Determination of sodium,tungsten,iron,zinc,titanium and manganese in aluminum nitride powder by super microwave digestion-inductively coupled plasma mass spectrometry with collision cell
WU Qianye, SUN Jianmin, ZHANG Weiquan, FU Luoling, LI Ying, LI Jian
Hangzhou PuYu Technology Development Co.,Ltd.,Hangzhou 311300, China
Abstract:Aluminum nitride powder is the raw material for the preparation of aluminum nitride materials. The content of impurity metal elements in aluminum nitride powder will have an important impact on the thermal conductivity and dielectric properties of aluminum nitride products. In experiments, the samples were treated by super microwave digestion with mixture of sulfuric acid and phosphoric acid, which solved the problem that the aluminum nitride powder sample was difficult to be dissolved completely. 23Na, 182W, 54Fe, 66Zn, 46Ti and 55Mn were selected as the isotopes to be measured. The flow rate of helium was controlled at 1.52 mL/min to eliminate the mass spectrum interference using helium collision cell technology mode (CCT mode). 50 μg/L of 89Y was used to correct 23Na, 54Fe, 66Zn, 46Ti and 55Mn, while 50 μg/L 185Re was used to correct 182W. Consequently, a method for the determination of six impurity metal elements (including sodium, tungsten, iron, zinc, titanium and manganese) by inductively coupled plasma mass spectrometry (ICP-MS) with collision cell was established. Under the optimized experimental conditions, the limits of detection for six elements were in range of 0.03-0.64 mg/kg, and the limits of quantification were in range of 0.10-2.13 mg/kg. The aluminum nitride powder sample was determined according to the experimental method. The relative standard deviations (RSD, n=6) of determination results for six elements were all less than 4%. The recoveries were between 96% and 103%. The method comparison tests were conducted by inductively coupled plasma atomic emission spectrometry (ICP-AES) and graphite furnace atomic absorption spectrometry (GF-AAS), and the determination results were basically consistent with those obtained by the experimental method.
吴浅耶, 孙建民, 张维权, 付罗岭, 李鹰, 李剑. 超级微波消解-碰撞池-电感耦合等离子体质谱法测定氮化铝粉中钠钨铁锌钛锰[J]. 冶金分析, 2022, 42(7): 19-25.
WU Qianye, SUN Jianmin, ZHANG Weiquan, FU Luoling, LI Ying, LI Jian. Determination of sodium,tungsten,iron,zinc,titanium and manganese in aluminum nitride powder by super microwave digestion-inductively coupled plasma mass spectrometry with collision cell. , 2022, 42(7): 19-25.
[1] 李清涛,吴清仁,孙创奇,等.高导热率AlN陶瓷材料制备与应用进展[J].陶瓷学报,2007,28(1):57-64. LI Qingtao,WU Qingren,SUN Chuangqi,et al.Progress in fabrication and application of high thermal conductivity AlN ceramics[J].Journal of Ceramics,2007,28(1):57-64. [2] 严光能,邓先友,林金堵.高导热氮化铝基板在航空工业的应用研究[J].印制电路信息,2017,25(10):32-37. YAN Guangneng,DENG Xianyou,LIN Jindu.The research of high-thermal-conductive aluminum nitride substrate in airport power electronics[J].Printed Circuit Information,2017,25(10):32-37. [3] 高冬云.氮化铝陶瓷材料制备工艺与应用[J].现代技术陶瓷,2002,23(3):14-23. GAO Dongyun.Preparation of aluminum nitride material and its application[J].Advanced Ceramics,2002,23(3):14-23. [4] 王广阳.氮化铝陶瓷的酸洗提纯与高温纯化研究[D].武汉:武汉理工大学,2018. [5] 墨淑敏,李爱嫦,邱长丹,等.微波消解-火焰原子吸收光谱法测定氮化铝粉中钾和钠[J].冶金分析,2020,40(9):70-74. MO Shumin,LI Aichang,QIU Changdan,et al.Determination of potassium and sodium in aluminum nitride powder by microwave digestion-flame atomic absorption spectrometry[J].Metallurgical Analysis,2020,40(9):70-74. [6] 卢桂萍,汪正,邱德仁,等.