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(300 mm ×30 mm ×10μm)反相柱为半制备柱,ChromatorexC18(250 mm ×4.6 mm ×5μm)反相柱为分析柱,甲醇为流动相,流动相流速为1.0 m L/min ,柱温为室温,紫外检测器波长为254 nm。实验表明,醛肟和酮肟均在质量浓度为0.4μg/mL~1.50 mg/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 mean‐ingful to establish a simple and feasible method for the determination of aldoxime and ketoxime contents in LIX984N copper 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 LIX984N as material ,which was then used as standard sample .The analysis method of aldoxime and ke‐toxime in hydrometallurgy LIX984N copper extractants by high performance liquid chromatography (HPLC) was established .The optimized HPLC parameters were as follows :the Chromatorex C18 (300 mm × 30 mm × 10 μm) reversed‐phase column was used as semi‐preparation column ;the Chromatorex C18 (250 mm × 4.6 mm × 5 μm) 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 wave‐length of ultraviolet detector was 254 nm .The results showed that the mass concentration of aldoxime and ketoxime in range of 0.4 μg/mL‐1.50 mg/mL had good linear relationship to the corresponding chromato‐graphic peak area .The correlation coefficients were higher than 0.998 .The detection limit of aldoxime and ketoxime was 0.12 and 0.15 μg/mL ,and the low limit of determination was 0.4 and 0.5 μg/mL ,respec‐tively .The content of aldoxime and ketoxime in LIX984N copper extractant samples was determined ac‐cording to the experimental method .The relative standard deviations (RSD ,n=5) were less than 0.5% . The recoveries were between 94% and 129% .
参考文献
[1] | 裴世红;谢瑞丽;金猛;高枫;秦栋.湿法炼铜常用的铜萃取剂[J].当代化工,2009(1):78-82. |
[2] | 彭钦华;陈述一;李绍民;阳光.铜萃取剂BK992和LIX984的性能研究[J].有色金属(冶炼部分),2002(5):18-20. |
[3] | 黄荣华;张捷.香加皮中4-甲氧基水杨醛含量测定方法的改进[J].西北药学杂志,2008(3):149-151. |
[4] | 任信荣;邵可声;唐孝炎.高效液相色谱法测定水杨酸及其羟基化产物[J].色谱,2001(2):191-192. |
[5] | 张丽.高效液相色谱法分析空气污染物中的醛和酮[J].环境科技,2011(z2):60-62. |
[6] | 纪然;阮虹.液相色谱法测定空气中17种醛酮类化合物[J].化工环保,2009(2):188-192. |
[7] | Waters公司北京实验室.利用Waters Sep-Pak小柱提取空气及饮用水中的甲醛及其它醛酮类污染物[J].环境化学,2001(03):297-298. |
[8] | 周志军;刘应希;曾俊宁;李莹;杨培慧;冯德雄.空气中13种醛酮类有机污染物的高效液相色谱同时测定法[J].环境与健康杂志,2005(4):297-299. |
[9] | 曾红艳;段正康;陈韩志;曾志丁;罗爱文.高效液相色谱法测定2,6-二甲基吡喃酮和乙酰丙酮的含量[J].分析化学,2011(3):382-386. |
[10] | 刘文光;李云芝;石瑞常;胡自江;衣葵花.高效液相色谱法测定蚕用异噻唑啉酮溶液含量[J].安徽农业科学,2009(32):15667-15668. |
[11] | 李喆宇;张春然;王宇驰;邓晶晶;唐克慧.高效液相色谱法测定帕潘立酮的含量及有关物质[J].中国抗生素杂志,2013(2):125-129. |
[12] | 陈文利;欧阳贻德;李蕾;陈中.高效液相色谱法测定废水中水杨酸及相关物质的含量[J].分析科学学报,2003(3):297-298. |
[13] | 于林华 .新型羟肟类萃取剂的分子设计合成与性能研究[D].广西大学,2014. |
[14] | LIU Xiao-rong;QIU Guan-zhou;HU Yue-hua.Degradation of Lix984N and its effect on interfacial emulsion[J].中南工业大学学报(英文版),2006(06):668-672. |
[15] | 成洪达;李彤;张维冰.温度对高效液相色谱分离性能的影响[J].现代科学仪器,2006(5):74-78. |
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