Preparation and characterization of immobilized 8-hydroxyquinoline for chromatographic application

크로마토그래피용 고정화 8-hydroxyquinoline의 제조 및 특성분석

  • Received : 1999.11.13
  • Published : 2000.02.25

Abstract

The 8-hydroxyquinoline derivative of silica gel has been prepared through the 5 step reaction. We carried out infrared as well as nuclear magnetic resonance spectrometric characterization of products taken from each step of reaction. IR study of bare silica gel showed free and hydrogen bonded hydroxyl. From the 1st step reaction, we observed IR bands for N-H and C-H as well as NMR peaks for three methylene carbons in APTS group. From the 2nd step, we observed IR bands for carbonyl, nitro and aromatic carbon group with NMR peaks for aliphatic, aromatic and carbonyl carbons. The reduction of $NO_2$ group to $NH_2$ group is confirmed by IR and NMR from 3rd step reaction. In the last step, the immobilization of 8-quinolinol is confirmed by disappearance of $N{\equiv}N$ IR peak observed in 4th step.

Keywords

8-hydroxyquinoline;HPLC;DRiFfS;C-13 CPIMAS NMR

References

  1. J. Coll. and Interface Sci. v.74 J.L.M. van de Venne;J.P.M. Rindt;G.J.m.M. Coenen
  2. Anal. Chim. Acta v.70 F. Vernon;H. Eccles
  3. Anal. Chim. Acta v.70 J.R. Parrish;R. Stevenson
  4. Talanta v.32 D.K. Ryan;J.H. Weber
  5. Chromatographia v.22 K.H. Faltynski;J.R. Jezorek
  6. Anal. Chim. Acta. v.186 C.H. Risner;J.R. Jezorek
  7. Anal. Chim. Acta v.363 Y. Sohrin;S. Iwamoto;S. Akiyama;T. Fujita;T, Kugii;H. Obata;M. Matsui
  8. Anal. Chem. v.46 K.F. Sugawara;H.H. Weetall;G.D. Schucker
  9. Anal. Chem. v.60 A.K. Kolstad;P.Y.T. Chow;F.F. Cantwell
  10. Chromatographia v.45 D. Agbaba;A. Mihajlovic;P. Beljanski;D. Zivanov-Stakic;S. Vladimirov
  11. Synthic Metals v.85 F. Papadimitrakopoulos;X.M. Zhang
  12. J. Chromatogr. v.76 J.M. Hill
  13. Anal. Chim. Acta v.371 R.H. Zhu;W.T. Kok
  14. Anal. Chim. Acta v.160 F. Malamas;M. Bengtsson;G. Johansson
  15. Anal. Chem. v.55 M.A. Marshall;H.O. Mottola
  16. Anal. Chem. v.51 J.R. Jezorek;H. Freiser
  17. Anal. Chem. v.60 P.Y.T. Chow;F.F. Cantwell
  18. Anal. Chem. v.57 M.A. Marshall;H.A. Mottola
  19. Talanta v.32 J.R. Jezorek;K.H. Faltynski;L.G. Blackburn;P.J. Henderson;H. Darlene Medina
  20. Anal. Chem. v.57 M.A. Marshall;H.A. Mottola
  21. J. Inorg. Nucl, Chem. v.40 F. Vernon;K.M. Nyo
  22. Anal. Chem v.54 J.R. Parrish
  23. Chem. v.115 B.Berg;J. Prakd