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作 者:温世杰 陈绯宇 WEN Shijie;CHEN Feiyu(Jiangxi South Rare Earth High Tech Limited by Share Ltd.,Ganzhou 341000,Jiangxi,China)
机构地区:[1]江西南方稀土高技术股份有限公司,江西赣州341000
出 处:《有色金属科学与工程》2021年第6期123-130,共8页Nonferrous Metals Science and Engineering
基 金:国家标准化管理委员会资助项目(国标委发[2020(6)])。
摘 要:采用电感耦合等离子体发射光谱法(ICP-OES)测定镧铁合金中铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钇稀土杂质元素。镧铁合金试料在硝酸介质中,以近似基体匹配法校正基体对测定的影响,直接以氩等离子体光源激发,用标准曲线法进行光谱测定。为选择合适的分析线,先根据光谱波长表预选几条强度大,激发电位低的谱线,然后对此谱线进行轮廓扫描,从而选出一条背景平坦,信背比大,基体及共存元素干扰少或无干扰的谱线作为分析线。用基体匹配法配制标准溶液,根据产品标准XB/T 407—2020指标,以铁(85%)与镧(15%)配制成混合基体,配制6个系列标准溶液进行曲线绘制。该方法适用于铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥、钇含量在0.005%~0.25%的分析测定。方法的相对标准偏差(n=11)在0.74%~2.58%之间,用标准加入法对方法的回收率进行试验,测得回收率在91.75%与107.75%之间,能满足产品测定要求。The rare earth impurities of Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Y in lanthanum-iron alloy were determined by inductively coupled plasma optical emission spectrometry(ICP-OES).The effect of matrix on the determination of lanthanum-iron alloy in nitric acid medium was corrected by approximate matrix matching method,and the spectrum was determined by standard curve method.The analytic lines were selected by profile scanning method to screen the optimum lines with flat background,high signal to background ratio and low matrix interference from several pre-selected lines.The standard solution was prepared by matrix matching method,according to product standard XB/T 407—2020 index by iron(85%)and lanthanum(15%)and 6 series of standard solutions for curve drawing.The method obtained is suitable to determine Ce,Pr,Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb,Lu,Y contents in the range of 0.005%~0.25%and the RSD is between 0.74%and 2.58%(n=11).Standard addition method was applied for accuracy test and the recovery rate is in the range of 91.75%~107.75%.
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