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Determination of Palladium, Platinum and Gold by X-ray Fluorescence Spectrometry with Resin Separation

Author: HanXiaoFeng
Tutor: ZuoXuRan
School: Yantai University
Course: Analytical Chemistry
Keywords: Dowex1-X10resin D301R resin Amberlyst A26resin 717resin high grade nickel matte gold deposit copper anode slime TXRF XRF
CLC: O658
Type: Master's thesis
Year: 2013
Downloads: 44
Quote: 0
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Abstract


Resin separation technique has the advantages of high separating efficiency, less environmental pollution, easy operation, and recyclable. Resin separation technique applied to separation concentration of elements that is an effectively separation and enrichment method. At present, the kind of the resins is getting more and more, its application is wider and wider.The Partial new resins that have good selectivity, high adsorption efficacy and good performance begins to be commercialization. Resin has been called green extraction technology which has attracted much attention of domestic and international researchers.The method of XRF has advantages in determination, low detection limit, good quantitative characters, quick inspection, simple operation, low operation cost, non-destructive testing. This experiment on the basis of resin separation and the study of XRF,used the commercial TXRF and ICP-MS as comparison, developed a new method that can do separation and concentration of palladium, platinum and gold effectively. And then puts forward some basic ideas andpolicy suggestions on initial determination of Pd,Pt,Au in gold mine tailings.This paper mainly includes four parts.The first part briefly introduced the topic selection background, experimental samples and determination of the instrument. As well as the research meaning and content of our re search group.In the second part, the research examines the sensitivity calibration curve, detection limit, and precision of XRF developed by our research group. The sensitivity calibration curve of an element of the deviation is less than2%. The detection limit of the XRF method were0.025μg/mL(Pd),0.022μg/mL (Pt) and0.018μg/mL (Au). The quantification limit of the XRF method were0.083μg/g (Pd),0.073μg/g (Pt) and0.060μg/g (Au). Continuous sample preparation on the preparation of standard solution determination of10times, the relative standard deviations (RSD s) of the the elements between1.6%and7.5%. Results proved that homemade XRF instrument has good detection performance The reaction conditions were studied and optimized, the optimized conditions were determined: column height10cm, flow rate1-5mL/min, concentration of HC10.2moL/LThe third part:In high grade nickel matte, Dowexl-X10anion exchange resin has selective adsorption for Pd, Pt and Au. A new method based on this theory and TXRF technology has been developed. The column of Dowexl-X10was prepared. The solution for the selective adsorption for Pd, Pt and Au of Dowexl-X10was selected. Underthe optimized conditions, The relative standard deviations (RSD s) of the determination method were less than5.7%. The detection limit of the TXRF methodwere0.020μg/mL(Pd),0.014μg/mL (Pt) and0.016μg/mL (Au). The quantification limit of the TXRF method were0.067μg/g (Pd)、0.047μg/g (Pt) and0.052μg/g (Au). And the average recoveries of standard addition were90.9%-100.6%, which was in agreement with the results of ICP-MS. TXRF is a fast method for the determination of noble metal simultaneously with satisfied results.The adsorption force of717, D301R and Amberlyst A-26resin were discussed.717resin have strong adsorption of Zn. Therefore, the determination results were seriousln effected by Zn. Satisfactory results of gold deposit and copper anode slime was aquired by D301R and Amberlyst A-26resin. And the interference of Bi in copper anode slime were discussed, and the elimination method is determined。Under the optimized conditions, the relative standard deviations (RSD s) of the determination method were less than5.8%and the standard added recoveries were90.2%~102.1%. The detection limit of the XRF method were0.025μg/mL (Pd),0.022μg/mL (Pt) and0.018ug/mL (Au). The quantification limit of the XRF methodwere0.083ug/g (Pd),0.073μg/g (Pt) and0.060μg/g (Au). The results of gold deposit are in goodagreementwith reference value.The results of copper anode slime are in agreement with the results of ICP-MS.The last part:on the base of the measurement of trace Pd, Pt and Au, try to determine ultratrace ultra-Trace Pd, Pt and Au. Sample with dry method and wet method respectively, using xanthate cotton diphenyl thiourea-SanZheng octyl amine cotton diphenyl thiourea-carbon foam filling Amberlyst A26resin for Separation, enrichment and doing orthogonal experiment The samples with XRF and ICP-MS determination respectively. Results obtained for the instrument detection limit limits the reproducibility and stability. The reliability of the results is small, so not to evaluate the data. Gold tailings research remains to be further explored.

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