Capillary liquid chromatography: 2. Band broadening due to extracolumn effects

Coutinho, Lincoln F. M.; Lanças, Fernando M.

Palavras-chave: Capillary liquid chromatography, band broadening, extracolumn effects, micro-LC, capillary LC.

Resumo: Band broadening is one of the major factors to be avoided in chromatographic techniques, once it decreases the column efficiency (the number of plates, N) and deteriorates the Resolution (Rs). This effect is particularly critical in capillary liquid chromatography due to the very low volumes, instrumentation, connections and columns employed in this technique. As a part in a series of papers dealing with c-LC, this work describes the major factors responsible for band broadening in chromatography, as well as the ways to minimize it.

---

Referências Bibliográficas

1. Saito M, Hibi K, Ishii D, Takeuchi T. In: Ishii D, editor. Introduction to Microscale High-Performance Liquid Chromatograph. New York: VCH Publisher; 1988.

2. Knox JH. Journal of Chromatographic Science 1977; 15.:352.

3. Ishii D, Asai K, Hibi K, Jonokuchi T, Nagaya M. A study of micro-high-performance liquid chromatography: I. Development of technique for miniaturization of high-performance liquid chromatography. Journal of Chromatography A 1977; 144(2):157-68. http://dx.doi. org/10.1016/S0021-9673(00)99351-8

4. Scott RPW, Simpson CF. Journal of Chromatographic Science 1982; 20:62.

5. Vonk N, Verstraeten WP, Marinissen JW. Journal of Chromatographic Science 1992; 30:296.

6. Chervet JP, Ursem M, Salzmann JP. Instrumental Requirements for Nanoscale Liquid Chromatography. Analytical Chemistry 1996; 68:1507-12. http://dx.doi. org/10.1021/ac9508964

7. Heron S, Tchapla A, Chervet JP. Influence of injection parameters on column performance in nanoscale high-performance liquid chromatography. Chromatographia, 2000; 51:495-9. http://dx.doi. org/10.1007/BF02490492

8. Beisler AT, Schaefer KE, Weber SG. Simple method for the quantitative examination of extra column band broadening in microchromatographic systems. Journal of Chromatography A 2003; 986(2):247-51. http://dx.doi.org/10.1016/S0021-9673(02)02018-6

9. Szumski M, Buszewski B. State of the Art in Miniaturized Separation Techniques. Critical Reviews in Analytical Chemistry 2002; 32(1):1-46. http:// dx.doi.org/10.1080/10408340290765434

10. Scott RPW. Liquid Chromatography Column Theory. New York: Wiley; 1992.

11. Sternberg JC. In: Giddings JC, Keller RA, editors. Adavances in Chromatography. New York: Marcel Dekker; 1966. vol. 2, p. 205-270.

12. Martin M, Eon C, Guiochon G. Study of the pertinency of pressure in liquid chromatography: II. Problems in equipment design. Journal of Chromatography A 1975.; 108(2):229-41. http://dx.doi.org/10.1016/S0021- 9673.(00)84666-X

13. Kirkland JJ, Yau WW, Stoklosa HJ, Dilks Junior CH. Journal of Chromatographic Science 1977; 15:303.

14. Reese CE, Scott RPW. J. Chromatogr. 1980; 18:479.

15. Lauer HH, Rozing GP. The selection of optimum conditions in HPLC I. The determination of external band spreading in LC instruments. Chromatographia 1981; 14.(11):641-7. http://dx.doi.org/10.1007/BF02291104

16. DiCesare JL, Dong MW, Atwood JG. Very-high-speed liquid chromatography: II. Some instrumental factors influencing performance. Journal of Chromatography A 1981; 217:369-86. http://dx.doi.org/10.1016/S0021- 9673.(00)88091-7

17. Freebaim KW, Knox JH. Dispersion measurements on conventional and miniaturised HPLC systems. Chromatographia 1984; 19(1):37-47. http://dx.doi. org/10.1007/BF02687717

18. Hupe KP, Jonker RJ, Rozing G. Determination of band-spreading effects in high-performance liquid chromatographic instruments. Journal of Chromatography A 1984; 285:253-65. http://dx.doi. org/10.1016/S0021-9673(01)87767-0

19. Cohen KA, Stuart JD. Journal of Chromatographic Science 1987; 25:381.

20. Liu G, Svenson L, Djordjevie N, Erni F. Extra-column band broadening in high-temperature open-tubular liquid chromatography. Journal of Chromatography A 1993.; 633(1-2):25-30. http://dx.doi.org/10.1016/0021- 9673.(93)83134-E

21. Bakalyar SR, Phipps C, Spuce B, Olsen K. Choosing sample volume to achieve maximum detection sensitivity and resolution with high-performance liquid chromatography columns of 1.0, 2.1 and 4.6 mm I.D. Journal of Chromatography A 1997; 762(1-2):167‑85. http://dx.doi.org/10.1016/S0021-9673(96)00851-5

22. Prüβ A, Kempter C, Gysler J, Jira T. Extracolumn band broadening in capillary liquid chromatography. Journal of Chromatography A 2003; 1016(2):129-41. http://dx.doi.org/10.1016/S0021-9673(03)01290-1

23. Visser JPC. Recent developments in microcolumn liquid chromatography. Journal of Chromatography A 1999; 856(1-2):117-143. http://dx.doi.org/10.1016/ S0021-9673(99)00692-5

24. Claessens HA, Burcinova A, Cramers CA, Mussche P, Van Tilburg CE. Evaluation of injection systems for open tubular liquid chromatography. Journal of Microcolumn Separations 1990; 2(3):132-37. http://dx.doi.org/10.1002/mcs.1220020309

25. Harvey MC, Stearns SD, Averette JP. LC Liq. Chromatogr. HPLC Mag. 1985; 3:5.

26. Jorgenson JW, Guthrie EJ. Liquid chromatography in open-tubular columns : Theory of column optimization with limited pressure and analysis time, and fabrication of chemically bonded reversedphase columns on etched borosilicate glass capillaries Journal of Chromatography A 1983; 255:335-48. http://dx.doi.org/10.1016/S0021-9673(01)88293-5

27. Manz A, Simon W. Injectors for open-tubular column liquid chromatography with 106 theoretical plates at retention times in the minute range. Journal of Chromatography A 1987; 387:187-96. http://dx.doi. org/10.1016/S0021-9673(01)94523-6

28. Taylor G. Proceedings of the Royal Society A: Mathematical, Physical and Engineering Sciences 1953.; 219:186.

29. Taylor G. Proceedings of the Royal Society A: Mathematical, Physical and Engineering Sciences 1954.; 225:473.

30. Cazes J. Chromatography Theory. New York: Marcel Dekker Inc.; 2002.

31. Scott RPW, Kucera P. Journal of Chromatographic Science 1971; 9:641.

32. Schmauch L. J. Response Time and Flow Sensitivity of Detectors for Gas Chromatography. Analytical Chemistry 1959; 31(2):225-30. http://dx.doi.org/10.1021/ ac60146a021

33. Vandenheuvel FA. Estimation and Correction of Post- Column Dead Volume Effect in Chromatography. Analytical Chemistry 1963; 35(9):1193-98. http:// dx.doi.org/10.1021/ac60202a064

34. McWilliam IG, Bolton HC. Instrumental peak distortion. I. Relaxation time effects. Analytical Chemistry 1969; 41(13):1755-62. http://dx.doi. org/10.1021/ac60282a001.