Determination of rhenium in platinum rhenium spent catalyst byinductively coupled plasma atomic emission spectrometry
MA Wang-rui,LIU Wen,ZHANG Xuan-dong,LUO Xian,CHONG Biao,HAN Shou-li*
State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals, Sino-Platinum MetalsResources (Yimen) Co., Ltd., Sino-Platinum Metals Co., Ltd., Kunming 650106, China
Abstract：The carbon, sulfur and organic matters in platinum rhenium spent catalyst could be removed by high temperature ignition. However, the volatilization loss of rhenium was also serious. According to the principle that the carbon, sulfur and organic matters could be removed by perchloric acid fuming while the rhenium was not volatilized when the temperature was less than 300℃, the sample was digested by nitric acid and perchloric acid in this study. The determination method of rhenium in platinum rhenium spent catalyst by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The following experimental conditions were obtained: the amount of sample was 0.15g; 2.0mL of nitric acid and 1.0mL of perchloric acid were added followed by fuming at 260-290℃; then 2.0mL of nitric acid was added and the solution was heated until fume just appeared; the operation was repeated for twice until the sample solution was clear; 10.0mL of hydrochloric acid was added; the solution was transferred into 100mL volumetric flask and diluted to the mark; the content of rhenium was determined by ICP-AES using Re 221.426nm as the analytical line. The coexisting ions including aluminum (III), platinum (IV) and iron (III) had no interference with the determination. The proposed method was applied for the determination of rhenium (639.4-5854.8g/t) in one test sample and four actual samples of platinum rhenium spent catalyst. The determination value of test sample was basically consistent with the recommended value. The relative standard deviations (RSD, n=11) of determination results were between 0.17% and 0.63%, and the spiked recoveries were between 98.8% and 100.3%.
李红梅,贺小塘,赵雨,等.铼的资源、应用和提取[J].贵金属,2014,35(2):77-81.LI Hong-mei,HE Xiao-tang,ZHAO Yu,et al. Resources,application and extraction status of rhenium[J].Precious Metals, 2014,35(2):77-81.
[2]
董海刚,刘杨,范兴祥,等.铼的回收技术研究进展[J].有色金属:冶炼部分,2013(6):30-33.DONG Hai-gang,LIU Yang,FAN Xing-xiang,et al.Research progress on recovery of research[J].Nonferrous Metals :Extractive Metallurgy,2013(6):30-33.
[3]
周煜,谭艳山,朱利亚,等. 硫脲光度法测定粗铼酸钾中铼时钼干扰的消除[J].冶金分析,2013,33(9): 57-60.ZHOU Yu,TAN Yan-shan,ZHU Li-ya,et al.Elimination of the interference of molybdenum in determination of rhenium in raw potassium rhenate by thiourea spectrophotometry[J].Metallurgical Analysis,2013,33(9):57-60.
[4]
史谊峰,唐慧,王传飞,等.电感耦合等离子体发射光谱法(ICP-AES)测定富铼渣中的铼[J].中国无机分析化学,2015,5(3):59-63.SHI Yi-feng,TANG Hui,WANG Chuan-fei,et al.Determination of rhenium in rhenium rich slag samples by inductively coupled plasma atomic emission spectrometry[J].Chinese Iournal of Inorganic Analytical Chemistry,2015,5(3):59-63.
[5]
梁波,沈宏伟,罗明标,等.铼的分析方法研究进展[J].江西化工,2014(3):76-80.LIANG Bo,SHEN Hong-wei,LUO Ming-biao,et al.Research progresson the determination of rhenate[J].Jiangxi Chemical Industry,2014(3):76-80.
[6]
孙宝莲,周恺,李波,等.分光光度法测定铼回收溶液中的铼含量[J].光谱实验室,2013,30(2):3922-3925.SUN Bao-lian,ZHOU Kai,LI Bo,et al.Determination of rhenium comount in the liquids of rhenium recovering by spectrophotometry[J].Chinese Journal of Spectroscopy Laboratory,2013,30(2):3922-3925.
[7]
郑文英,李君,房勇,等.硫氰酸钾光度法测定铜精矿冶炼污酸中铼[J].冶金分析,2015,35(9):68-72.ZHENG Wen-ying,LI Jun,FANG Yong,et al.Determination of rhenium in smelting waste acid of copper concentrate samples by potassium rhodanate extraction spectrophotometry[J].Metallurgical Analysis,2015,35(9):68-72.
[8]
郭俊梅,李锟,贺小塘,等.四苯砷氯盐酸盐重量法测定粗铼化合物中铼[J].冶金分析,2016,36(11):29-33.GUO Jun-mei,LI Kun,HE Xiao-tang,et al.Determination of rhenium in raw rhenium complexs by tetraphenylarsonium hydrochloride gravimetry[J].Metallurgical Analysis,2016,36(9):29-33.
[9]
李锟,贺小塘,韩守礼,等.氢还原重量法测定铼酸铵制备铼粉产品中铼[J].冶金分析,2017,37(7):57-62.LI Kun,HE Xiao-tang,HAN Shou-li,et al.Determination of rhenium in rhenium powder products prepared with ammonium rhenate by hydrogen reduction gravimetry[J].Metallurgical Analysis,2017,37(7):57-62.
[10]
李延超,李来平,周恺,等.加压氧化钼精矿浸出液中铼的测定[J].分析试验室,2014,33(9):1030-1033.LI Yan-shao,LI Lai-pin,ZHOU Kai,et al.Determination of rhenium in leaching solution of molybdenum oxide under pressure[J].Chinese Journal of Analysis Laboratory,2014,33(9):1030-1033.
