Interference Corrections During EDXRF Determination of Molybdenum and Sulphur in Powder Samples

ABSTRACT Complete elemental characterization of Molybdenum sulfide, an electro‐catalyst for hydrogen evolution reactions, is essential without much compromise on the material integrity. Energy dispersive x‐ray fluorescence (EDXRF) spectrometry can non‐destructively determine the chemical composition. Mo and S were determined by EDXRF, after addressing the matrix interferences. The interferences due to attenuation of characteristic low energy x‐rays of S by the Mo‐matrix and overlap of S and Mo characteristic x‐rays, lead to rotational and translational matrix effects. These effects on calibration curves were corrected by adopting multiple standard additions, along with matrix correction factors. Herein, the pragmatic inferences, obtained via optimization of experimental variables, were combined with a theoretically calculated correction factor, to solve the extreme spectral overlap problem, during S determinations in the presence of Mo. The results were validated using QC standards and the methodology was applied for real sample analyses. Accuracies better than ±5% were achieved.