感耦等离子体发射光谱法测定高纯氧化钇中的痕量稀土元素

本文采用国产WPG-100型一米光栅摄谱仪、GP3.5-D1型高频等离子体发生器、气动雾化器,以不去溶方式进样直接测定纯度为99.995%的氧化钇中十四个稀土杂质元素。其中除镨(17μg/g)和钸(7μg/g)外,测定下限均为0.3-3μg/g(以氧化物计)。当被测元素的含量为3-17μg/g时,相对标准偏差为2.3-7.3%(钸和镨除外)。样品用盐酸溶解,酸度和共存元素的影响很小,方法简便、快速。

APPLICATION OF AN INDUCTIVELY COUPLED PLASMA TO THE EMISSION SPECTROSCOPIC DETERMINATION OF TRACE RARE EARTHS IN HIGH PURITY YTTRIUM OXIDE

Inductively coupled plasma (ICP) source was applied success fully to the direct spectrographic determination of trace amounts of 14 rare earth elements in high purity Y₂O₃.A simple method was suggested to study the effect of the matrix concentrations on detection limits.Spectrographic conditions were as follows: Chinese Ebert type spectro-graph (WPG-100), linear dispersion 3.6 Å/mm (second order); Chinese radio frequency generator (GP3.5-D1), frequency 33 MHz, anode voltage 3.5 kV, anode current 0.9 A, grid current 0.22 A; Scott-Fassel type plasma torch, pneumatic concentric nebulizer, carrier gas Ar 0.77 1/min, plasma gas Ar 0.5 1/min, coolant gas Ar 14 1/min, observation height 15-16mm. Samples were dissolved simply in HC1 (6N) and diluted before determination.The lower limits of the determination were 0.3-3μg/g (as oxides) for the rare earth impurities, except 7μg/g for CeO₃ and 17μg/g for Pr₆O₁₁ Yttrium oxide with 99.995% purity could be analysed. The relative standard deviations were 2.3-7.3%, when the concentrations of rare earth oxides (except Pr₆O₁₁ and CeO₂) were 3-17μg/g. Effects of rare earths and 13 non-rare earths (Ca, Mg, Al, Fe, Na etc.) impurities on results of determination might be often neglected.