title: Theoretical study of closed-loop recycling liquid-liquid chromatography and experimental verification of the theory.
abstract: The non-ideal recycling equilibrium-cell model including the effects of extra-column dispersion is used to simulate and analyze closed-loop recycling counter-current chromatography (CLR CCC). Previously, the operating scheme with the detector located before the column was considered. In this study, analysis of the process is carried out for a more realistic and practical scheme with the detector located immediately after the column. Peak equation for individual cycles and equations describing the transport of single peaks and complex chromatograms inside the recycling closed-loop, as well as equations for the resolution between single solute peaks of the neighboring cycles, for the resolution of peaks in the recycling chromatogram and for the resolution between the chromatograms of the neighboring cycles are presented. It is shown that, unlike conventional chromatography, increasing of the extra-column volume (the recycling line length) may allow a better separation of the components in CLR chromatography. For the experimental verification of the theory, aspirin, caffeine, coumarin and the solvent system hexane/ethyl acetate/ethanol/water (1:1:1:1) were used. Comparison of experimental and simulated processes of recycling and distribution of the solutes in the closed-loop demonstrated a good agreement between theory and experiment.
authors: Kurnakov Institute of General & Inorganic Chemistry, Russian Academy of Sciences, Leninsky Prospekt 31, Moscow 119991, Russia. Electronic address: kost@igic.ras.ru.
authors: Artak E
authors: AE
authors: Kostanyan
authors: Kurnakov Institute of General & Inorganic Chemistry, Russian Academy of Sciences, Leninsky Prospekt 31, Moscow 119991, Russia.
authors: Andrey A
authors: AA
authors: Erastov
mesh_terms: D000085:Acetates / Q000737:chemistry; D001241:Aspirin / Q000032:analysis; D002110:Caffeine / Q000032:analysis; D003374:Coumarins / Q000032:analysis; D003377:Countercurrent Distribution / Q000379:methods*; D000431:Ethanol / Q000737:chemistry; D006586:Hexanes / Q000737:chemistry; D008962:Models, Theoretical; D059027:Recycling; D015203:Reproducibility of Results; D012996:Solutions; D012997:Solvents / Q000737:chemistry; D014867:Water / Q000737:chemistry
chemical_list: D000085:Acetates; D003374:Coumarins; D006586:Hexanes; D012996:Solutions; D012997:Solvents; D014867:Water; C026385:n-hexane; D002110:Caffeine; D000431:Ethanol; C007650:ethyl acetate; C030123:coumarin; D001241:Aspirin
keywords: Closed-loop recycling counter-current chromatography; Non-ideal recycling equilibrium cell model; Peak and chromatogram equations; Resolution