悬浮液进样自吸扣背景石墨炉原子吸收光谱法测定高纯氧化铝中铜、铁和钠含量[J].光谱学与光谱分析,2011,31(1):244-248. LU Guiping,WANG Zheng,QIU Deren,et al.Direct determination of copper, iron and sodium in high-purity alumina by slurry introduction furnace atomic absorption spectrometry with Smith-Hieftje background correction[J].Spectroscopy and Spectral Analysis,2011,31(1):244-248. [7] 戴品中,李齐春,潘齐存,等.电感耦合等离子体原子发射光谱法测定高纯氧化铝中15种痕量元素[J].现代化工,2011,31(z1):430-433. DAI Pinzhong,LI Qichun,PAN Qicun,et al.Determination of 15 trace elements in high-purity alumina by ICP-AES[J].Modern Chemical Industry,2011,31(z1):430-433. [8] 赵子云,梅连平,史鑫,等.悬浮液直接进样ICP-OES法测定高纯氧化铝中的铁、钛、硅、铬[J].化学分析计量,2017,26(1):55-57. ZHAO Ziyun,MEI Lianping,SHI Xin,et al.Determination of iron, titanium, silicon, chromium in high purity alumina by suspension sampling inductively coupled plasma emission spectrometry[J].Chemical Analysis and Meterage,2017,26(1):55-57. [9] 李洪亮,曲凤娇,曹阳,等.ICP-AES测定铝及铝合金中锌元素含量的影响因素研究[J].有色金属加工,2021,50(5):37-39. LI Hongliang,QU Fengjiao,CAO Yang,et al.Study on influencing factors of determination of zinc element in aluminum and aluminum alloy by ICP-AES[J].Nonferrous Metals Processing,2021,50(5):37-39. [10] 陈玉红,王海舟,张华,等.微波消解电感耦合等离子体质谱法测定铝合金中多元素[J].冶金分析,2008,28(7):1-6. CHEN Yuhong,WANG Haizhou,ZHANG Hua,et al.Determination of multi-elements in aluminum alloys by using microwave digestion inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2008,28(7):1-6. [11] 成学海,夏传波,郑建业,等.封闭压力酸溶-电感耦合等离子体质谱法同时测定电气石中29种元素[J].岩矿测试,2017,36(3):231-238. CHENG Xuehai,XIA Chuanbo,ZHENG Jianye,et al.Simultaneous determination of 29 trace elements in tourmaline by inductively coupled plasma-mass spectrometry with sealed press acid decomposition[J].Rock and Mineral Analysis,2017,36(3):231-238. [12] 张丽,陈雄飞,张力久,等.碱熔融分光光度法测定氮化铝中硅的质量分数[J].当代化工研究,2018(2):13-14. ZHANG Li,CHEN Xiongfei,ZHANG Lijiu,et al.Determination of the mass fraction of silicon in aluminum nitride by alkali melt spectrophotometry[J].Modern Chemical Research,2018(2):13-14. [13] 艾靖娇,王建文,方文韬,等.硫磷混酸溶矿测定矿样中铝、铬方法研究[J].云南地质,2013,32(3):347-351. AI Jingjiao,WANG Jianwen,FANG Wentao,et al.A study on the method of Al,Cr testing of ore sample by S-P mixed acid solution[J].Yunnan Geology,2013,32(3):347-351. [14] 何崇慧,顾青,尹玲玲,等.消解法-原子吸收法测定氧化铝基催化剂中钯含量[J].石化技术与应用,2019,37(5):352-355. HE Chonghui,GU Qing,YIN Lingling,et al.Determination of palladium in alumina-based catalysts by digestion-atomic absorption spectrometry[J].Petrochemical Technology & Application,2019,37(5):352-355. [15] 王艳君,蒋晓光.ICP-AES法测定氧化铝粉中硅、钙、铁、钛、钒和锌[J].分析测试技术与仪器,2002,8(1):31-33. WANG Yanjun,JIANG Xiaoguang.Determination of silica,calcium,iron,titanium,vanadium and zinc content in aluminium oxide by inductively coupled plasma atomic emission spectrometry[J].Analysis and Testing Technology and Instruments,2002,8(1):31-33. [16] 姜郁,王通胜,魏志勇,等.微波消解-ICP-AES法测定氧化铝中杂质元素[J].分析试验室,2006,25(8):57-61. JIANG Yu,WANG Tongsheng,WEI Zhiyong,et al.Determination of sodium,potassium,calcium,silicon,iron,titanium, manganese,zinc,copper,vanadium,chromium and boron in alumina by inductively coupled plasma atomic emission spectrometry with microwave digestion[J].Chinese Journal of Analysis Laboratory,2006,25(8):57-61. [17] 孙宝莲,张小燕,李波.石墨炉原子吸收法测定合金钢、铜合金及铝合金中微量钛[J].稀有金属材料与工程,2003,32(1):76-79. SUN Baolian,ZHANG Xiaoyan,LI Bo.Determination of trace titanium in metallurgical material[J].Rare Metal Materials and Engineering,2003,32(1):76-79.