Abstract: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 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 ketoxime 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 wavelength 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 chromatographic 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, respectively. The content of aldoxime and ketoxime in LIX984N copper 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%.
刘本发, 刘海波. 高效液相色谱法测定湿法冶金LIX984N铜萃取剂中醛肟和酮肟[J]. 冶金分析, 2016, 36(10): 62-68.
LIU Ben-fa, LIU Hai-bo. Determination of aldoxime and ketoxime in hydroxyoxime copper extractant of hydrometallurgy LIX984N by high performance liquid chromatography. , 2016, 36(10): 62-68.
裴世红,谢瑞丽,金猛,等.湿法炼铜常用的萃取剂[J].当代化工,2009,38(1):78-82.PEI Shi-hong,XIE Rui-li,JIN Meng,et al.Extractants in copper hydrometallurgy[J].Contemporary Chemical Industry,2009,38(1):78-82.
[2]
彭钦华,陈述一,李绍民,等.铜萃取剂BK992和LIX984的性能研究[J].有色冶金:冶炼部分,2002(5):18-20.PENG Qin-hua,CHEN Shu-yi,LI Shao-min,et al.Properties study on copper extractant BK992 and LIX984[J].Nonferrous Metals:Extractive Metallurgy,2002(5):18-20.
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,2001,19(2):503-504.REN Xin-rong,SHAO Ke-sheng,TANG Xiao-yan.Determination of salicylic acid and its hydroxylated products using high performance liquid chromatography and fluorescence detection[J].Chinese Journal of Chromatography,2001,19(2):503-504.
[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,2011,24(z2):60-62.ZHANG Li.Determination of aldehydes and ketones in air pollutants by HPLC[J].Environmental Science and Technology,2011,24(z2):60-62.
[6]
安彩秀,刘金巍,王磊.反相高效液相色谱法测定水中醛酮类化合物[J].分析试验室(Chinese Journal of Analysis Laboratory),2010,29(s1):371-374.
[7]
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,2009,29(2):188-192.JI Ran,RUAN Hong.Determination of 17 aldehydes and ketones in air by HPLC[J].Environmental Protection of Chemical Industry,2009,29(2):188-192.
周志军,刘应希,曾俊宁.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,2005,22(4):297-299.ZHOU Zhi-jun,LIU Ying-xi,ZENG Jun-ning.Determination of 13 kinds of aldehyde and ketone pollutants of indoor air by HPLC at one time[J].Journal of Environment and Health,2005,22(4):297-299.
[11]
曾红艳,段正康,陈韩志,等.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,2011,39(3):382-386.ZENG Hong-yan,DUAN Zheng-kang,CHEN Han-zhi,et al.Determination of 2,6-dimethyl-gamma-pyrone and acetylacetone by high performance liquid chromatography[J].Chinese Journal of Analyical Chemistry,2011,39(3):382-386.
[12]
刘文光,李云芝,石瑞常,等.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,2009,37(32):15667-15668.LIU Wen-guang,LI Yun-zhi,SHI Rui-chang,et al.Determination on lisothiazolonesolution content for silkworm by RP-HPLC[J].Journal of Anhui Agricultural Sciences,2009,37(32):15667-15668.
[13]
李喆宇,张春然,王宇驰,等.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,2013,38(2):125-129.LI Zhe-yu,ZHANG Chun-ran,WANG Yu-chi,et al.Determination of related substances and content of paliperidone by HPLC[J].Chinese Journal of Antibiotics,2013,38(2):125-129.
[14]
陈文利,欧阳贻德,李蕾,等.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,2003,19(3):297-298.CHEN Wen-Li,OUYANG Yi-de,LI Lei,et al.Determination of salicylic acid and its correlation compound using high performance liquid chromatography[J].Journal of Analyical Science,2003,19(3):297-298.
[15]
于林华.新型羟肟类萃取剂的分子设计合成与性能研究[D].南宁:广西大学,2014.
[16]
LIU Xiao-rong.Degradation of Lix984N and its effect on interfacial emulsion[J].Journal of Central South University of Technology(English Edition),2006,13(6):668-672.
[17]
邹汉法,张玉峰,卢佩章.高效液相色谱法[M].北京:科学出版社,1998:361-390.
[18]
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.CHENG Hong-da,LI Tong,ZHANG Wei-bing. Influence of temperature on separation behaviors of HPLC[J].Modern Scientific Instruments,2006(5):74-78.