Abstract:The high-purity oxalic acid is an important reagent in the electronics industry. Its purity and cleanliness have important influence on the rate of finished products, the electrical property and reliability of products. If the impurities are determined by the chemical wet method, the pretreatment process will be complicated. Due to the lack of corresponding standard reference materials, the elemental fractionation effect and matrix effect cannot be well corrected, which limits the application of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) in quantitative analysis.The influence of laser ablation conditions on the determination results by LA-ICP-MS was systematically investigated. A series of high-purity oxalic acid calibration standard samples were prepared after drying and grinding by adding different amounts of standard solutions of analytes. Meanwhile, the actual sample was also prepared to tablets. The determination of four impurity elements including Zn, Ni, Ba and Pb in high-purity oxalic acid by LA-ICP-MS was realized. Under the optimized experimental conditions, the linear ranges of elements were between 50.0 ng/g and 600.0 ng/g. The correlation coefficients were higher than 0.98, and the detection limits were in the range of 3.2-21.1 ng/g. The contents of Zn, Ni, Ba and Pb in different six bathes of high-purity oxalic acid sample were determined according to the experimental method. Each sample was determined for 5 times. Meanwhile, the method of ICP-MS after microwave digestion was also used for comparison. The results showed that two methods had good consistency. The relative standard deviations (RSD, n=5) were between 3.0% and 15%. One sample was determined repeatedly within three days, and the RSDs (n=5) were between 5.7% and 16%.
贺静, 苏爽, 张培, 卢梦娜, 韩华云. 激光剥蚀-电感耦合等离子体质谱法测定高纯草酸中锌镍钡铅[J]. 冶金分析, 2019, 39(8): 1-7.
HE Jing, SU Shuang, ZHANG Pei, LU Meng-na, HAN Hua-yun. Determination of zinc, nickel, barium and lead in high-purity oxalic acid by laser ablation-inductively coupled plasma mass spectrometry. , 2019, 39(8): 1-7.
穆启道.集成电路制作技术的发展与超净高纯试剂的应用[J].集成电路应用,2003,14(2):56-60.MU Qi-dao.Development of integrated circuit fabrication technology and application of ultra-clean high-purity reagents[J].Integrated Circuit Application,2003,14(2):56-60.
[2]
郑学根,邱晓生,汪道明.一种新型超净高纯试剂在半导体技术中的应用[J].半导体技术,2005,30(9):20-23.ZHENG Xue-gen,QIU Xiao-sheng,WANG Dao-ming.Application of a new super-clean and high-purity reagent type in semiconductor technology[J].Semiconductor Technology,2005,30(9):20-23.
[3]
刘天煦.介绍SEMI标准的化学试剂规范[J].中国石油和化工标准与质量,1991(10):30-31.LIU Tian-xi.Introduction of the SEMI standard chemical reagent specification[J].Chinese Chemical Standards and Quality in Petroleum,1991(10):30-31.
[4]
陈晓峰,胡芳菲,张煦,等.激光剥蚀-电感耦合等离子体质谱法测定纯铜中铁锌砷锡锑铅铋[J].冶金分析,2018,38(12):1-6.CHEN Xiao-feng,HU Fang-fei,ZHANG Xu,et al.Determination of iron, zinc, arsenic, tin, antimony, lead and bismuth in pure copper by laser ablation inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2018,38(12):1-6.
[5]
金献忠,陈建国,张建波.冷等离子体激光剥蚀电感耦合等离子体质谱法测定钢铁中14种元素[J].冶金分析,2014,34(1):10-16.JIN Xian-zhong,CHEN Jian-guo,ZHANG Jian-bo.Determination of fourteen elements in iron and steel by cool plasma laser ablation inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2014,34(1):10-16.
[6]
Ming L,Hu Z,Shan G,et al.Direct quantitative determination of trace elements in fine-grained whole rocks by laser ablation-inductively coupled plasma-mass spectrometry[J].Geostandards & Geoanalytical Research,2015,35(1):7-22.
[7]
Kim U J,Kannan K.Method for the determination of iodide in dried blood spots from newborns by high performance liquid chromatography tandem mass spectrometry[J].Analytical Chemistry,2018,90:3291-3298.
[8]
StRk H J,Wennrich R.A new approach for calibration of laser ablation inductively coupled plasma mass spectrometry using thin layers of spiked agarose gels as references[J].Analytical and Bioanalytical Chemistry,2011,399(6):2211-2217.
[9]
Claverie F,Fernández B,Pécheyran C,et al.Elemental fractionation effects in high repetition rate IR femtosecond laser ablation ICP-MS analysis of glasses[J].Journal of Analytical Atomic Spectrometry,2009,24(7):891-902.
[10]
Limbeck A,Galler P,Bonta M,et al.Recent advances in quantitative LA-ICP-MS analysis: challenges and solutions in the life sciences and environmental chemistry[J].Analytical & Bioanalytical Chemistry,2015,407(22):6593-6617.
[11]
Leite T D F,Jr R E,Fonseca T C O D,et al.Determination of major, minor and trace elements in rock samples by laser ablation inductively coupled plasma mass spectrometry:Progress in the utilization of borate glasses as targets[J].Spectrochimica Acta Part B Atomic Spectroscopy,2011,66(5):314-320.
[12]
Hsieh H F,Chang W S,Hsieh Y K,et al.Lead determination in whole blood by laser ablation coupled with inductively coupled plasma mass spectrometry[J].Talanta,2009,79(2):183-188.
[13]
徐鸿志,靳兰兰,李爱荣,等.激光剥蚀等离子体质谱分析中激光剥蚀参数对信号响应的影响[J].岩矿测试,2005,24(3):171-175.XU Hong-zhi,JIN Lan-lan,LI Ai-rong,et al.The effects of laser ablation operating parameters on signal response in LA-ICP-MS microanalysis[J].Rock and Mineral Analysis,2005,24(3):171-175.