Continuous Annular Chromatography

253

Fig. 10. Photograph of the separation of the PGM and base metals in a two-phase (mixed mode) P-CAC system

sition after iridium as the last precious metal to leave the annular column, the base metals were stripped of the cation-exchange resin by using a step-eluent (2–3 mol/l HCl). In this eluent the base metals were not retained by either of the two stationary phases. Therefore a fraction consisting of the sum of the base metals could be collected finally at the end of the annular column (Fig. 10). It has been found from batch experiments that the base metals Fe, Ni and Co are fully adsorbed by the cation-exchange resin when the hydrochloric acid concentration of the eluent does not exceed 0.4 M. If the concentration exceeds 0.4 M the base metals start to break through. The same thing happens when the hyRhodium Palladium

base metals
Platin Iridium IV base metals (Fe, Ni, Co)

elution angle [°]
Fig. 11. Experimental chromatogram of a separation of a solution containing PGMs and base

metals using a mixed mode P-CAC system1

The adsorption isotherm represents the equilibrium of a compound between the liquid and the solid phase in chromatography. Wolfgang drochloric acid concentration of the feed solution exceeded 4 M. is to couple the continuous chromatograph to a continuous fermenter system.254 J. The height is directly proportional to the maximum capacity of the resin. 8 References 1. Broughton DB (1961) U. 2. its productivity and resolution improvement. A very promising application of the P-CAC technology. step and displacement elution are possible on a CAC. Continuous bioreactors are receiving attention as an efficient method of producing biochemicals. 3. No precise timing of a valve system for the introduction of feed and the product removal are needed. The maximum capacity of the resin for the mixture of all three cations was calculated from the adsorption isotherm. The apparatus retains its relative mechanical simplicity in comparison with fixed-bed processes. For this application it was necessary to develop a P-CAC unit where the column can be autoclaved by steam. The coupling of a continuous fermentation to a continuous capturing step promises a significant improvement in terms of throughput and product yield. isotherms can be estimated by batch shaking experiments. Sisson WG (1976) J Chromatogr 126:381 . 7 Conclusion Several applications throughout the last two decades have shown that starting from batch chromatography experiments a scale-up to a continuous annular chromatograph is easy and straightforward. and its truly continuous operational capabilities. which depending on the exact conditions results in dilution factors between 2 and 10. which at the time this article was written was undergoing intensive studies. Patent 2 985:589 Wolfgang J (1996) PhD Thesis. including isocratic.S. It was also shown that the feed inlet band of the PGMs broadens when it passes through the cation-exchange resin layer. Spence RD. It has also been shown that many operating modes. Technische Universität Graz Giddings JC (1962) Anal Chem 34 Martin AJP (1949) Discuss Faraday Soc 7:32 Scott CD. The minimum height of the cation-exchange resin in the P-CAC depends on the concentration of the base metals present in the feed solution. The key advantages of annular chromatography over fixed-bed operations are likely the simplicity of the apparatus. Compared to the SMB system the annular chromatography allows the continuous separation of a multicomponent mixture as it is most often the case in biopharmaceutical separations. This means that the concentration of the platinum group metals in the sample decreases accordingly. Figure 11 shows the experimental chromatogram of the separation of a mixture used in the studies. 4. 5.

20. 32. Freitag R (2001) Biotech Bioeng 73(6):521 Uretschläger A. 25. 34. 37. Jungbauer A (2000) J Chromatogr A 890:7 Uretschläger A. Amundson NR (1970) Trans R Soc A267:419 Howard AJ (1987) MS Thesis. 22. McGraw-Hill. 18. Wiley. New York. 39. Sisson WG. Palekar AA (1998) Appl Biochem Biotechnol 73:215 Prior J (2000) Personal communications (with Prior Separation Technology) Ruthven DM (1984) Principles of adsorption and adsorption processes.Continuous Annular Chromatography 255 6. 14. 26. 12. Josic D (2000) Biotechnol Prog 17(1):140 Hunt B. Couder M. Michelsen ML (1978) Solution of differential equation models by polynomial approximation. 27. Carta G (1990) Biotechnol Prog 6:13 Bloomingburg GF. 15. 8. Goto S (1994) Sep Sci Technol 29:1311 Kitakawa A. Wilke CR (1975) Mass transfer. Martin AJP. N. 7. Brazda M. Begovich JM. Messenböck RC. 21. Byers CH (1988) Ind Eng Chem Res 27:1873 Byers CH. Wolfgang J (1996) Chem Eng Process 35:459 Wolfgang J. Goto S (1991) Sep Sci Technol 26:1 Takahashi Y. Wolfgang J (2000) Erzmetall (submitted) Received: July 2001 . Bart HJ. 40. Sisson WG (1983) Sep Sci Technol 18:1167 Howard AJ. Yonemoto T (1997) Ind Eng Chem Res 36:3809 Bart HJ. 43.J. 42. Bart HJ. Goto S (1992) J Chem Eng Japan 25:403 Takahashi Y. 29. Sisson WG (1978) J Liquid Chromatogr 1:427 Canon RM. 13. Yonemoto T (1995) Sep Sci Technol 30:3089 Kitakawa A. 33. p 548 Carta G (1988) Chem Eng Sci 43:2877 Villadsen J. Wolfgang J (2001) Am Biotechnol Lab 19(1):42 Prior A. 11. New York Wankat PC (1977) AIChE J 23:859 Rhee HK. 19. 30. 31. Vasudevan PT. Canon RM. 38. 28. Iberer G. Byers CH (1997) Sep Sci Technol 32:71 Reißner K. Wolfgang J (2000) Internal study. Yamanishi Y. Carta G (1994) Chem Eng J 55:19 DeCarli JP II. 24. Jungbauer A. DeCarli JP II. Jungbauer A (2001) J Chromatogr A 908:243 Genest PW. Shang Y. Messenböck RC. 45. Prior A. Sisson WG (1982) Resources Conserv 9:219 Begovich JM. Byers CH (1990) AIChE J 36:1220 Takahashi Y. 46. 9. Carta G. Byers CH. 16. Prior Separation Technology GmbH Blanche F. Prior A. Field TG. Schwinn H. 10. 17. Wolfgang J. Yamanishi Y. Pigford RL. Englewood Cliffs. Sisson WG (1980) Sep Sci Technol 15:655 Begovich JM. Einhauer A. 35. University of Virginia. 44. 41. Byers CH. Charlottsville Thomas HJ (1944) J Am Chem Soc 66:1664 Sherwood RK. Aris R. Goto S (1991) J Chem Eng Japan 24:121 Takahashi Y. Byers CH (1997) J Chromatogr A 763:49 Rögner K (1995) Personal communications (with Prior Separation Technology) Kaufmann T (1997) Personal communications (with Prior Separation Technology) Geisenhof C (1998) Personal communications (with Prior Separation Technology) Pritschet M (1999) Personal communications (with Prior Separation Technology) Giovannini R. 23. Carta G. Synge RLM (1941) Biochem J 35:1358 Said AS (1956) AIChE J 3:477 Ringer T (1998) Personal communications (with Prior Separation Technology) Buchacher A. Prior A. 36. Prentice-Hall.

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