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荧光分光光度法测定痕量铌已有报导,其中文献曾报导过少数铌钽精矿样品中铌的测定,但未见广泛应用于各类地质样品中痕量铌的测定。我们在文献的基础上,进一步研究了铌在桑色素(morin)-十六烷三甲基溴化铵(CTMAB)胶束体系的荧光特性,共存元素的干扰及其用阳离子树脂交换分离的条件。实验测得本法检出限为0.27ng/ml,测定限为0.54ng/ml,比文献提高1.9倍;0.5μgNb经11次测定标准偏差为0.0125,变动系数为2.49％;标准加入回收率为:96.00—110.00％。实验结果表明:本法具有简单、灵敏、准确等特点,适合于岩石、土壤、水系沉积物等成分复杂的地质样品中痕量铌的测定。
The determination of trace niobium by fluorescence spectrophotometry has been reported. The literature has reported the determination of niobium in a few samples of niobium-tantalum concentrate, but it has not been widely applied to the determination of trace niobium in various geological samples. Based on the literature, we further studied the fluorescence characteristics of niobium in the morin-CTMAB micellar system, the interference of coexisting elements and the conditions for the exchange and separation with cationic resins . The detection limit of this method was 0.27ng / ml and the limit of determination was 0.54ng / ml, 1.9 times higher than that of the literature. The standard deviation of 0.5μgNb determined by 11th determination was 0.0125 and the coefficient of variation was 2.49%. The standard addition recovery was : 96.00-110.00%. The experimental results show that the method is simple, sensitive and accurate. It is suitable for the determination of trace niobium in geological samples with complex compositions such as rocks, soil and sediments.