An inter-laboratory comparison of EPMA analysis of alloy steel at low voltage

We present the results of an inter-laboratory comparison of EPMA analysis at low voltage (5-6 kV) of three monophasic alloy steel samples. The aim of the work was to obtain an estimate of the present situation of low-voltage analysis of steel and identify needs for improvement. EPMA analyses of the samples were conducted by seven participant groups using electron microprobes and scanning electron microscopes of different kind, equipped with wavelength- and/or energy-dispersive X-ray spectrometers, and employing their own methodology of analysis. The results using WDS showed essentially an underestimation of the Cr contents, with relative deviations from the reference values ranging from -0.7 % to -17 %, and an overestimation of Fe and Ni, with relative deviations from the reference composition ranging from -4 % to +30 %, and from +14 % to +42 %, respectively. The relative deviations obtained by using EDS showed larger scatter, ranging from -16 % to +54 % for Cr, -0.4 % to +66 % for Fe and from +13 % to +90 % for Ni. Reasons for the differences observed and the scatter of results are discussed.