Determination of thirteen elements in denitrification catalyst by microwave digestion-inductively coupled plasma atomic emission spectrometry
WANG Yong,GONG Hou-liang,DAN Juan,CHEN Xiao-yi,LIU Lin
National Quality Supervision and Testing Center of Vanadium and Titanium Products, Product Quality Supervision and Testing Institute of Panzhihua, Panzhihua 617000, China
Abstract：The elements in denitrification catalyst are important research objects to evaluate and improve the efficiency of catalyst. Therefore, the accurate and rapid determination of contents of elements is of great significant to in-depth studies of catalyst such as performance evaluation, deactivation and regeneration, poisoning, etc. The sample was dissolved by microwave digestion in tartaric acid-hydrofluoric acid-nitric acid system. Combined with dynamic background correction technique, the matrix effect was eliminated by matrix matching method. The contents of vanadium, tungsten, molybdenum, silicon, aluminum, calcium, barium, iron, manganese, chromium, magnesium, phosphorus and arsenic were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) under selected optimum analytical lines and proper instrumental working conditions. Consequently the analysis method for the simultaneous determination of 13 elements in denitrification catalyst by ICP-AES was established. Within linear range for elements, the correlation coefficients of calibration curves were all higher than 0.999. The detection limits were between 0.001% and 0.021% (mass fraction). The proposed method was applied for the determination of vanadium, tungsten, molybdenum, silicon, aluminum, calcium, barium, iron, manganese, chromium, magnesium, phosphorus and arsenic in denitrification catalyst sample. The relative standard deviations (RSD, n=7) of results were all less than 2.0%. The recoveries were between 94% and 103%. The contents of 13 elements in three denitrification catalyst samples were determined according to the experimental method. Meanwhile, other methods were also adopted for comparison (the contents of molybdenum, tungsten, silicon, vanadium, aluminum, barium and calcium were determined by X-ray fluorescence spectrometry in national standard GB/T 31590-2015; the contents of magnesium, iron, chromium, phosphorus, manganese and arsenic were determined by ICP-AES in national standard GB/T 34701-2017). The determination results were in good agreement.
李云涛,毛宇杰,钟秦,等.SCR催化剂的组成对其脱硝性能的影响[J].燃料化学学报,2009,37(5):601-606.LI Yun-tao,MAO Yu-jie,ZHONG Qin,et al.Effects of components of SCR catalyst on DeNOx performance[J].Journal of Fuel Chemisiry and Technalogy,2009,37(5):601-606.
[3]
赵宁,李丽,韦正乐,等.燃煤电厂选择性催化还原脱硝催化剂失活及其原因分析[J].环境污染与防治,2013,35(12):68-71,77.ZHAO Yu,LI Li,WEI Zheng-le,et al.Discussion and research on the deactivation of the SCR de-NOx catalyst in the coal-fired power plants[J].Environmental Pollution and Control,2013,35(12):68-71,77.
[4]
王丽朋,陈宝康,姚燕,等.脱硝催化剂失活及再生实验[J].热力发电,2017,46(11):67-72.WANG Li-peng,CHEN Bao-kang,YAO Yan,et al.Experimental study on deactivation and regeneration performance of denitration catalysts[J].Thermal Power Generation,2017,46(11):67-72.
[5]
曹俊,傅敏,周林,等.SCR脱硝催化剂中毒的研究进展[J].应用化工,2018,47(2):380-385.CAO Jun,FU Min,ZHOU Lin,et al.Research progress of SCR denitrification catalyst poisoning[J].Applied Chemical Industry,2018,47(2):380-385.
[6]
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.
[7]
聂西度,谢华林,李坦平.SCR脱硝尿素中微量元素的质谱法测定[J].环境工程学报,2015,9(6):3037-3040.NIE Xi-du,XIE Hua-lin,LI Tan-ping.Detection of trace metal elements in SCR denitration urea by inductively coupled plasma mass spectrometry[J].Chinese Journal of Environmental Engineering,2015,9(6):3037-3040.
[8]
周小燕,邓成新.ICP-OES测燃煤电厂SCR催化剂中砷含量[J].山东化工,2017(21):81-82.ZHOU Xiao-yan,DENG Cheng-xin.Determination of arsenic content in SCR catalyst of coal fired power plant by ICP-OES[J].Shandong Chemical Industry,2017(21):81-82.
[9]
成勇,袁金红,彭慧仙,等.电感耦合等离子体原子发射光谱法测定钒钛高炉渣中钡[J].冶金分析,2014,34(11):18-23.CHENG Yong,YUAN Jin-hong,PENG Hui-xian,et al.Determination of barium in vanadium-titanium blast slag by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):18-23.
[10]
郭国龙,杨丹丹,王春叶.微波消解-电感耦合等离子体原子发射光谱法测定废脱硝催化剂中钨和钛[J].冶金分析,2018,38(1):70-74.GUO Guo-long,YANG Dan-dan,WANG Chun-ye.Determination of tungsten and titanium in waste denitration catalyst by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(1):70-74.
[11]
杨惠玲,班俊生,夏辉.微波消解电感耦合等离子发射光谱法测定三水铝土矿中的有效铝、活性铝和活性硅[J].岩矿测试,2017,36(3):246-251.YANG Hui-ling,BAN Jun-sheng,XIA Hui.Determination of available alumina, active alumina and active silicon in gibbsite bauxite by inductively coupled plasma-optical emission spectrometry with microwave digestion[J].Rock and Mineral Analysis,2017,36(3):246-251.
[12]
郭传华,李化全,董文戎.电感耦合等离子体发射光谱法(ICP-OES)测定高钛渣中的铁、钴、镍的含量[J].山东化工,2017(24):89-90,93.GUO Chuan-hua,LI Hua-quan,DONG Wen-rong.Inductively coupled plasma emission spectrometry (ICP-AES) and engage in the determination of high titanium slag iron,cobalt,nickel content[J].Shandong Chemical Industry,2017(24):89-90,93.
[13]
成勇.微波消解-电感耦合等离子体原子发射光谱法测定五氧化二钒中痕量硼和铋[J].冶金分析,2015,35(3):56-60.CHENG Yong.Determination of trace boron and bismuth in vanadium pentoxide by microwave digestion-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2015,35(3):56-60.
[14]
李寅寅.微波消解ICP-AES法测定土壤中的金属元素研究[J].环境科学与管理,2014,39(7):133-135.LI Yin-yin.Determination of metals in soil by inductively coupled plasma atomic emission spectrometry with microwave digestion[J].Environmental Science and Management,2014,39(7):133-135.
[15]
王妮,何美玲,范建凤.微波消解-ICP-OES法测定五台山蘑菇中的元素含量[J].食品研究与开发,2017,38(13):162-165.WANG Ni,HE Mei-ling,FAN Jian-feng.Determination of elements in mushrooms from mount Wutai by ICP-OES with microwave digestion[J].Food Research and Development,2017,38(13):162-165.
[16]
杜米芳.微波消解-电感耦合等离子体原子发射光谱法测定镍基合金中硅[J].冶金分析,2017,37(4):71-75.DU Mi-fang.Determination of silicon in nickel base alloy by inductively coupled plasma atomic emission spectrometry after microwave digestion[J].Metallurgical Analysis,2017,37(4):71-75.
