1998 The Japan Society for Analytical Chemistry 769 Analysis on mass-transfer phenomena in reversed-phase liquid chromatography Kanji MIYABE** **F acu
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1 1998 The Japan Society for Analytical Chemistry 769 Analysis on mass-transfer phenomena in reversed-phase liquid chromatography Kanji MIYABE** **F aculty of Education, Toyama University, 3190, Gofuku, Toyama (Received 11 March 1998, Accepted 26 June 1998) An analytical study was made concerning mass-transfer phenomena in reversed-phase liquid chromatography (RP-LC). A moment method was applied for analyzing the properties of chromatographic peaks measured under various conditions related to sample substances as well as stationary and mobile phases. First moment analyses provided some pieces of information concerning the mass-transfer equilibrium in RP-LC. The isosteric heat of adsorption (-Qst) was smaller than the corresponding heat of vaporization. The relatively small value of -Qst could be explained by solvophobic theory. From second moment analyses, it was indicated that the contribution of intraparticle diffusion to the overall mass-transfer resistance in a column was usually important, and that surface diffusion played a significantly dominant role for mass transfer in RP packing materials. The activation energy of the surface diffusion (Es) was larger than -Qst, in RP-LC. The correlation between Es and Qst could be quantitatively interpreted based on the absolute rate theory by assuming that surface diffusion was an activated process similar to molecular diffusion in the liquid phase. The establishment of both an enthalpy-entropy compensation effect and a linear free-energy relation was confirmed irrespective of the separation conditions in RP-LC. A nondimensional rate equation was derived on the basis of moment analysis theory. The equation consists of several terms representing the contributions of mass-transfer processes, such as molecular diffusion, eddy diffusion, fluid-toparticle mass transfer, and intraparticle pore and surface diffusions, to peak spreading. The influence of some operational parameters on the column efficiency was numerically analyzed while considering the individual contribution of each term. It was demonstrated that fundamental studies of surface diffusion provided some essential pieces of information for elucidating the separation mechanism in RP-LC. Keywords : reversed-phase liquid chromatography; mass transfer; surface diffusion; moment analysis; nondimensional rate equation.
2 770 BUNSEKI KAGAKU Vol. 47 (1998) (1) (2) (3) (4) (5) (6) (7) (8) (9) (10)
3 Table 1 Thermodynamic properties in reversed-phase liquid chromatography (from ref. 14 with permission)
4 772 BUNSEKI KAGAKU Vol ) Fig. 1 Correlation of the adsorption equilibrium constant with the hydrocarbonaceous surface area of the solute (from ref. 14 with permission) Keys: refer to Table 1. Mobile phase: A and B, 70 vol% acetonitrile; C and D, 70 vol% methanol
5 Fig. 2 Comparison of retention factor in 60 vol% methanol and 60 vol% ethanol (from ref. 23 with permission) Conditions: column, Develosil ODS-3, 150 X 4.6 mm i.d.; temperature, 313 K; flow rate, 0.5 cm' min Fig. 4 Correlation of the logarithm of adsorption equilibrium constant with hydrocarbonaceous surface area of adsorbates (from ref. 18 with permission) For key to symbols, refer to Table 1 Fig. 3 Relationship between isosteric heat of adsorption and composition of mobile phase (from ref. 18 with permission)
6 774 BUNSEKI KAGAKU Vol. 47 (1998) Table 2 Comparison of the contributions of axial dispersion, fluid-to-particle mass transfer, and intraparticle diffusion to second moments (from ref. 14 with permission)
7 Table 3 Comparison of the contributions of pore and surface diffusions to intraparticle diffusion (from ref. 14 with permission) Fig. 5 Schematic interpretation of thermodynamic properties concerning adsorption and surface diffusion phenomena (from ref. 13 with permission)
8 776 BUNSEKI KAGAKU Vol. 47 (1998) Fig. 6 Correlation of frequency factor with the activation energy of the surface diffusion (from ref. 14 with permission)
9 Fig. 7 Correlation of the surface diffusion coefficient with the adsorption equilibrium constant (from ref. 14 with permission)
10 778 BUNSEKI KAGAKU Vol. 47 (1998) Fig. 8 Surface diffusion coefficient as a function of alkyl chain length of stationary phases (from ref. 21 with permission) Fig. 9 Surface diffusion coefficient as a function of volumetric fraction of organic modifiers in mobile phases (from ref. 18 with permission)
11 Fig. 10 Contributions of each mass transfer process in a column to peak spreading phenomena at K = 1 and 10 (from ref. 36 with permission)
12 780 BUNSEKI KAGAKU Vol. 47 (1998) Fig. 11 Contributions of each mass transfer process in a column to the correlation between h and K at 1, = 10 and 100 (from ref. 36 with permission) Fig. 12 Contributions of each mass transfer process in a column to the correlation between h and v at /3 = 0.1, 0.2, 0.3, 0.4, and 0.5 (from ref. 36 with permission)
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14 782 BUNSEKI KAGAKU Vol. 47 (1998)
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