Abstract：There is no unified standard method for the determination of impurity elements in rhodium compounds. The impurity elements in product standard are usually analyzed by spectrography after reducing the compound into rhodium powder. This method not only requires to reduce compound into rhodium powder, but also consumes powdered standard sample for spectrochemical analysis. The analytical procedures are long and the cost is high. In experiment, the sample was dissolved with hydrochloric acid-nitric acid mixture. Ni 221.647 nm, Fe 259.940 nm, Cu 324.754nm, Al 396.152 nm, Pb 220.353 nm, Pd 340.458 nm, Pt 299.797 nm, Ca 393.366 nm, Mg 279.553 nm, Zn 213.856 nm and Cr 205.552 nm were selected as the analytical lines. The background interference was eliminated by background subtraction. The experiments indicated that there was no matrix effect and interference among testing elements. Consequently, the determination method of 11 impurity elements in rhodium trichloride by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The linear correlation coefficient (r) of calibration curves of all elements were greater than 0.999. The limits of quantification were all lower than 0.001% (mass fraction). The proposed method was applied for the determination of nickel, iron, copper, aluminum, lead, palladium, platinum, calcium, magnesium, zinc, and chromium in rhodium trichloride. The relative standard deviations (RSD, n=11) of determination results were between 6.4% and 16.5%. The determination results of 11 impurity elements in rhodium trichloride were consistent with those obtained by national standard method GB/T 1421-2004.
[1] 李继霞,蒋凌云,李俊,等.含铑物料中铑测定方法的研究进展[J].贵金属,2014,35(4):88-91. LI Jixia,JIANG Lingyun,LI Jun,et al.Research progress on determination methods of rhodium in materials containing rhodium[J].Precious Metals,2014,35(4):88-91. [2] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会. GB/T 1421—2004 铑粉[S].北京:中国标准出版社,2004. [3] 陈新坤.电感耦合等离子体光谱法原理和应用[M].天津:南开大学出版社,1987:193-235. [4] 辛仁轩.等离子体发射光谱分析[M].北京:化学工业出版社,2005:155-171. [5] 龚琦.对电感耦合等离子体发射光谱法中一些问题的认识[J].冶金分析,2018,38(9):26-30. GONG Qi.Understanding of some issues about inductively coupled plasma emission spectrometry[J].Metallurgical Analysis,2018,38(9):26-30. [6] Metody Karadjov,Nikolaya Velitchkova,Olga Veleva,et al.Spectral interferences in the determination of rhenium in molybdenum and copper by inductively coupled plasma optical emission spectrometry[J].Spectrochimica Acta Part B Atomic Spectroscopy,2016,119:76-82. [7] 杨平,邓传东,孙琳,等.电感耦合等离子体原子发射光谱法测定核级铁铬铝合金中10种杂质元素[J].冶金分析,2019,39(11):74-78. YANG Ping,DENG Chuandong,SUN Lin,et al.Determination of ten impurity elements in nuclear grade iron-chromium-aluminum alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis, 2019,39(11):74-78. [8] 李秋莹,甘建壮,王应进,等.共沉淀分离-电感耦合等离子体原子发射光谱法测定含难熔金属岩石中12种稀土元素[J].冶金分析,2019,39(12):25-30. LI Qiuying,GAN Jianzhuang,WANG Yingjin,et al.Determination of twelve rare earth elements in rock containing refractory metals by inductively coupled plasma atomic emission spectrometry with coprecipitation separation[J].Metallurgical Analysis,2019,39(12):25-30. [9] 周凯红,张立锋,刘晓杰,等.电感耦合等离子体原子发射光谱法测定镧玻璃废粉中五氧化二铌、二氧化锆和二氧化钛[J].冶金分析,2016,36(12):44-49. ZHOU Kaihong,ZHANG Lifeng,LIU Xiaojie,et al.Determination of niobium pentoxide,zirconium dioxide and titanium dioxide in waste powder of La glass by inductively coupled plasma atomic emission spectrometry [J].Metallurgical Analysis,2016,36(12):44-49. [10] 任玲玲.微波消解-电感耦合等离子体原子发射光谱法测定炉渣中硼[J].冶金分析,2018,38(2):71-75. REN Lingling.Determination of boron in slag by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(2):71-75. [11] 方卫,冯璐,李青,等.ICP-AES法测定三苯基膦氯化铑中的微量杂质[J].贵金属,2016,37(3):56-59. FANG Wei,FENG Lu,LI Qing,et al.Determination of trace impurities in triphenylphosphine rhodium chloride by ICP-AES method[J].Precious Metals,2016,37(3):56-59. [12] 王应进,徐光,李秋莹,等.电感耦合等离子体原子发射光谱法测定碘化铑中10种杂质元素[J].云南冶金,2019,48(6):75-78. WANG Yingjin,XU Guang,LI Qiuying,et al.Determination of 10 impurity elements in rhodium iodide by inductively coupled plasma atomic emission spectrometry[J].Yunnan Metallurgy,2019,48(6):75-78. [13] 王应进,李秋莹,李玉萍,等.电感耦合等离子体原子发射光谱法测定辛酸铑催化剂中铂钯铅铁铜铝镍[J].冶金分析,2019,39(6):24-28. WANG Yingjin,LI Qiuying,LI Yuping,et al.Determination of platinum,palladium,lead,iron,copper,aluminum,nickel in rhodium octanate dimer catalyst by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2019,39(6):24-28.
