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间硝基偶氮氯膦在酸性溶液中与稀土离子形成蓝或绿色的络合物。当草酸存在下,可掩蔽钇组稀土而测定铈组稀土。本文试验了测定条件并试用于测定铁基、镍基合金中微量铈组稀土元素。在实验条件下,在与试样相应的铁、镍、镍铬含量存在下,铈的摩尔吸光系数依次为8. 7×10~4、8. 6×10~4及9. 3×10~4升·摩尔~(-1) ·厘米~(-1) ;Sandell 灵敏度依次为0. 0016、 0. 0016及0. 0015微克、铈(Ⅲ)/厘米~2;比耳定律范围依次为0～12、 0～10及0～10微克铈(Ⅲ)/25毫升,五倍钇存在时不干扰。对铁基合金中含铈量为0. 025%、镍硅合金中含铈量为0. 022%、镍铬合金中含铈量为0. 021%分别作10次平行测定时,其标准偏差依次为0. 0036、 0. 0017及0. 0011;变异系数依次为1. 7%、0. 74%及0. 46%。铈的回收率为96～105%。用本法测定铁基、镍基合金中微量铈组稀土元素,可获得满意结果。
Nitrochlorophosphoramidite forms a blue or green complex with rare earth ions in an acidic solution. In the presence of oxalic acid, rare earths in the cerium group can be masked by the rare earths of the yttrium group. In this paper, the test conditions were tested and used to determine the trace cerium rare earth elements in iron-based and nickel-based alloys. Under the experimental conditions, the molar extinction coefficients of cerium in the presence of iron, nickel, and nickel-chromium corresponding to the samples are, in order, 8. 7 × 10 -4, 8.6 × 10 -4 and 9.3 × 10 -3, 4 liters · mol -1 (cm -1); Sandell sensitivity was 0. 0016, 0.0016 and 0. 0015 μg, cerium (Ⅲ) / cm 2, and Beer’s law range was 0 ~ 12, 0 ~ 10 and 0 ~ 10 micrograms cerium (III) / 25 ml, five times the existence of yttrium does not interfere. The iron-based alloy containing cerium 0. 025%, nickel-silicon alloy containing 0. 022% of cerium, nickel-chromium alloy containing cerium was 0. 021% for 10 parallel determination, the standard deviation Followed by 0. 0036, 0. 0017 and 0. 0011; coefficient of variation were 1.7%, 0.74% and 0.46%. The recovery of cerium is 96 to 105%. By this method for the determination of rare earth elements in the cerium group of iron-based and nickel-based alloys, satisfactory results can be obtained.