固相萃取-液相色谱联用检测镍电解液中的有机磷萃取剂  

Determination of organophosphorus extracting agent in nickel electrolyte by solid phase extraction-high performance liquid chromatography

作　　者：李亦婧[1] 周通[2] 卢建波[2] 郑军福[2] 陈自江[2] 郭勇[1] 

机构地区：[1]中国科学院兰州化学物理研究所,甘肃兰州730030 [2]金川集团股份有限公司,甘肃金昌737100

出　　处：《现代化工》2015年第12期162-164,166,共4页Modern Chemical Industry

基　　金：甘肃省科技重大专项项目(143GKDC012)

摘　　要：建立了固相萃取（SPE）-高效液相色谱（HPLC）联用测定镍电解液中P204、P507和C272的分析方法。优化了萃取溶剂、SPE柱填料类型、SPE淋洗溶剂等前处理条件以及HPLC检测条件。采用C18填料的SPE柱进行固相萃取，检测方法的线性范围为0．1～100mg／L；检出限为0．02mg／L。加标样品回收率为68．6％～83．5％，RSD为5．5％～9．2％。该方法灵敏度高，重复性良好，操作简便快速，适用于镍电解液中3种有机磷萃取剂的检测。A solid phase extraction （SPE） coupled with high performance liquid chromatographic （HPLC） method is developed for the determination of P204, P507 and C272 in nickel electrolyte. The effects of extraction solvent, the type of SPE column, elution solvents and corresponding instrumental conditions for HPLC detection are optimized in detail. The sample is enriched and purified through a C18 solid-phase extraction column. The liner rang is from 10 to 100 mg/ L. the detection limit is 0.02 mg/L. The average recovery is from 68. 6% -83.5% and the RSD is from 5. 5% -9.2%. The method shows the advantages of simplicity, rapidness and sensitivity, which is suitable for the determination of the amounts of organophosphorus extracting agent in nickel electrolyte.

关 键 词：固相萃取 高效液相色谱 萃取剂 电解液 

分 类 号：O657.72[理学—分析化学]