电感耦合等离子体原子发射光谱法测定镝铁电解粉尘中15种稀土元素

摘要

用硝酸和氢氟酸溶解试样,高氯酸冒烟除氟,在硝酸介质中用电感耦合等离子体原子发射光谱法(ICP-AES)测定了镝铁电解粉尘中La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Lu、Y15种稀土元素.为了提高高含量元素的测定准确度,在测定基体元素Dy时,采用铟作内标;为了消除基体效应对稀土杂质元素测定的影响,采用基体匹配的校准曲线.镝铁电解粉尘中铁含量很低(铁的质量分数不超过1％),对测定没有影响.实验方法测定了一镝铁电解粉尘样品,结果表明,La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Ho、Er、Tm、Yb、Lu和Y 14个稀土杂质元素测定值与ICP-MS的测定值基本一致,镝和14个稀土元素的合量与重量法测得的稀土总量吻合.%The sample was dissolved in nitric acid and hydrofluoric acid.The fluorine was removed by perchloric acid fuming.Fifteen rare earth elements (La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu and Y) in Dy-Fe electrolysis dust were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES).In order to improve the determination accuracy of high content elements,indium was used as internal standard during the determination of matrix element Dy.The calibration curves with matrix matching were used to eliminate the matrix effect on determination of rare earth elements.The content of iron in Dy-Fe electrolysis dust was very low (the mass fraction of iron was less than 1 ％),so it had no influence on the determination.The proposed method was applied to the determination of one Dy-Fe electrolysis dust.The results showed that the determination results of fourteen rare earth impurity elements (La,Ce,Pr,Nd,Sm,Eu,Gd,Tb,Ho,Er,Tm,Yb,Lu and Y) were consistent with those obtained by ICP-MS.The total content of dysprosium and fourteen rare earth impurity elements was consistent with that obtained by gravimetric method.