum-target tube (50 kV, 20 mA), a LiF(200) crystal and a scintillation counter.
社団法人日本分析化学会の論文
1980-01-05