Development and application of new iondashexchange techniques for the separation of the platinum group and other siderophile elements from geological samples

Talanta. 1997 Apr;44(4):663-72. doi: 10.1016/s0039-9140(96)02100-5.

Abstract

Two new aniondashexchange techniques have been developed for the separation of the platinum group elements Ru, Pd, Ir, Pt and the siderophile metals Re, Ag, Zn and Cd from geological samples following a NiS fire assay digestion procedure. Both methods are simple and permit the isolation of these elements in sufficient purity for quantitative analysis by isotope dilutiondashinductively coupled plasma mass spectrometry (ID-ICPMS) at yields of 75-95%. The high affinity of the considered elements to anion exchange resins allows the use of small (1.25 ml) columns even for the processing of 5-10 g sized silicate rock samples. Following fire assay digestion and dissolution of the NiS buttons in aqua regia, the samples are loaded onto the resin bed as solutions in 1 M HCl. After elution of the bulk sample matrix with dilute HCl and HNO(3), Zn and Cd are stripped from the column using 0.8 M HNO(3). Small amounts of bromine water are added to the dilute mineral acids for the stabilization of strongly retained Ir(IV). Following this, the iondashexchange techniques permit the sequential elution of Ag, Re and the PGE using 11 M HCl, 8 M HNO(3) and 13.5 M HNO(3). The iondashexchange methods have been applied to separation of Ru, Pd, Re, Ir and Pt from the geological reference material SU-la prior to concentration measurements by ID-ICPMS. Our analytical results are in good agreement with previously published data for this sample and display an external reproducibility (based upon repeat dissolutions) of approximately 2-10% for the elements considered in this study.