Determination of fourteen metal elements in coal fly ash by inductively coupled plasma mass spectrometry with microwave digestion
ZHOU Yu-min,TIAN Kan,FENG Yue-peng,SUN Zi-jie*
Institute for Environmental Reference Materials of Ministry of Environmental Protection, State Environmental Protection Key Laboratory of Environmental Pollutant Metrology and Reference Materials, Beijing 100029, China
Abstract：The coal fly ash sample was treated by microwave digestion in HNO3-HF mixed acid system. A determination method of fourteen trace elements in coal fly ash by inductively coupled plasma mass spectrometry(ICP-MS) was established. The microwave digestion procedures for sample were as follows: 10 mL of HNO3 and 5 mL of HF were added into 0.2 g of sample; the temperature was increased to 110 ℃ within 5 min and kept for 5 min; then, the temperature was increased to 150 ℃ within 5 min and kept for 5 min; finally, the temperature was increased to 190 ℃ within 5 min and kept for 30 min. The elements with high content such as Be, Co, Cr, Cu, Mn, Mo, Ni, Pb, Sn, V and Zn were diluted for 10 times to reduce the content of total dissolved solid(TDS) followed by determination with external standard method. For the elements with low content such as Cd, Sb and Tl, the standard addition method was adopted to eliminate the matrix interference. The detection limit of method was 0.001-0.04 mg/kg. The proposed method was applied to the determination of eleven metal elements (Be, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sb, V, Zn) in certified reference material of coal fly ash (SRM 1633c), and the results were consistent with the certified values. The relative standard deviations(RSD,n=6) were between 0.3% and 3.6%. The recoveries were between 83% and 112%. The determination results of coal fly ash actual sample according to the experimental method were compared with the average values obtained by inductively coupled plasma atomic emission spectrometry(ICP-AES), ICP-MS, atomic absorption spectrometry(AAS), X-ray fluorescence spectrometry(XRF) and titration method in 12 laboratories. The t test statistics indicated that there was no significant difference.
周裕敏,田衎,封跃鹏,孙自杰. 微波消解-电感耦合等离子体质谱法测定煤飞灰中14种金属元素[J]. 冶金分析, 2016, 36(9): 42-46.
ZHOU Yu-min,TIAN Kan,FENG Yue-peng,SUN Zi-jie. Determination of fourteen metal elements in coal fly ash by inductively coupled plasma mass spectrometry with microwave digestion. , 2016, 36(9): 42-46.
胡敏,唐倩,彭剑飞,等.我国大气颗粒物来源及特征分析[J].环境与可持续发展,2011,36(5):15-19.HU Min,TANG Qian,PENG Jian-fei,et al.Study on characterization and source apportionment of atmospheric particulate matter in China[J].Environment and Sustainable Development,2011,36(5):15-19.
[2]
杨绍晋,杨亦男,钱琴芳.京津地区大气颗粒物的表征及来源鉴别[J].环境科学学报,1987,7(4):411-423.YANG Shao-jin,YANG Yi-nan,QIAN Qin-fang.Characterization and source identification of atmospheric particulate matter in Beijing and Tianjin[J].Acta Scientiae Circumstantiae,1987,7(4):411-423.
[3]
徐光.辽宁省三城市大气颗粒物来源解析研究[J].中国环境监测,2007,23(3):57-61.XU Guang.Study on source apportionment for ambient air particulate matter in three cities of Liaoning province[J].Environmental Monitoring in China,2007,23(3):57-61.
[4]
王淑兰,柴发合,张远航,等.成都市大气颗粒物污染特征及其来源分析[J].地理科学,2004,24(4):488-492.WANG Shu-lan,CHAI Fa-he,ZHANG Yuan-hang,et al.Analysis on the sources and characters of particles in Chengdu[J].Scientia Geographica Sinica,2004,24(4):488-492.
[5]
黄辉军,刘红年,蒋维楣,等.南京市主城区大气颗粒物来源探讨[J].气象科学,2007,27(2):162-168.HUANG Hui-jun,LIU Hong-nian,JIANG Wei-mei,et al.Source apportionment research of atmospheric particulate in Nanjing[J].Scientia Meteorologica Sinica,2007,27(2):162-168.
[6]
刘咸德,封跃鹏,贾红,等.青岛市大气颗粒物来源的定量解析:化学质量平衡方法[J].环境科学研究,1998,11(5):51-54.LIU Xian-de,FENG Yue-peng,JIA Hong,et al.Source apportionment of air particulate matter in Qingdao: chemical mass balance[J].Research of Environmental Sciences,1998,11(5):51-54.
王晖,宋蔷,姚强,等.微波消解与ICP-OES/ICP-MS测定飞灰中的多种元素[J].光谱实验室,2012,29(1):525-528.WANG Hui,SONG Qiang,YAO Qiang,et al.Determination of multi-elements in fly ash by ICP-OES and ICP-MS with microwave digestion[J].Chinese Journal of Spectroscopy Laboratory,2012,29(1):525-528.
[9]
Lachas H,Richaud R,Herod A,et al.Determination of 17 trace elements in coal and ash reference materials by ICP-MS applied to milligram sample sizes[J].Analyst,1999,124(2):177-184.
[10]
周勇义,谷学新,范国强,等.微波消解技术及其在分析化学中的应用[J].冶金分析,2004,24(2):30-36.ZHOU Yong-yi,GU Xue-xin,FAN Guo-qiang,et al.Application of microwave digestion in analytical chemistry[J].Metallurgical Analysis,2004,24(2):30-36.
[11]
刘华.微波消解技术在分析食品中微量元素方面的应用[J].中国卫生检验杂志,2001,11(4):406-408.LIU Hua.The technical application of the method breaking down the food sample in the special microwave oven for analyzing microelement[J].Chinese Journal of Health Laboratory Technology,2001,11(4):406-408.
[12]
刘丽萍,张妮娜,周珊,等.电感耦合等离子体质谱法(ICP-MS)测定饮用水及水源水中31种元素[J].中国卫生检验杂志(Chinese Journal of Health Laboratory Technology),2005,15(8):932-934.
[13]
陈杭亭,曹淑琴,曾宪津.电感耦合等离子体质谱方法在生物样品分析中的应用[J].分析化学,2001,29(5):592-600.CHEN Hang-ting,CAO Shu-qin,ZENG Xian-jin.Application of inductively coupled plasma mass spectrometry in biological samples analysis[J].Chinese Journal of Analytical Chemistry,2001,29(5):592-600.
[14]
袁倬斌,吕元琦,张裕平,等.电感耦合等离子体质谱在铂族元素分析中的应用[J].冶金分析,2003,23(2):24-30.YUAN Zhuo-bin,L Yuan-qi,ZHANG Yu-ping,et al.The application of inductively coupled plasma mass spectrometry in analysis of platinum group elements[J].Metallurgical Analysis,2003,23(2):24-30.
[15]
U.S.Environmental Protection Agency (EPA).Method 3052—Microwave assisted acid digestion of siliceous and organically based matrices[S].Washington DC:[s.n.],1996.
[16]
刘素华,刘岚铮,翟明霞,等.微波消解测定食品中金属元素的方法探讨[J].中国食品卫生杂志,2004,16(4): 342-344.LIU Su-hua,LIU Lan-zheng,ZHAI Ming-xia,et al.Discussion on the microwave digestion method for determination of metals in foods[J].Chinese Journal of Food Hygiene,2004,16(4):342-344.
