Abstract:Silicon carbide is a kind of most widely used and cost-optimal refractory raw material. Since the trade of silicon carbide is active, it is necessary to rapidly and accurately determine the surface impurity components. The sample was dissolved in hydrofluoric acid and nitric acid. After perchloric acid fuming to almost dryness, the soluble salts were dissolved with hydrochloric acid. The testing components could be separated from silicon carbide by filtration. Fe 259.939nm, Al 394.401nm, Ca 317.933nm, Mg 285.213nm, K 766.490nm and Na 589.592nm were selected as the analytical lines. The contents of iron, aluminum, calcium, magnesium, potassium oxide and sodium oxide were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). Consequently the analysis method of impurity components (iron, aluminum, calcium, magnesium, potassium oxide and sodium oxide) on surface of high-content silicon carbide by ICP-AES was established. The linearity of calibration curves was good for iron (0.020%-0.50%), aluminum and calcium (0.020%-0.20%), magnesium, potassium oxide and sodium oxide (0.0020%-0.020%). The linear correlation coefficients were higher than 0.9998. The detection limits were in range of 0.000042%-0.00064% (mass fraction). The proposed method was applied for the determination of iron, aluminum, calcium, magnesium, potassium oxide and sodium oxide on surface of silicon carbide sample, and the relative standard deviations (RSD, n=10) of measured results were between 1.9% and 9.5%. The contents of iron, aluminum, calcium, magnesium, potassium oxide and sodium oxide on surface of silicon carbide sample were determined according to the experimental method, and the found results were consistent with those obtained by national standard method.
成勇.电感耦合等离子体原子发射光谱法测定高钛型钒渣中铬、钴、镍、镓、钪、锆的含量[J].理化检验:化学分册,2018,54(1):49-54.CHENG Yong.ICP-AES Determination of chromium,cobalt,nickel,gallium,scandium and zirconium in the high titanium vanadium slag[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2018,54(1):49-54.
[2]
黄超冠,蒙义舒,郭焕花,等.过氧化钠碱熔-电感耦合等离子体发射光谱法测定钛铝合金中的铬铁钼硅[J].岩矿测试,2018,37(1):30-35.HUANG Chao-guan,MENG Yi-shu,GUO Huan-hua,et al.Determination of chromium,iron,molybdenum and silicon in Ti-Al alloy by inductively coupled plasma-optical emission spectrometry with sodium peroxide alkali fusion[J].Rock and Mineral Analysis,2018,37(1):30-35.
[3]
宋召霞,高云,张志刚.电感耦合等离子体原子发射光谱(ICP-AES)法测定硫化物矿石中的铜铅锌[J].中国无机分析化学,2017,7(1):35-38.SONG Zhao-xia,GAO Yun,ZHANG Zhi-gang.Determination of copper,lead,and zinc in sulphide ores by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(1):35-38.
[4]
李帆,丁妍,杨春晟,等.电感耦合等离子体原子发射光谱法测定纯铼中痕量的铝、镉、铜、镁、锰和钛[J].理化检验:化学分册,2016,52(10):1223-1226.LI Fan,DING Yan,YANG Chun-sheng,et al.ICP-AES determination of trace amounts of Al,Cd,Cu,Mg,Mn and Ti in pure rhenium[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(10):1223-1226.
[5]
余荣旻,邹龙,刘荣丽,等.电感耦合等离子体原子发射光谱法测定氯化烟尘中的钪铁钛[J].冶金分析,2017,37(11):29-33.YU Rong-min,ZOU Long,LIU Rong-li,et al.Determination of scandium, iron and titanium in chlorination dust by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2017,37(11):29-33.
[6]
柳洪超,鲁毅,刘霞萍,等.等离子体发射光谱法测定碳化硅中的游离总硅含量[J].化学分析计量,2013(6):26-28.LIU Hong-chao,LU Yi,LIU Xia-ping,et al.Determination of total free silicon content in silicon carbide by inductively coupled plasma atomic emission spectrometry[J].Chemical Analysis and Measurement,2013(6):26-28.
[7]
曹海洁,汪玲,王本辉,等.ICP-AES法快速测定氮化硅结合碳化硅材料中氧化物杂质[J].分析试验室,2009(B12):192-194.CAO Hai-jie,WANG Ling,WANG Ben-hui,et al.Rapid determination of oxide impurities in silicon nitride bonded silicon carbide by ICP-AES method[J]. Analytical Laboratory,2009(B12):192-194.
[8]
姚永生.电感耦合等离子体原子发射光谱法测定碳化硅中杂质元素[J].冶金分析,2010,30(7):48-51.YAO Yong-sheng.Determination of impurity elements in silicon carbide by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2010,30(7):48-51.
[9]
Winge R K,Fassle V A,Peterson V J,et al.电感耦合等离子体发射光谱图册[M].北京:中国光学学会光谱学会,1986.