Measurement of difference in amplitude of components at about 51.75 degrees and 51.40 degrees 2theta (Co Kalpha radiation) of the asymmetric X-ray diffraction peak resulting from partial superposition of strong diffractions from corresponding planes in hexagonal and monoclinic pyrrhotite structures allows rapid quantitative determination of amounts and proportions of these structures in certain sulfide ores carrying at least 3 percent of either pyrrhotite type. The differences in amplitudes from synthetic mixtures of the pure structures are divided by amplitudes of a nearby diffraction peak from an internal standard added in constant proportion; resulting ratios are plotted against known proportions of either structure. The plot may be checked against weights of magnetic concentrates of monoclinic pyrrhotites from ores under study.

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