Standardless energy-dispersive X-ray fluorescence analysis using primary radiation monochromatized with LiF(200) crystal

Energy-dispersive X-ray fluorescence spectrometer (EDXRF) with primary radiation monochromatized by LiF(200) crystal was developed. In the constructed spectrometer, the radiation from the Ag target X-ray tube operated at 50 kV and 40 mA excites the secondary target (Cu, Se, Zr or Mo). The characteristic radiation (Cu Kα, Se Kα, Zr Kα or Mo Kα) of the target is monochromatized with LiF(200) crystal and excites elements in the analyzed sample. The X-ray spectra are collected by thermoelectrically cooled Si-PIN detector with resolution of 145 eV at 5.9 keV. The pinhole collimator placed in front of the X-ray detector allows reducing size of the analyzed area. Quantitative analysis is performed using standardless fundamental parameters (FP) method. Because sample is excited using highly monochromatized radiation, the calculations are much simpler and analysis error resulting from uncertainty of X-ray tube spectral distribution is completely eliminated. Moreover, EDXRF system allows obtaining very low background and appropriate secondary target can be selected for the best excitation of the determined elements and to avoid overlapping of the analyte peaks with characteristic radiation originating from the secondary target. The FP calculations were verified using several certified reference materials of stainless steel. The spectrometer was used for nondestructive analysis of mono- and polycrystals of selenide spinels of general formula MxNyCrzSe4 (where M, N are Cu2+, Zn2+, Cd2+, Mn2+, Ge2+, Ni2+, V3+, Sb3+, Ga3+). The results from EDXRF were compared with those obtained by means of the wavelength-dispersive X-ray fluorescence spectrometry (WDXRF).