2-(2-噻唑偶氮)-对-甲酚螯合物反相高效液相色谱同時分离测定镍、钴的研究——合金中微量钴和镍的测定  

Simultaneous Separation and Determination of Ni and Co with TAC Chelates by Reversed Phase HPLC

作　　者：李玲颖[1] 桂明德[1] 周志芬[1] 趙亞秋 

机构地区：[1]南开大学化学系,天津300071

出　　处：《分析试验室》1993年第3期27-30,共4页Chinese Journal of Analysis Laboratory

摘　　要：本文研究了2-(2-噻唑偶氮)-对-甲酚(TAC)与镍(Ⅱ)、钴(Ⅱ)螯合物的柱前衍生条件和液相色谱的分离条件。于KYWG-C_(18)柱上,用含有0.03mol/L KH_2PO_4-Na_2HPO_4(pH7.77)和2.5×10^(-4)mol/L TAC的甲醇-四氢呋喃-水(40∶10∶50 V/V)混合液为流动相,流速为1.0mL/min。于580nm处检测。该法用于四种标准合金中镍和钴的测定,回收率在98%～101.5%之间。Ni(Ⅱ)和Co(Ⅱ)的检出限(信噪比为2∶1)分别为0.2ng和1.5ng。建立了同时测定镍,钴的高灵敏、高选择性,快速的HPLC-光度法。The high performance liquid chromatographic separation of Ni(Ⅱ)-and Co(Ⅱ)-2(2-thiazolylazo)-p-cresol (TAC) chelates was investigated. It was shown that the pH value is very critical. Using a KYWG-C_(18) column(φ 4. 6mm×150mm, 10μm) as the stationary phase,and the solution of CH_3OH-tetrahydrofuran-H_2O (40:10: 50V/V) containing 0.03mol/mL KH_2PO_4-Na_2HPO_4 (pH7.77) and TAC (2.5×10^(-4)mol) as the mobile phase,and detecting at 580nm,a good chromatogram with high resolution and sensitivity was obtained. The detection limits of Ni(Ⅱ) and Co(Ⅱ) are 2×10^(-10)g and 1.5× 10^(-9)g (s/n=2) respectively. Ni and Co may be determined in the presence of any other metal without interference in four standard alloys with good accuracy.

关 键 词：高效液相色谱 噻唑偶氮 甲酚 镍 钴 

分 类 号：O613.81[理学—无机化学]