电感耦合等离子体原子发射光谱法测定高含量碳化硅表面6种杂质成分

摘要

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 cou-pled plasma atomic emission spectrometry(ICP-AES).Consequently the analysis method of impurity com-ponents(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 lim-its were in range of 0.000042%-0.00064%(mass fraction).The proposed method was applied for the de-termination of iron,aluminum,calcium,magnesium,potassium oxide and sodium oxide on surface of sili-con 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 ox-ide 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.%碳化硅是应用最广泛、最经济的一种耐火原料,由于碳化硅贸易活跃,需要对表面杂质成分进行快速、准确的测定.样品采用氢氟酸、硝酸溶解,高氯酸冒烟至近干,再使用盐酸溶解可溶性盐类,通过过滤使得被测成分与碳化硅分离,选择Fe 259.939 nm、Al 394.401 nm、Ca 317.933 nm、M g 285.213 nm、K 766.490 nm、Na 589.592 nm为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铁、铝、钙、镁、氧化钾、氧化钠,从而建立了使用 ICP-A ES测定高含量碳化硅表面铁、铝、钙、镁、氧化钾、氧化钠等杂质成分的方法.铁在0.020% ~0.50%,铝、钙在0.020% ~0.20%,镁、氧化钾、氧化钠在0.0020% ~0.020% 范围内校准曲线呈线性,线性相关系数均不小于0.9998.方法检出限为0.000042% ~0.00064%(质量分数).实验方法用于测定碳化硅样品表面铁、铝、钙、镁、氧化钾、氧化钠,结果的相对标准偏差(RSD,n=10)为1.9% ~9.5%.按照实验方法测定碳化硅样品表面铁、铝、钙、镁、氧化钾、氧化钠,测定值与国家标准方法的测定结果相吻合.