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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。
A method for separation and enrichment of zirconium in ore by HD-8 cation exchange resin micro-chromatographic column was established. The effects of acidity, eluent, eluent and interfering ions on the adsorption of zirconium were studied. The results showed that the optimal acidity was 0.5 ~ 2 mol / L HCl, 1 mol / L HCl, 1 mol / L H2SO4 and the best adsorption and elution of zirconium. The o-chlorophenylfluorone was chosen as the chromogenic reagent, which was directly colorized in sulfuric acid medium and measured by micellar solubilization spectrophotometry. The method was simple, sensitive, and selective. Resin adsorption capacity of 81.4 mg / g. Compared with the conventional column, the elution volume of the micro-column after adsorption is reduced by 16 times, the column efficiency is high, the separation speed is fast, the amount of the reagent is small, and the sensitivity is high. The method can be used for the separation and determination of the actual ore. The standard values of the method are validated. The measured values are close to the standard values. The relative standard deviations of the method are 1.9% -2.7% after multiple parallel determinations, indicating that this method can be used to analyze the actual samples.