The identification and accurate characterization of discrete grains of rare minerals in sulfide base-metal ores is usually a cumbersome procedure due to the small grain sizes (typically <10 μm) and complex mineral assemblages in the material. In this article, a new strategy for finding and identifying indium minerals, and quantifying their composition and abundance is presented, making use of mineral liberation analysis (MLA) and electron probe microanalysis (EPMA). The method was successfully applied to polymetallic massive sulfide ores from the Neves-Corvo deposit in Portugal. The presence of roquesite and sakuraiite could be systematically detected, their concentration quantified by MLA measurements, and their identity later confirmed by EPMA analyses. Based on these results, an almost complete indium deportment could be obtained for the studied samples. This validates the approach taken, combining automated mineralogy data with electron microprobe analysis. A similar approach could be used to find minerals of other common minor and trace elements in complex base-metal sulfide ores, for example Se, Ge, Sb, or Ag, thus permitting the targeted development of resource technologies suitable for by-product recovery.

Accurate quantification of the chemical composition of eudialyte group minerals (EGM) with the electron probe microanalyzer is complicated by both mineralogical and X-ray-specific challenges. These include structural and chemical variability, mutual interferences of X-ray lines, in particular of the rare earth elements, diffusive volatility of light anions and cations, and instability of EGM under the electron beam. A novel analytical approach has been developed to overcome these analytical challenges. The effect of diffusive volatility and beam damage is shown to be minimal when a square of 20×20 µm is scanned with a beam diameter of 6 µm at the fastest possible speed, while measuring elements critical to electron beam exposure early in the measurement sequence. Appropriate reference materials are selected for calibration considering their volatile content and composition, and supplementary offline overlap correction is performed using individual calibration factors. Preliminary results indicate good agreement with data from laser ablation inductively coupled plasma mass spectrometry demonstrating that a quantitative mineral chemical analysis of EGM by electron probe microanalysis is possible once all the parameters mentioned above are accounted for.

Identification and accurate characterization of platinum-group minerals (PGMs) is usually a very cumbersome procedure due to their small grain size (typically below 10 µm) and inconspicuous appearance under reflected light. A novel strategy for finding PGMs and quantifying their composition was developed. It combines a mineral liberation analyzer (MLA), a point logging system, and electron probe microanalysis (EPMA).

As a first step, the PGMs are identified using the MLA. Grains identified as PGMs are then marked and coordinates recorded and transferred to the EPMA. Case studies illustrate that the combination of MLA, point logging, and EPMA results in the identification of a significantly higher number of PGM grains than reflected light microscopy. Analysis of PGMs by EPMA requires considerable effort due to the often significant overlaps between the X-ray spectra of almost all platinum-group and associated elements. X-ray lines suitable for quantitative analysis need to be carefully selected. As peak overlaps cannot be avoided completely, an offline overlap correction based on weight proportions has been developed. Results obtained with the procedure proposed in this study attain acceptable totals and atomic proportions, indicating that the applied corrections are appropriate.