This work details, on a laboratory scale, a method to prepare small solid ingot calibration standards of palladium and platinum for use in solid sampling instrumentation such as arc/spark OES, spark ablation OES and GD-MS. Standards were prepared by first precipitating and co-precipitating spiked solutions of palladium and platinum along with the desired analytes then melting the stock powder with a bulk amount of 99.999% pure metal to attempt to achieve a final concentration in the metal of (5~10) ×10-6 for 33 elements. Losses occurred in both the precipitation step and the thermal step with a final of 25 elements for Pd being quantitatively incorporated into the final ingot and 26 elements in Pt. Several contamination issues arose with Au, B, Fe, and Si. |