Determination of palladium,platinum and gold by energy dispersive X-ray fluorescence spectrometry with thin sample technology
WU Xu-ran1,2, HAN Xiao-feng1,2 , WANG Li1,2, L Jian-gang1,2XUE Guang2, TIAN Yu-hong1
1.College of Chemistry and Chemical Engineering, Yantai University, Yantai 264005,China; 2.Shandong Applied Research Centre of Gold Nanotechnology Au-SDARC,Yantai 264005, China
Abstract：Palladium, platinum and gold in gold ore and copper anode slime were separated and enriched by resin. Combining with thin sample technique, these three elements were simultaneously determined using self-made X-ray fluorescence energy spectrometer. Three types of resin were tested and Amberlyst A26 resin was finally selected for the separation. The column height of Amberlyst A26 resin, flow rate and concentration of hydrochloric acid were optimized by single factor method. The optimal experimental conditions were as follows: column height of 10 cm, flow rate of 3 mL/min and hydrochloric acid concentration of 0.2 mol/L. Meanwhile, the methodology validation of X-ray fluorescence spectrometry was performed. The energy dispersive X-ray fluorescence spectrometer used Mo excitation target and novel SDD detector. The matrix effect could be basically eliminated combining with optimized thin sample technique. The quantitative analysis could be realized by internal standard method. The lower limit of detection (LLD) of instrument was 0.021, 0.019 and 0.015 μg/mL for Pd, Pt and Au, respectively. The limit of detection of method (LDM) was 0.066, 0.062 and 0.050 μg/mL, respectively. The relative standard deviations (RSD) of mixed standard of 11 elements were between 1.6% and 7.5%. The determination results of gold ore samples were consistent with those obtained by national method,and the determination results of copper anode slime were consistent with those obtained by ICP-MS.
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