模拟高放废液玻璃固化体溶解液的ICP/AES分析法

ANALYSIS OF SIMULATED WASTE VITRIFICATION GLASS SPECIMENS BY ICP/AES

利用我院制造的高浓盐雾化器解决了送样过程中同心雾化器堵塞的问题,并且详细观察了存在于溶解液中诸元素,尤其是具有复杂光谱结构的元素之间的谱线干扰现象。我们注意到硫的最灵敏的主共振线S 180.73nm为Ca线所干扰,为此,采用次灵敏的S 1820.4nm谱线;还观察到铀和钛对Li323.26nm和Na330.24nm的谱线干扰。改变等离子体的工作参数,即增加载气流,减小高频功率,可提高被测元素Li,Na的谱线强度,同时降低干扰元素的谱线强度,从而可以在U,Ti共存的溶液中测定Li和Na。本法可测定玻璃模拟体中主次成分,共十九个元素:B,Si,Na,Li,Al,Ca,Mg,Sr,Zr,Ti,Ce,La,Nd,Fe,Cr,Mn,Ni,S,U。方法的相对标准偏差随元素不同约为1%～5%。

For determination of the element contents in simulated waste vitrification glassspecimens being dissolved by LiBO_2 fusion method or sealed acid dissolution me-thod the following problems have been solved: 1. The nebulizer made in our institute specially designed for the analysis ofhigh solid content solution has been used in our work to eliminate the nebulizerblokage caused by large content of H_3BO_3 or LiBO_2 in sample solution. 2. The spectral interference has been checked. We noticed that a calcium linecoincides with the main resonance line of sulfur S 180.73 nm, also uranium andtitanium line wings interfere Li 323.26 nm and Na 330.23 nm. By changing ofoperating parameters of plasma discharge, i. e. increasing carrier gas flow rate anddecreasing RF power the line intensities of Li 323.26 nm and Na 330.23 nm canbe enchanced, at the same time the line intensities of interfering elements (U, Ti)are weakend. 19 elements (Si B, Na, Li, Ca, Mg, Al, Ti, Zr, Mn, Sr, Cr Ni, Fe,La, Nd, Ce, S, U) in glass solidifier have been determined. The RSD is rangingfrom 1%--5%.