Analysis of Noble Metals. Overview and Selected Methods by F. E. Beamish
By F. E. Beamish
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Sample text
The solutions were evaporated to dryness and the residue collected in a sodium chloride matrix, which was analyzed qualitatively by spectrograph. They suggested that this procedure could be made quantitative. Miyamoto (83), in 1961, used a gold-silver alloy bead from fire assaying for the spectrographic determination of platinum and palladium in ores. Ginzburg (84), in 1963, divided methods for spectrographic analyses of platinum metals into the following two groups: (1) direct determination and (2) the composite method in which use is made of preliminary enrichment of initial samples and separation of the elements to be determined as concentrate in a collecting metal.
Heat over a Meker burner until the melt appears clean and shiny; the platinum metals will appear as floating specks until they have dissolved c o m pletely. A l l o w the melt to cool to room temperature under hydrogen. A s s i g n a small triangular file to each standard; keep each file in a properly labeled, clean, container. File each master standard to obtain a sufficient amount of filings for dilution. (b) The preparation of working standards. Each of the constant gold standards con tains 5% of g o l d , platinum, palladium, rhodium, and silver in concentrations suitable for establishing spectrographic curves and contains lead to make 100%.
Results in grams per metric ton can be readily obtained by calculation but more easily by selecting a convenient metric sample w e i g h t . ) It may be necessary to assay larger samples of rocks or to c o m b i n e the lead fusion buttons from several assays to obtain an adequate concentration for detection. For the conventional fire assay (see Chapter 6, Procedure 121), add 5 m g of gold or 10 mg of silver as a collector, depending on whether a gold or silver bead is desired. W e i g h the assay bead, w h e n ready, in a graphite crucible with sufficient lead to provide either a 5% g o l d - 9 5 % lead alloy or a 10% s i l v e r - 9 0 % lead alloy.