Determination of palladium in nuclear-waste samples by inductively coupled plasma emission-fluorescence spectrometry
Determination of palladium in nuclear-waste samples by inductively coupled plasma emission-fluorescence spectrometry
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电感耦合等离子体发射荧光光谱法测定核废料样品中的钯
DOI：
10.1039/an9830800297
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发表时间：
1983
期刊：
影响因子：
--
通讯作者：
N. Omenetto
中科院分区：
文献类型：
--
作者：
P. Cavalli;G. Rossi;N. Omenetto
用0.5 m单色器电感耦合等离子体（ICP）发射光谱法测定核废料样品溶液中的钯，在钯的所有分析有用波长上都存在严重的光谱干扰。钯谱线在363.47、324.27、340.45和360.95 nm处受到了氩、钇、锆、钐和钕谱线的干扰。为了克服这些干扰，需要一台高分辨率的光谱仪。这就排除了多通道光谱仪的使用，表明了高分辨率扫描单色仪的应用。在本文中，我们提出了一种简单而有效的替代方法，将ICP发射特性与原子荧光光谱的光谱选择性相结合。在氩气屏蔽空气-乙炔火焰中雾化的样品在363.47 nm处测量钯原子荧光，通过将纯净的5000 μ g ml-1的钯溶液送入ICP火炬激发，可以精确和准确地测定钯，没有散射问题。此外，样品中的钯浓度使得ICP -共振单色仪技术可以在没有样品稀释的情况下快速有效地使用，只要有足够的样品，并且放射性处于可容忍的水平。
The determination of palladium in sample solutions of nuclear waste by inductively coupled plasma (ICP) optical emission spectrometry with a 0.5-m monochromator is hindered by severe spectral interference that occurs at all the analytically useful wavelengths of palladium. Interferences from argon, yttrium, zirconium, samarium and neodymium lines have been experienced with the palladium lines at 363.47, 324.27, 340.45 and 360.95 nm. In order to overcome these interferences a spectrometer of high resolution is required. This precludes the use of a multi-channel spectrometer and indicates the application of a high-resolution scanning monochromator. In this paper we show that a simple and effective alternative approach to the problem is offered by combination of the ICP emission characteristics with the spectral selectivity of atomic-fluorescence spectrometry. Measurement of the palladium atomic fluorescence at 363.47 nm from a sample atomised in an argonshielded air - acetylene flame, excited by the emission of a pure 5000 µg ml–1 solution of palladium fed into the ICP torch, allows for the precise and accurate determination of palladium, with no problems due to scattering. In addition, the palladium concentration in the samples is such that the ICP - resonance monochromator technique could be quickly and effectively used with no sample dilution, provided that sufficient sample is available and that radioactivity is at a tolerable level.