流动注射微柱预富集等离子体原子发射光谱法测定高纯锌中痕量稀土元素

本文报道以DCS-偶氮胂固定于活性炭上作为固定相,用于流动注射微柱预富集体系和等离子体原子发射光谱测定痕量稀土元素.测定了吸附材料对稀土元素的静态和动态吸附容量,分别达几十和几个mg/g吸附材料;对影响柱预富集的PH、上柱速度、洗脱酸度、柱尺寸等因素进行了详细考察;在优化条件下,富集倍数为10倍左右.对La、Nd、Eu、Gd、Tb、Dy、Ho和 Lu等元素的检出限为 μg/L级,RSD在 1.5％～3.9％之间(n=6,单一稀土浓度0.085 mg/L).该法应用于高纯锌中痕量稀土元素的测定,试样加入回收率在 84.5％～97.6％之间,分析结果满意.

Determination of Trace Rare Earth Elements in High Purity Zinc by Inductively Coupled Plasma-Atomic Emission Spectrometry With Micro-column Preconcentration in a Flow Injection System

The DCS-arsenazo is used as a complex reagent in a micro-column preconcen-tration system for the determination of trace rare earth elements (REEs) by ICP-AES. The static and dynamic adsorption capacity of the immobilized material to REEs is determined respectively. The several influencing parameters such as pH, flow rate of sample, elueiit acidity, amount of the absorbent are studied and optimized. Enrichment factor is about 10. The detection limit of the method is at ng/mL level with RSD of 1. 5%-3. 9%(n = 6). The method proposed has been applied to the determination of trace REEs in high purity zinc with satisfactory results.