Spectrochemical Analysis of Palladium by the Sponge Technique

"AbstractA technique is described for preparation of palladium sponge and for spectrochemical analysis of the metal in this form. The precision and accuracy of the method are discussed. Analyses are compared with previous spectrochemical analyses of palladium in the black form. Good agreement was found in the two sets •of results and it is concluded that they are more reliable than wet chemical .analyses of the same material.IntroductionFOR SEVERAL YEARS the problem of platinum metal analysis by spectrochemical methods has been under investigation at the Spedtrographic Laboratory, Department of Geological Sciences, Queen's University. The problem, briefly -stated, is as follows: Samples of platinum, palladium,-rhodium, ruthenium, and iridium are received as fine metal powders, called sponge. Direct spectrographic analysis of this material has not been found satisfactory due to its heterogeneity •as regards contaminant metals, which may be present up to a total of one per •cent or more. Further-more, spectrographic standards are difficult to obtain and difficult to prepare accurately by adding weighed portions of contaminant metals to the sponge. The fact that •contaminant metals in original samples are probably alloyed with the major constituent is a further difficulty since complete fusion of these refractory metals proved impractical in the present case as a means of standard preparation. It •has, therefore, been found most satisfactory to dissolve the metals, prepare standards by addition of solutions of contaminant metals, and to reduce both standards and samples to a homogeneous form. A previous paper, by Hawley, Wark, Lewis and Ott (2) dealt with a method for spectrochemical analysis of platinum and palladium in their black form. Since completion of research on the black technique, the possibility of analyzing palladium accurately in its sponge form has• been investigated."