Performance of columns packed with the new shell particles,Kinetex-C18

The performance of the new Kinetex-C₁₈ column was investigated. Packed with a new brand of porous shell particles, this column has an outstanding efficiency. Once corrected for the contribution of the instrument extra column volume, the minimum values of the reduced plate heights for a number of low molecular weight compounds (e.g., anthracene and naphtho[2,3-a]pyrene) were between 1.0 and 1.3, breaking the legendary record set 3 years ago by Halo-C₁₈ packed columns. The liquid-solid mass transfer of proteins (e.g., insulin and lyzozyme) is exceptionally fast on Kinetex-C₁₈ much faster than on the Halo-C₁₈ column. The different contributions of dispersion and mass transfer resistances to the column efficiency were determined and discussed. The possible reasons for this extremely high column efficiency are discussed.     

Performance of new prototype packed columns for very high pressure liquid chromatography

The reduced heights equivalent to a theoretical plate (HETP) of naphtho[2,3-a]pyrene were measured at room temperature on two sets of new prototype columns designed to be used in very high pressure liquid chromatography (VHPLC). The mobile phase used was pure acetonitrile. The columns are 50, 100, and 150 mm long. Those of the first set are 2.1 mm I.D., those of the second set, 3.0 mm I.D. The performance of these new columns were compared to those of the first generation of VHPLC columns, commercially available in 2.1 mm I.D. The prototype and commercial columns behave similarly at low reduced linear velocities (ν<5$\nu <5$), when the heat effects are negligible. At high flow rates, the shorter prototype columns have a twice better efficiency and less steep C-branches than the commercial columns. In contrast, the C-branch of the 150 mm long prototype columns are slightly steeper than those of the commercial columns. The important contribution to the reduced HETP that is due to the heat effects at high flow rates can in part be accounted for by a band broadening model governed by a flow mechanism with the shortest prototype columns. The sole heat effects cannot, however, explain the mediocre reduced HETPs of the 2.1 and 3.0 I.D. 150 mm long prototype columns. It seems that radial heterogeneity of the flow rate of the long prototype columns is significantly larger than that of the short columns. The contribution of the packing heterogeneity adds up to that of the heat effects to yield a poor column efficiency when sub-2μm$\text{sub-}2\mu \text{m}$ are packed into thin, long column tubes.     

On the relationship between band broadening and the particle-size distribution of the packing material in liquid chromatography: theory and practice

The influence of the particle size distribution (PSD) on the band broadening and the efficiency of packed columns is investigated on both theoretical and practical viewpoints. Each of the classical contributions to mass transfer kinetics, those due to longitudinal diffusion, eddy dispersion, and solid–liquid mass transfer resistance are measured and analyzed in terms of their expected and observed intensity as a function of the PSD of mixtures of the commercially available packing materials, 5 and 3 μm Luna-C₁₈(2) particles (Phenomenex, Torrance, CA, USA). Six 4.6 mm × 150 mm columns were packed with different mixtures of these two materials. The efficiencies of these columns were measured for a non-retained and a retained analytes in a mixture of acetonitrile and water. The longitudinal diffusion coefficient was directly measured by the peak parking method. The solid–liquid mass transfer coefficient was measured from the combination of the peak parking method, the best model of effective diffusion coefficient and the actual PSDs of the different particle mixtures measured by Coulter counter experiments. The eddy diffusion term was measured according to a recently developed protocol, by numerical integration of the peak profiles. Our results clearly show that the PSD has no measurable impact on any of the coefficients of the van Deemter equation. On the contrary and surprisingly, adding a small fraction of large particles to a batch of small particles can improve the quality of the packing of the fine particles. Our results indirectly confirm that the success of sub-3 μm shell particles is due to the roughness of their external surface, which contributes to eliminate most of the nefarious wall effects.