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采用吡咯二硫代氨基甲酸铵(APDC)沉淀富集高纯氧化镥中痕量的铁,再将沉淀溶于甲基异丁基酮(MIBK)溶液中,分离富集后的溶液用石墨原子吸收法直接测定.当盐酸酸度控制在0.4 mol/L,加2%APDC溶液2 m L,沉淀放置时间为15 min,选取石墨炉原子吸收光谱仪的灰化温度1 100℃,原子化温度2 300℃时,铁的测定效果最佳.铅、镍、铬、钴、铜等基体元素对铁的测定基本无干扰.该方法具有较好的精密度和准确度,相对标准偏差为4.5%,加标回收率在94.0%~108.0%之间.
Ammonium pyrithiocarbamate (APDC) was used for the precipitation of trace amounts of iron in high-purity lutetium oxide. The precipitate was dissolved in a solution of methyl isobutyl ketone (MIBK). The separated solution was separated with graphite atoms Absorption method directly measured when the acidity of hydrochloric acid control 0.4 mol / L, plus 2% APDC solution 2 m L, the precipitation time is 15 min, selected graphite furnace atomic absorption spectrometry ashing temperature of 1 100 ℃, atomization temperature 2 300 ℃, the determination of iron is the best.The lead, nickel, chromium, cobalt, copper and other matrix elements have almost no interference with the determination of iron.The method has good precision and accuracy, the relative standard deviation of 4.5%, plus The standard recoveries ranged from 94.0% to 108.0%.