Calibration of an Energy Dispersive X-Ray Fluorescence Spectrometer

Abstract

The purpose of this work was to develop accurate calibration standards which were fully characterized in terms of uniformity and concentration using fundamental measuring methods. Three similar sets of vacuum deposits were commercially made, each set containing the single deposits CuS, KCl, CaF2, Cr, Fe, Cu, RbNO3, SrF2, MoO3 , BaF2, and Pb. Thickness variations in each deposit were measured with PIXEA (proton induced x-ray excitation analysis) measurements taken at 6 to 8 positions along the deposit diameters. Relative elemental concentrations on corresponding deposits from each set were measured using multiple XRF intercomparisons. One set of deposits was destructively analyzed at the National Bureau of Standards with isotope dilution thermal ionization mass spectrometry (IDMS) in order to calibrate the remaining sets of vacuum deposits. The calibrated deposits were compared with standards from two commercial sources. For seven elements heavier than chlorine there was an average deviation of 13.5% between the calibrated deposits and the commercial standards. Disagreements as large as 15% were observed between standards from the two commercial suppliers.