Abstract：The high purity graphite is a kind of excellent function materials and it has been widely used in national defense and aerospace industries. The determination requirements of trace impurities content are increasing year by year. At present, the detection limits of current testing methods are relatively high, which could not meet the increasing determination requirements. 1 g of high purity graphite sample was put into muffle furnace at 1 100 ℃ and completely ashed. After cooling, 3 g of flux (m(H3BO3)∶m(Na2CO3)=1∶2) was added. Then, the sample was put into muffle furnace again for melting at 1 100 ℃ for 40 min. The cooled salts were dissolved with hydrochloric acid (1+1). Thus, a determination method of nine impurities including aluminum, calcium, chromium, copper, iron, magnesium, nickel, silicon and zinc in high purity graphite was established by inductively coupled plasma atomic emission spectrometry (ICP-AES) with Al 396.152 nm, Ca 396.847 nm, Cr 267.716 nm, Cu 324.754 nm, Fe 238.204 nm, Mg 279.553 nm, Ni 231.604 nm, Si 251.612 nm and Zn 213.856 nm as analytical lines. The results showed that the mass concentration of aluminum, calcium, chromium, copper, iron, magnesium, nickel, silicon and zinc in range of 0.50-500 μg/mL was linear to the emission intensity. The linear correlation coefficients of calibration curves were all higher than 0.999 5. The detection limits of elements were between 0.037 μg/g and 0.87 μg/g. The proposed method was applied to the determination of nine impurities in high-purity graphite samples. The results were consistent with those obtained by inductively coupled plasma mass spectrometry. The relative standard deviations (RSD, n=7) were less than 6.0%. The recoveries were between 93% and 108%.
杨倩倩, 何石, 胡月, 彭霞, 李美玲. 电感耦合等离子体原子发射光谱法测定高纯石墨中9种元素[J]. 冶金分析, 2016, 36(3): 49-53.
YANG Qian-qian, HE Shi, HU Yue, PENG Xia, LI Mei-ling. Determination of nine elements in high purity graphite by inductively coupled plasma atomic emission spectrometry. , 2016, 36(3): 49-53.
谢刚,李晓阳,臧健,等.高纯石墨制备现状及进展[J].云南冶金,2011,40(1):48-51.XIE Gang,LI Xiao-yang,ZANG Jian,et al.Current situation and development on preparation of high purity graphite[J].Yunnan Metallurgy,2011,40(1):48-51.
[2]
蔡绍勤,李昌世.高纯金属和半导体材料分析[M].北京:冶金工业出版社,1995:328-329.
[3]
钟琦,谢刚,愈小花,等.高纯石墨生产工艺技术的研究[J].炭素技术,2012,31(4): B13-B16.ZHONG Qi,XIE Gang,YU Xiao-hua,et al.Research on high purity graphite production technology[J].Carbon Techniques,2012,31(4):B13-B16.
[4]
Yukihiro K,Akira N.Determination of trace metal inpurities in graphite powders by acid pressure decomposition and inductively coupled plasma atomic emission spectrumetry[J].Analyst,1993,118:827-830.
[5]
郑国经.电感耦合等离子体原子发射光谱分析仪器与方法的新进展[J].冶金分析,2014,34(11):1-10. ZHENG Guo-jing.New advances in inductively coupled plasma atomic emission spectrometric instruments and methods[J].Metallurgical Analysis,2014,34(11):1-10.
[6]
Kazuo W,Jun I.Determination of impurity elements in graphite by acid decomposition inductively coupled plasma atomic emission spectrometry[J]. Analyst,1996,121: 623-625.
[7]
张爱滨,魏进武,王燕,等.顺序扫描ICP-AES法测定高纯石墨灰分中14种杂质金属元素的方法研究[J].青岛海洋大学学报,2003,33(4):609-614.ZHANG Ai-bin,WEI Jin-wu,WANG Yan,et al.Determination of inpurity elements in high purity graphite ash by equential scan inductively coupled plasma atomic emission spectrometry[J].Periodical of Ocean University of China,2003,33(4):609-614.
[8]
Mitsuyoshi W,Akira N.Determination of impurity elements in high purity graphite by inductively coupled plasma atomic emission spectrometry after microwave decomposition[J]. Analyst,2000,125:1189-1191.
[9]
李存根,黄新平,王丽君,等.电感耦合等离子体原子发射光谱法测定类石墨中磷[J].冶金分析,2009,29(9):52-54.LI Cun-gen,HUANG Xin-ping,WANG Li-jun,et al.Determination of phosphorus in graphite like materials by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2009,29(9): 52-54.
[10]
王干珍,严慧,易晓明.电感耦合等离子体-原子发射光谱法测定石墨中的钙[J].光谱实验室,2011,28(5):2599-2602.WANG Gan-zhen,YAN Hui,YI Xiao-ming. Determination of calcium in graphite by ICP-AES[J]. Chinese Journal of Spectroscopy Laboratory,2011,28(5): 2599-2602.
[11]
葛鹏,王化军,解琳,等.高纯石墨中杂质成分的检测研究[J].矿业工程,2010,30(3):96-99.GE Peng,WANG Hua-jun,XIE Lin,et al.Study on deteation of impurity composition in high-purity graphite[J].Mining and Metallurgical Engineering,2010,30(3):96-99.
[12]
贾静,张英新,童坚,等. ICP-MS法测定高纯石墨中的痕量元素杂质[J].精细化工,2009,26(7):671-674.JIA Jing,ZHANG Ying-xin,TONG Jian,et al.Determination of impurity elements in high purity graphite by inductively coupled plasma-mass spectrometry[J].Fine Chemicals,2009,26(7):671-674.
