阳离子交换树脂微柱分离测定矿石中锆的研究

建立了HD-8阳离子交换树脂微色谱柱分离富集矿石中锆的方法。研究了上柱酸度、淋洗液、洗脱液、干扰离子等对锆的吸附性能的影响。结果表明,上柱最佳酸度0.5~2 mol/L HCl、淋洗液1 mol/L HCl、洗脱液1 mol/L H2SO4,锆的吸附与洗脱效果最好。选用邻氯苯基荧光酮为显色剂,直接在硫酸介质中显色,胶束增溶光度法测定,操作简便,灵敏度高,选择性好。树脂的吸附容量为81.4 mg/g。与常规柱相比,微色谱柱吸附后,洗脱体积减少了16倍,柱效高,分离速度快,试剂用量少,灵敏度高。该方法可以用于实际矿石的分离测定,经标准值验证,测定值与标准值相近,多次平行测定后,方法的相对标准偏差为1.9%~2.7%,说明此法可用于分析实际样品。

Determination of Trace Amount of Zirconium in Ores Using Micro-chromatographic Column Packed with Cation Exchange Resins

A method for separation and preconcentration of trace zirconium in ores by a micro-column packed with HD-8 cation exchange resins was established.Effects of acidity,washing liquor,eluent and interfered ions on adsorption properties were studied.Results indicated that zirconium has the best adsorption and elution under the conditions of the adsorption acidity,washing liquor and eluent as 0.5~2 mol/L HCl,1 mol/L HCl and 1 mol/L H2SO4.O-chlorophenyl fluorone was used as chromogenic reagent and zirconium was determined by micellar solubilization spectrophotometry.The adsorption capacity of HD-8 resins was 81.4 mg/g for Zr.Compared with general column,the micro-column has advantages of high column efficiency,quick separation speed,a small amount of reagent and good separation efficiency.The method was applied to analyze Zr in ores and the measured values were close to standard values,with RSD as 1.9%~2.7%.The proposed method can be used to determine Zr in real samples.