高效液相色谱法测定湿法冶金LIX984N铜萃取剂中醛肟和酮肟

Determination of aldoxime and ketoxime in hydroxyoxime copper extractant of hydrometallurgy LIX984N by high performance liquid chromatography

醛肟和酮肟的含量直接决定其羟肟类铜萃取剂(以下简称铜萃取剂)的萃取性能状况,因此建立简便可行的测定铜萃取剂中醛肟和酮肟含量的方法意义重大。实验在无醛肟和酮肟标准样品的前提下,选取LIX984N为原料,采用液相色谱仪以半制备方法制备了纯醛肟和酮肟,并以此为标准品,建立了测定湿法冶金LIX984N铜萃取剂产品中醛肟和酮肟的高效液相色谱(HPLC)分析方法。优化后的液相色谱仪操作条件如下:Chromatorex(迪玛)C18(300mm×30mm×10μm)反相柱为半制备柱,ChromatorexC18(250mm×4.6mm×5μm)反相柱为分析柱,甲醇为流动相,流动相流速为1.0mL/min,柱温为室温,紫外检测器波长为254nm。实验表明,醛肟和酮肟均在质量浓度为0.4μg/mL^1.50mg/mL范围内与其对应的色谱峰面积呈良好的线性关系,相关系数均大于0.998。醛肟和酮肟的方法检出限分别为0.12和0.15μg/mL,测定下限分别为0.4和0.5μg/mL。按照实验方法对LIX984N铜萃取剂样品中醛肟和酮肟进行测定,结果的相对标准偏差(RSD,n=5)均小于0.5%,加标回收率为94%~129%。

The content of aldoxime and ketoxime directly decided the extraction performance of hydroxyoxime copper extractants（hereinafter referred to as copper extractants）.Therefore,it was meaningful to establish a simple and feasible method for the determination of aldoxime and ketoxime contents in LIX984 Ncopper extractants.Since there were no certified reference materials of aldoxime and ketoxime,the pure aldoxime and ketoxime were prepared by semi-preparation method of liquid chromatography using LIX984 Nas material,which was then used as standard sample.The analysis method of aldoxime and ketoxime in hydrometallurgy LIX984 N copper extractants by high performance liquid chromatography（HPLC）was established.The optimized HPLC parameters were as follows：the Chromatorex C18（300mm×30mm×10μm）reversed-phase column was used as semi-preparation column;the Chromatorex C18（250mm×4.6mm×5μm）reversed-phase column was used as analytical column;the mobile phase was methanol with flow velocity of 1.0 mL/min;the column temperature was room temperature;the wavelength of ultraviolet detector was 254 nm.The results showed that the mass concentration of aldoxime and ketoxime in range of 0.4μg/mL-1.50mg/mL had good linear relationship to the corresponding chromatographic peak area.The correlation coefficients were higher than 0.998.The detection limit of aldoxime and ketoxime was 0.12 and 0.15μg/mL,and the low limit of determination was 0.4and 0.5μg/mL,respectively.The content of aldoxime and ketoxime in LIX984 Ncopper extractant samples was determined according to the experimental method.The relative standard deviations（RSD,n=5）were less than 0.5%.The recoveries were between 94% and 129%.