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本文系统地研完了大量NaCl基体存在下稀土元素和钪在该体系中的分离富集及ICP光谱测定条件。对盐酸的浓度和用量,静止时间及盐酸—乙醇混合比等因素的影响进行了研究,对ICP放电参数,NaCl残留量及酸度的影响进行了最佳选择。在实验条件下,测定15个稀土元素和Sc的检出限为0.87~570ppb(ng/ml);测定的相对标准偏差为0.50~3.8%(c=5ug/ml,n=10)平均回收率为84~95%。结果表明:本方法具有灵敏、准确、快速和操作简便等优点,可用于以NaCl为基体的试样中痕量稀土杂质的测定。
In this paper, we systematically studied the separation and enrichment of rare earth elements and scandium in this system in the presence of a large amount of NaCl and the determination conditions of ICP spectroscopy. The effects of hydrochloric acid concentration and amount, resting time and hydrochloric acid - ethanol mixture ratio were studied. The best choice of ICP discharge parameters, NaCl residual amount and acidity were studied. Under the experimental conditions, the detection limits of 15 rare earth elements and Sc were 0.87 ~ 570ppb (ng / ml); the relative standard deviations were 0.50 ~ 3.8% (c = 5ug / ml, n = 10) For 84 ~ 95%. The results show that this method is sensitive, accurate, rapid and easy to operate. It can be used for the determination of trace rare earth impurities in NaCl-based samples.