Trace analysis of high-purity copper by total reflection X-ray fluorescence spectrometry

Total reflection X-ray fluorescence (TXRF) analysis after the separation of matrix element was studied for the determination of trace impurity elements (Ca, Sc, V, Cr, Mn, Fe, Co, Ni and Zn) in high purity copper. Matrix copper was removed by electrolysis (0.2 A, 8 h) of a nitric acid solution. A 10 mu L aliquot of the remaining solution of the electrolysis was dropped on a silicon-wafer sample-carrier and dried in a vacuum. This was repeated five times and the precipitate of five 10 mu L-aliquots was analyzed by TXRF using a W-L beta beam with an incident angle of 0.05 degrees. TXRF analytical values were obtained by using relative sensitivity factors of the analytes to the internal standard element (Pd). Detection limits of the analytes ranges from 0.077 ng for Zn to 0.785 ng for Ca.