Elution Behavior of Pd(II) - Isonitrosoethylacetoacetate Imine Chelates by Reversed Phase High Performance liquid Chromatography

역상 액체 크로마토그래피에 의한 Pd(II) - Isonitrosoethylacetoacetate Imine 유도체 킬레이트들의 용리 거동

  • Kim, In-Whan (Department of Chemistry Education, Taegu University) ;
  • Shin, Han-Chul (Department of Chemistry Education, Taegu University) ;
  • Lee, Man-Ho (Department of Industrial Chemistry, Kyungpook National University) ;
  • Yoon, Tai-Kun (Calculation and CRM Center, Korea Research Institute of Standards and Science) ;
  • Kang, Chang-Hee (Department of Chemistry, Cheju National University) ;
  • Lee, Won (Department of Chemistry, Kyunghee University)
  • 김인환 (대구대학교 사범대학 화학교육과) ;
  • 신한철 (대구대학교 사범대학 화학교육과) ;
  • 이만호 (경북대학교 공과대학 공업화학과) ;
  • 윤태건 (한국표준과학연구원 검교정 CRM 센타) ;
  • 강창희 (제주대학교 자연과학대학 화학과) ;
  • 이원 (경희대학교 문리과대학 화학과)
  • Received : 1992.10.26
  • Published : 1992.12.25

Abstract

Liquid Chromatographic behavior of Pd(II) in Isonitrosoethylacetoacetate lmine, $Pd(IEAA-NR)_2$ (R=H, $CH_3$, $C_2H_5$, $n-C_3H_7$, $C_6H_5-CH_2$, $n-C_4H_9$) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of $Pd(IEAA-NR)_2$ chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It wass found that metal chelates were properly eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the logarithm of capacity factor(k') on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extration distribution ratio($D_c$) in methanol-water/n-alkane extration system was investigated. Both kinds of dependence are linear, which susggests that the retention of the electroneutral metal chelate is largely due to the solvophobic effect. Standard adsorption enthalpy changes (${\Delta}H^{\circ}$) and standard adsorption entropy changes (${\Delta}S^{\circ}$) of Pd(II) Isonitrosoethylacetoacetate imine chelates on Micropak MCH-5 column were calculated by measuring capacity factor with changing temperature of the column.

Keywords

Reversed-phase liquid chromatography;Pd (II)-Isonitrosoethylacetoacetate imine chelates