Respective determination of gold and platinum in gold-platinum waste liquid by gravimetry and inductively coupled plasma atomic emission spectrometry with extraction separation
MA Wangrui1, YAO Yanbo1, LIN Bo1, WU Xilong1, ZHAO Yu1, XIONG Qingfeng*1,2
1. Sino-Platinum Metals ResourcesYimenCo.,Ltd.,Yuxi 651100,China; 2. Kunming Institute of Precious Metals,Kunming 650016, China
Abstract:It is of great significance to accurately determine Au and Pt in the gold-platinum waste liquid with large disparities in content for the metal balance in market transactions and metallurgical production. During the respective determination of high content Au and low content Pt in gold-platinum waste liquid by fire assay-gravimetry and inductively coupled plasma atomic emission spectrometry (ICP-AES), the error of determination results was relatively high due to the mutual interference between Au and Pt, which could not meet the requirements in the metal balance in market transactions and metallurgical production that the absolute error should not be higher than ±0.05%. Combining the technology of metallurgical refining gold with the determination method of Pt by ICP-AES, Au was determined by ether extraction separation-ammonium oxalate reduction-gravimetry and Pt was determined by ether extraction separation-ICP-AES. The experimental conditions for determination of Au by gravimetry were listed as below: 2 g of gold-platinum waste liquid was extracted for three times with total 30 mL of ether to separate Au(Ⅲ); then Au(Ⅲ) was reduced with 2.4-3.2 g of ammonium oxalate for 40 min followed by drying at 105 ℃ for 55 min. The experimental conditions for determination of Pt were listed as below: 0.15 g of gold-platinum waste liquid was extracted twice with total 8 mL of ether to separate Au(Ⅲ); then the content of Pt was determined by ICP-AES in the medium of 10% hydrochloric acid. The contents of Au in range of 84%-89% (mass fraction, similarly hereinafter) and Pt in range of 0.5%-5% in gold-platinum waste liquid were determined according to the proposed method. The relative standard deviations (RSDs, n=11) of determination results were 0.030%-0.036% for Au and 0.12%-0.30% for Pt. The recoveries of Au and Pt were 99.88%-100.19% and 99.45%-100.36%, respectively.
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