Determination of rhodium in waste rhodium-aluminum oxide catalyst by inductively coupled plasma atomic emission spectrometry with potassium hydrogen sulfate fusion
FENG Lei, WANG Qin-long*, WANG Lei-lei, YANG Tai-bao, HUANG Chang-rong, LI Jing
Wanhua Chemical Group Co., Ltd., Yantai 264006, China
Abstract:The waste rhodium-aluminum oxide catalyst contains much rhodium. The recovery of rhodium from catalyst can reduce the production cost. Therefore, the accurate determination of rhodium content in waste rhodium-aluminum oxide catalyst is of great importance. However, the composition of waste rhodium-aluminum oxide catalyst is very complicated, and the sample cannot be completely dissolved by conventional wet digestion and microwave digestion methods. In proposed study, 0.1g of waste rhodium-aluminum oxide catalyst and 3.0g of potassium hydrogen sulfate were fused at 650℃ for 4h. The melt was dissolved with 10mL of 10% (volume fraction) sulfuric acid under heating. Then, the content of rhodium in sample solution was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The determination method of rhodium in waste rhodium-aluminum oxide catalyst by ICP-AES after fusion was established. The working conditions of ICP-AES were listed as follows: the radio frequency (RF) power was 1.20kW and the atomizing gas flow rate was 0.85L/min. The linear correlation coefficient of calibration curve was R2=0.9999. The detection limit was 0.01mg/L and the low limit of determination was 0.1mg/L. The content of rhodium in two waste rhodium-aluminum oxide catalyst samples was determined according to the experimental method. The relative standard deviation (RSD, n=9) of determination results was in range of 0.52%-0.56%. The recoveries were between 99.6% and 100.3%. The content of rhodium in two simulation samples of waste rhodium-aluminum oxide catalyst was determined according to the experimental method. The found results were consistent with the theoretical values.
李芬,周西林.微波消解-电感耦合等离子体原子发射光谱法测定铂铑系列合金中铑[J].冶金分析,2012,32(2):59-62.LI Fen,ZHOU Xi-lin.Determination of rhodium in platinum-rhodium series alloy by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2012,32(2):59-62.
[6]
刘伟,刘文,吴喜龙,等.电感耦合等离子体原子发射光谱法(ICP-AES)快速测定砂铂矿中的铂、铱、钌、铑、钯和金含量[J].中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry),2013(3):7-9.
[7]
徐文松,尤静林,王小欢.便携式X射线荧光光谱测定车用三元催化剂中铂钯铑[J].冶金分析,2014,34(3):30-34.XU Wen-song,YOU Jing-lin,WANG Xiao-huan.Determination of platinum, palladium and rhodium in vehicle-used ternary catalyst by portable X-ray fluorescence spectrometry[J].Metallurgical Analysis,2014,34(3):30-34.
[8]
刘杨,范兴祥,董海刚,等.贵金属物料的溶解技术及进展[J].贵金属,2013,34(4):65-72.LIU Yang,FAN Xing-xiang,DONG Hai-gang,et al.Dissolving techniques of precious metal materials and their development[J].Precious Metals,2013,34(4):65-72.
[9]
董海刚,汪云华,李柏榆,等.稀贵金属铑物料溶解技术研究进展[J].稀有金属,2011,35(6):939-944.DONG Hai-gang,WANG Yun-hua,LI Bai-yu,et al.Progress in dissolution technique of precious metal rhodium materials[J].Chinese Journal of Rare Metals,2011,35(6):939-944.
[10]
朱利亚,赵忆宁,赵辉,等.微波消解技术应用于难分解贵金属化合物的分析[J].冶金分析,2007,27(12):11-16.ZHU Li-ya,ZHAO Yi-ning,ZHAO Hui,et al.Application of microwave digestion technique to analysis of indissoluble precious metal compounds[J].Metallurgical Analysis,2007,27(12):11-16.