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流动注射离子交换分离分光光度法测定煤矸石中痕量钪
Determination of Trace Scandium in Coal Gangue by Spectrophotometry after Separation and Preconcentration with Flow Injection Ion Exchange
【摘要】 采用流动注射技术进行痕量钪的离子交换分离富集 ,在 0 .40mol·L- 1 HBr介质中 ,Sc3+ 与Br- 形成络阴离子 ,被离子交换树脂交换富集 ,用 0 .2 5mol·L- 1 HNO3 1 5 %硫脲溶液洗脱 ,用对氯偶氮氯膦 (CPA pCl)分光光度法测定。有色络合物的最大吸收波长为 615nm ,钪的质量浓度在 0~ 10 0 0 μg·L- 1 范围内符合比耳定律 ,方法的检出限为 1.2 μg·L- 1 。经分离后 ,钪的测定灵敏度可提高数倍 ,大量共存离子不干扰钪的测定。该法已应用于煤矸石痕量钪的测定
【Abstract】 A method for the determination of trace scandium by chlorophosphonazo-pCl (CPA-pCl) spectrophotometry after separation and preconcentration with flow injection ion exchange was studied. In the medium of 0.40 mol·L-1 hydrobromic acid, Sc3+ reacts with Br- to form an anion complex which is then adsorbed on the column of alkali anion exchange resin. The anion complex is desorbed from the column with solution of 0.25 mol·L-1 nitric acid-1.5% thiourea and it reacts with CPA-pCl to form a color complex for spectrophotometric determination. The maximum absorption wavelength is 615 nm. Beer′s law is obeyed in the concentration range of 0~1000 μg·L-1 for scandium (Ⅲ), and the detection limit of the method is 1.2 μg·L-1. The sensitivity for the determination of scandium can be improved for several times, and a lot of co-ions do not disturb the determination of scandium after separation and preconcentration. The method has been applied to the determination of trace scandium in coal gangue with satisfactory results.
【Key words】 flow injection; ion exchange; spectrophotometry; chlorophosphonazo-pCl; scandium;
- 【文献出处】 稀有金属 ,Chinese Journal of Rare Metals , 编辑部邮箱 ,2005年01期
- 【分类号】TD849.5
- 【被引频次】10
- 【下载频次】140