Comparison of the mass transfer in totally porous and superficially porous stationary phases in liquid chromatography

Kiss, Ibolya; Bacskay, Ivett; Kilár, Ferenc; Felinger, Attila
June 2010
Analytical & Bioanalytical Chemistry;Jun2010, Vol. 397 Issue 3, p1307
Academic Journal
The characterization of mass-transfer processes in a chromatographic column during a separation process is essential, since the influence of the mass-transfer kinetics on the shape of the chromatographic band profiles and on the efficiency of the separation is crucial. Several sources of mass transfer in a chromatographic bed have been identified and studied: the axial dispersion in the stream of mobile phase, the external mass-transfer resistance, intraparticle diffusion, and the kinetics of adsorption–desorption. We measured and compared the characteristics and performance of a new brand of shell particles and those of a conventional brand of totally porous silica particles. The shell stationary phase was made of 2.7-µm superficially porous particles (a 1.7-µm solid core is covered with a 0.5-µm-thick shell of porous silica). The other material consisted of totally porous particles of conventional 3.5-µm commercial silica. We measured the first and second central moments of the peaks of human insulin over a wide range of mobile phase velocities (from 0.02 to 1.3 mL/min) at 20°C. The plate height equations were constructed and the axial dispersion, external mass transfer, as well as the intraparticle diffusion coefficients were calculated for the two stationary phases.


Related Articles

  • Silica, Hybrid Silica, Hydride Silica and Non-Silica Stationary Phases for Liquid Chromatography. Part II: Chemical and Thermal Stability. Borges, Endler M.; Volmer, Dietrich A. // Journal of Chromatographic Science;Aug2015, Vol. 53 Issue 7, p1107 

    In the first part of this review, stationary phases (silica, hybrid silica, hydride silica and non-silica stationary phases) were characterized and compared with respect to selectivity, efficiency, resolution, solvent consumption and analysis time. The present review focuses on the thermal and...

  • Monolithic and core-shell columns in comprehensive two-dimensional HPLC: a review. Jandera, Pavel; Hájek, Tomáš; Staňková, Magda // Analytical & Bioanalytical Chemistry;Jan2015, Vol. 407 Issue 1, p139 

    The crucial point affecting the separation time in comprehensive two-dimensional liquid chromatography is the performance of the column used in the second dimension, which should allow highly efficient fast chromatographic separations in the short time available for the analysis of fractions...

  • Stationary Phases for High-Temperature Liquid Chromatography. Yu Yang // LC-GC Europe;Jun2003, Vol. 16 Issue 6a, p37 

    Examines the use of stationary phases at temperatures considerably higher than room temperature. Use of ristocetin A chiral stationary phase in studying the effect of temperature on the retention of several chiral compounds; Investigation of the use of porous graphitic carbon on...

  • The Thermally Tuned Tandem Column Approach to Optimizing Selectivity in HPLC. Yun Mao; Carr, Peter W. // LC-GC North America;Jun2003 Supplement, Vol. 21 Issue 6, p69 

    Describes the thermally tuned tandem column concept for the optimization of selectivity in liquid chromatography by effectively continuously adjusting the stationary phase. Serial connection of two columns with distinctly different chromatographic selectivities; Comparison of thermally tuned...

  • Development of silica-based stationary phases for high-performance liquid chromatography. Hongdeng Qiu; Xiaojing Liang; Min Sun; Shengxiang Jiang // Analytical & Bioanalytical Chemistry;May2011, Vol. 399 Issue 10, p3307 

    Stationary phases are the basis of the development and application of high-performance liquid chromatography (HPLC). In this review we focused on the development of silica-based stationary phases, including the synthesis of silica gel and the application of silica in hydrophilic interaction...

  • Chromatographic Performance of Silica-Based Stationary Phases in High Temperature Liquid Chromatography: Pharmaceutical Applications. Guillarme, Davy; Russo, Rossana; Rudaz, Serge; Bicchi, Carlo; Veuthey, Jean-Luc // Current Pharmaceutical Analysis;Nov2007, Vol. 3 Issue 4, p221 

    High temperature liquid chromatography is currently well established in separation sciences. The decrease of mobile phase viscosity with temperature provides fast separations with high efficiency, limiting excessive backpressure. Furthermore, the water polarity decreases with temperature...

  • Effect of Ionic Liquid Additives to Mobile Phase on Separation and System Efficiency for HPLC of Selected Alkaloids on Different Stationary Phases. Petruczynik, Anna // Journal of Chromatographic Science;Apr2012, Vol. 50 Issue 4, p287 

    The silica-based stationary phases with favorable physical characteristics are the most popular in liquid chromatography. However, there are several problems with silica-based materials: severe peak tailing in the chromatography of basic compounds, non-reproducibility for the same chemistry...

  • HPLC analysis of K-48 concentration in plasma. Kalász, H.; Hasan, M. Y.; Sheen, R.; Kuca, K.; Petroianu, G.; Ludányi, K.; Gergely, A.; Tekes, K. // Analytical & Bioanalytical Chemistry;Aug2006, Vol. 385 Issue 6, p1062 

    K-48 is a new oxime-type compound to be used as an enzyme reactivator in the treatment of exposure to organophosphorous compounds. Plasma concentration of K-48 can be determined using reversed-phase HPLC. Analysis using octyl silica stationary phase and ultraviolet-absorbance detection is fast...

  • Development and Validation of HPTLCMethod for Estimation of Propranolol Hydrochloride and Flunarizine Dihydrochloride in Combined Dosage Form. Patel, Palak; Bhatt, Kashyap K. // ISRN Analytical Chemistry;2012, Vol. 2012, p1 

    A simple, sensitive, and precise high-performance thin layer chromatographic method has been developed for the estimation of propranolol hydrochloride and Flunarizine dihydrochloride in combined dosage form. The method employed HPTLC aluminum plates precoated with silica gel 60F as the...


Read the Article


Sorry, but this item is not currently available from your library.

Try another library?
Sign out of this library

Other Topics