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针对实验室现有的便携式液体阴极辉光放电光谱仪,重新设计了一种内嵌式液体阴极,其制作简单,采用蠕动泵直接进样,简化了便携式液体阴极辉光放电光谱仪的进样系统;刚玉阴极外管具有润湿作用,使得蠕动泵进样时阴极管口液面的起伏非常小,不会形成液滴,保证了放电的稳定、连续;可分析含低浓度HF的样品溶液,为简化锂辉石样品的前处理过程奠定理论基础,非常适用于野外现场分析锂辉石样品。选择Li的分析谱线波长为670.78 nm,利用新设计的内嵌式液体阴极,以3个锂矿石标样和11个锂辉石样品为研究对象,建立了锂辉石样品中Li的快速分析方法。在最佳工作条件下测得Li的检出限为4.6 ng/m L,方法的精密度(RSD)<3%。研究表明,采用标准加入法获得的锂矿石标样和锂辉石样品的分析结果与ICP-M S的测量值基本吻合,相对误差均小于10%,满足野外现场快速分析锂辉石样品中Li含量的需要。
Aiming at the existing portable liquid cathode glow discharge spectrometer in the laboratory, a new type of embedded liquid cathode is redesigned to make simple manufacture. The direct injection with peristaltic pump simplifies the injection system of portable liquid cathode glow discharge spectrometer. Corundum cathode outer tube has a wetting effect, making the peristaltic pump sample when the cathode nozzle level fluctuation is very small, does not form droplets, to ensure a stable discharge, continuous; can be analyzed with low concentration of HF sample solution, as Simplifies the pretreatment of spodumene samples laid the theoretical foundation, ideal for field analysis of spodumene samples. The wavelength of the analytical line of Li was selected to be 670.78 nm. A rapid analysis of Li in spodumene samples was established by using a newly designed embedded liquid cathode, taking three lithium ore samples and 11 spodumene samples as the research objects method. The detection limit of Li was 4.6 ng / m L under the best working conditions, and the precision (RSD) of the method was less than 3%. The results show that the analytical results of standard samples of lithium ore and spodumene obtained by standard addition method are basically consistent with the measured values of ICP-MS, the relative errors are less than 10%, which can meet the requirements of rapid field analysis of Li Content needs.