CAJ | 학술논문

基于电感耦合等离子体四极杆质谱仪进行Nd_2O_3中稀土杂质测定,着重研究了碰撞反应池技术(CCT)用于基体Nd氧化物和氢氧化物干扰离子的消除.研究表明,以10% O_2-10% Ar-80% He为碰撞反应气,保持反应气流速为0.1 mL/min,并通过调谐仪器参数,获得~(159)Tb, ~(165)Ho, ~(163)Dy 同位素的~(175)TbO, ~(179)DyO和~(181)HoO出现强氧化物峰,通过对这些氧化物离子进行检测而实现Tb, Dy, Ho的定量分析.在优化的条件下,基体导致的氧化物和氢氧化物质谱干扰可降低25～70倍.研究了CCT模式下不同内标元素用于基体效应的校正.结果表明,Re的校正效果最佳.其余La, Ce, Pr,Sm, Eu, Gd, Er, Tm, Yb和Lu等元素采用常规模式测定,其中Pr的测定采用高分辨以消除基体Nd前沿峰干扰.结合干扰系数校正,所建立的方法适用于99.999% Nd_2O_3的纯度分析,RSD小于5%, 加入回收率令人满意.
기우전감우합등리자체사겁간질보의진행Nd_2O_3중희토잡질측정,착중연구료팽당반응지기술(CCT)용우기체Nd양화물화경양화물간우리자적소제.연구표명,이10% O_2-10% Ar-80% He위팽당반응기,보지반응기류속위0.1 mL/min,병통과조해의기삼수,획득~(159)Tb, ~(165)Ho, ~(163)Dy 동위소적~(175)TbO, ~(179)DyO화~(181)HoO출현강양화물봉,통과대저사양화물리자진행검측이실현Tb, Dy, Ho적정량분석.재우화적조건하,기체도치적양화물화경양화물질보간우가강저25～70배.연구료CCT모식하불동내표원소용우기체효응적교정.결과표명,Re적교정효과최가.기여La, Ce, Pr,Sm, Eu, Gd, Er, Tm, Yb화Lu등원소채용상규모식측정,기중Pr적측정채용고분변이소제기체Nd전연봉간우.결합간우계수교정,소건립적방법괄용우99.999% Nd_2O_3적순도분석,RSD소우5%, 가입회수솔령인만의.
A method for the determination of impurities in high pure Nd_2O_3 employing inductively coupled plasma mass spectrometry(ICP-MS) was established, and emphasise was put on the elimination of matrix induced NdO~+ and NdOH~+ spectral interferences using cell collision technology(CCT). Using 10% O_2-10% Ar-80% He as the reaction/collision gas and with proper adjustment of the instrumental parameters, ~(159)Tb,~(165)Ho,~(163)Dy could be quantified at ~(175)TbO,~(179)DyO and ~(181)HoO respectively, while the matrix induced NdO~+ and NdOH~+ spectral interferences could be reduced by 25-70 folds. In addition, different elements were tested as internal standards for matrix effect correction under the CCT mode, and it was found that Re was best. Other impurities including La, Ce, Sm, Eu, Gd, Er, Tm, Yb and Lu were detected under conventional mode, except that Pr was detected under high instrumental resolution mode to eliminate peak tailing interference from Nd. In combination with mathematic correction, the established method can be applied for the determination of impurities in 99.999% Nd_2O_3 products with satisfactory RSDs and recoveries.