硫酸氢钾熔融-电感耦合等离子体原子发射光谱法测定废铑氧化铝催化剂中铑
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摘要
废铑氧化铝催化剂中含有大量铑元素,回收催化剂中铑元素可以降低生产成本,因此准确测定废铑氧化铝催化剂中铑元素含量至关重要。然而废铑氧化铝催化剂组成复杂,常规湿法消解和微波消解方法无法完全溶解样品。实验采用0.1g废铑氧化铝催化剂和3.0g硫酸氢钾在650℃下熔融4h,熔融物使用10mL 10%(体积分数)硫酸加热溶解,然后使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铑,建立了熔融-电感耦合等离子体原子发射光谱法测定废铑氧化铝催化剂中铑的方法。ICP-AES工作条件为射频(RF)功率1.20kW、雾化气流量0.85L/min。校准曲线的线性相关系数R2=0.999 9;方法检出限为0.01mg/L,测定下限为0.1mg/L。按照实验方法测定两个废铑氧化铝催化剂中铑,测定结果的相对标准偏差(RSD,n=9)为0.52%～0.56%;加标回收率为99.6%～100.3%。实验方法用于测定两个废铑氧化铝催化剂模拟样品中铑,测定值和理论值相一致。
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,0.1 g of waste rhodium-aluminum oxide catalyst and 3.0 g of potassium hydrogen sulfate were fused at 650℃for 4 h.The melt was dissolved with 10 mL 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(ICPAES).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 1.20 kW and the atomizing gas flow rate was 0.85 L/min.The linear correlation coefficient of calibration curve was R2=0.999 9.The detection limit was 0.01 mg/L and the low limit of determination was 0.1 mg/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.
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,0.1 g of waste rhodium-aluminum oxide catalyst and 3.0 g of potassium hydrogen sulfate were fused at 650℃for 4 h.The melt was dissolved with 10 mL 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(ICPAES).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 1.20 kW and the atomizing gas flow rate was 0.85 L/min.The linear correlation coefficient of calibration curve was R2=0.999 9.The detection limit was 0.01 mg/L and the low limit of determination was 0.1 mg/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.
引文
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[2]董守安.现代贵金属分析[M].北京:化学工业出版社,2006.
[3]全国有色金属标准化技术委员会.YS/T 561-2009贵金属合金化学分析方法铂铑合金中铑量的测定硝酸六氨合钴重量法[S].北京:中国标准出版社,2010.
[4]全国有色金属标准化技术委员会.YS/T 563-2009贵金属合金化学分析方法:铂钯铑合金中钯量、铑量的测定丁二肟重量法、氯化亚锡分光光度法[S].北京:中国标准出版社,2010.
[5]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 vehicleused 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.
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