Tests are described showing the results obtained for the determination of REE and the trace elements Rb, Y, Zr, Nb, Cs, Ba, Hf, Ta, Pb, Th and U with ICP‐MS methodology for nine basaltic reference materials, and thirteen basalts and amphibolites from the mafic‐ultramafic Niquelândia Complex, central Brazil. Sample decomposition for the reference materials was performed by microwave oven digestion (HF and HNO3, 100 mg of sample), and that for the Niquelândia samples also by Parr bomb treatment (5 days at 200°C, 40 mg of sample). Results for the reference materials were similar to published values, thus showing that the microwave technique can be used with confidence for basaltic rocks. No fluoride precipitates were observed in the microwave‐digested solutions. Total recovery of elements, including Zr and Hf, was obtained for the Niquelândia samples, with the exception of an amphibolite. For this latter sample, the Parr method achieved a total digestion, but not so the microwave decomposition; losses, however, were observed only for Zr and Hf, indicating difficulty in dissolving Zr‐bearing minerals by microwave acid attack.

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Determinations of the volatile elements carbon, hydrogen, sulfur and nitrogen in many geological RM, performed with the LECO CHN and SC analysers, are presented. The method allowed the determination of S in concentrations from a few % m/m to 0.001% m/m or less, of C from % m/m to 0.01% m/m and of H from % m/m to 0.004% m/m. Accuracy was usually better than the XRF method (for S). All obtained values passed the Sutarno‐Steger test, which establishes that |(meananalysed ‐ meancertified)|/ Scertified < 2, for the cases with an appropriate number of determinations (n > 10 for each element). It was possible to perform routine determination of C, H and S with the instrumentation, coupled with the determination of major and minor elements in geological materials. Determination of nitrogen could also be performed on an exploratory basis, with improvements in the method dependent on the future availability of more reference materials with reliable composition of this element.

The complete dissolution of representative test portions of powdered rock samples for the determination of the mass fractions of trace elements by ICP-MS relies either on aggressive and time-consuming acid digestions or fusion/sintering with appropriate fluxes. Here, we evaluate a microwave oven dissolution method that employs a solution of NH 4 HF 2 and HNO 3 . The entire procedure occurs in a closed vessel system and takes up to 4 h. In hundreds of digestions, the precipitation of fluorides was never observed. Replicate decomposition of 100 mg of twenty-one international reference materials (RMs) of igneous rocks, and also one of a shale presented mostly satisfactory recoveries of forty-one trace elements. Important exceptions were Zr and Hf in G-2 and GSP-2 (mean recoveries of ca. 70%), although for four other felsic rock RMs, the digestion was complete. For ultramafic rock RMs, we present Cr results that indicate quantitative dissolution of Cr-bearing phases. We discuss the findings and conclude that advances in sample preparation of geological materials for instrumental analysis would benefit from a better understanding of how specific characteristics, such as composition and crystallinity of certain minerals, may affect their reactivity.

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