Lutetium oxide analysis by direct arc atomic emission spectrometry

The requirements for the composition of initial oxides for the lutetium orthosilicate crystals are quite stringent: the content of the basic substance Lu2O3 is 99.999 wt%. Critical are coloring impurities: Fe, Ni, Cr, Co, Cu, V, Mn, the content of each should be no more than 0.0005 - 0.0010 wt%, Pr, Nd, Sm, Er, Tb, Yb no more than 0.0005 wt% for each one. It is also necessary to control the content of Al, As, Bi, Cd, Mg, Mo, Pb, Sb, Si, Sn, Ti, Zn, Y, La, Ce, Sc, Eu, Gd, Dy, Ho, Tm. To determine the impurity composition of lutetium oxide, one of the promising methods of analysis is direct arc atomic emission spectroscopy (DC Arc). The advantages of this method are the determination of the chemical composition without sample dissolution, a wide range of concentrations (10-6 - 10-1% wt%), a large number of determined elements. To realize the potential analytical capabilities of the method, the experimental conditions were studied: the interelectrode distance, the shape and size of graphite electrodes, the ratio of Lu2O3 to the spectral buffer, the type of carriers and operating modes of the generator. For most elements, the limits of determination are n ∙ 10-6 - n ∙ 10-4 wt%, that is significantly lower than in the current methods of DC Arc. The trueness of results is controlled by ICP-MS. The complex application of new approaches and modern capabilities of spectral equipment made it possible to develop a method with improved metrological characteristics.