无滤共沉淀富集-等离子体原子发射光谱法测定痕量稀土元素  

Inductively coupled plasma atomic emission spectrometric determination of trace rare earths with on-line fillerless coprecipitation

作　　者：富玉[1] 刘金霞[2] 王彦芬[1] 黄志荣[1] 

机构地区：[1]南开大学化学系 [2]郑州大学化学系,郑州450001

出　　处：《分析试验室》2007年第3期91-94,共4页Chinese Journal of Analysis Laboratory

摘　　要：以编结反应器（KR）作为反应场所，用NH3～NH4NO3缓冲溶液在线沉淀、富集，电感耦合等离子体原子发射光谱法（ICP-AES）检测稀土元素，系统地研究了稀土元素在线沉淀及溶解的最佳条件。实验结果表明：在80℃时，稀土离子与pH9．0的NH3-NH4NO3缓冲溶液在线混合后经2m KR富集120s，用1mol／L HNO3以1．0mL/min流速洗脱时富集效果最好，富集倍数可达52～76倍，进样频率为10／h。同时考察了共存离子的干扰及其消除方法。方法的稀土元素的检出限为0．07～1．23μg/L，精密度RSD在1．7％～4．3％之间（n=6），线性范围2～10μg/L。应用于标准样品中痕量稀土元素的测定，其测定值与标准值吻合。A flow injection （FI） on-line fillerless precipitation-dissolution system was developed for ICP-AES. Using a knotted reactor （KR） as a fillerless collector, on-line precipitation of REEs was achieved by mixing the sample with ammonia buffer solution （pH 9.0）. A serial of the most optimal conditions were obtained. At the same time, the interference of co-existing ions was also studied, and then the dosage of triethanolamine was tested to shelter Fe^3＋ , Mn^2＋ . 2μg/L of individual of REEs was precipitated by on-line mixed with ammonia buffer solution for 120 s, and then was dissolved by 1 mol/L nitric acid and delivered to ICP-AES for determination. An enhancement factor of 52 - 76 was achieved, and sample frequency was 10 h. The detection limits （3a） ranged from 0.07 to 1.23 μg/L and the precision （RSD） was in the range of 1.9 % ～ 4.3 %. Linear calibration was established over the concentration rang of 2 ～ 10μg/L. The analytical results of standard reference material were well inosculated with certified values.

关 键 词：流动注射 编结反应器 等离子体原子发射光谱法 无滤共沉淀 稀土元素 

分 类 号：O657.3[理学—分析化学]