The technique of microwave digestion was evaluated as a possible alternative to conventional sample preparation methods for the platinum ores prior to spectroscopic analysis. Microwave energy used with aqua regia in closed vessel provides elevated pressure and rapid heating which significantly reduce digestion time. All analyses were carried out by inductively coupled plasma atomic-emission spectroscopy (ICP-AES). To reduce matrix interferences during analysis, a predigestion step with 50 mL of 1:1 nitric acid was introduced. Both ICP-AES and inductively plasma mass spectroscopy (ICP-MS) were used for analysis of sample extracts. ICP-AES analyses showed improved recoveries of Pd (60-80%) and Pt (30-60%) in only two reference materials SARM7 and NBM-6b. ICP-MS analyses of the reference materials indicate that most PGE recoveries were 85-102%. Os and Au were less efficiently recovered. Relative percent difference in the determination of the more efficiently recovered elements ranged between 1-12%. Additionally PGE extraction with 10% KCN solution was investigated. Sample extracts were analyzed by ICP-MS. Analyses of the cyanide extracts showed similar PGE recoveries to aqua regia digestion for Ir, Pd, Ru, and Rh. Platinum, osmium and gold recoveries were less efficient. (Abstract shortened by UMI.)
