PMID- 22762953 OWN - NLM STAT- MEDLINE DCOM- 20121113 LR - 20220311 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1252 DP - 2012 Aug 24 TI - Repeatability of the efficiency of columns packed with sub-3mum core-shell particles: Part I. 2.6mum Kinetex-C(18) particles in 4.6mm and 2.1mmx100mm column formats. PG - 31-44 LID - 10.1016/j.chroma.2012.05.072 [doi] AB - The column-to-column repeatability of the mass transfer mechanism in columns packed with sub-3mum shell particles was investigated. The parameters of this mechanism were measured for twelve columns (six 2.1mmx100mm and six 4.6mmx100mm) packed with the same batch of 2.6mum Kinetex-C(18) particles (Phenomenex, CA, USA). For both series, the manufacturer provided columns at different positions in the efficiency distribution given by the quality test control. Three compounds were used, uracil, naphthalene and insulin. The reduced longitudinal diffusion term was measured with the peak parking (PP) method, the reduced solid-liquid mass transfer resistance term was given by a combination of the PP results and a model of effective diffusion in ternary composite materials (non-porous cores, concentric porous shell, and eluent matrix), validated previously. The overall eddy diffusion term was obtained by subtraction of these two HETP terms from the overall reduced HETP measured by numerical integration of the entire peak profiles. The results demonstrate that the dispersion of the column efficiencies is only due to the random nature of the packing process. At the highest reduced velocity achieved, the relative standard deviations (RSDs) of the eddy diffusion term for the 2.1mm I.D. columns were ca. 7% and 3% for the low molecular weight compounds and for insulin, respectively. For the 4.6mm I.D. columns, these RSDs were 15% and 5%, respectively. The larger RSDs for the 4.6mm I.D. columns is explained by the exceptionally low value of the eddy diffusion term. CI - Copyright (c) 2012 Elsevier B.V. All rights reserved. FAU - Gritti, Fabrice AU - Gritti F AD - Department of Chemistry, University of Tennessee, Knoxville, TN 37996-1600, USA. FAU - Guiochon, Georges AU - Guiochon G LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20120615 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Insulin) RN - 0 (Naphthalenes) RN - 2166IN72UN (naphthalene) RN - 56HH86ZVCT (Uracil) SB - IM MH - Chromatography, High Pressure Liquid/*instrumentation MH - Diffusion MH - Insulin/chemistry MH - *Microspheres MH - Models, Chemical MH - Molecular Weight MH - Naphthalenes/chemistry MH - Permeability MH - Porosity MH - Reproducibility of Results MH - Temperature MH - Uracil/chemistry EDAT- 2012/07/06 06:00 MHDA- 2012/11/14 06:00 CRDT- 2012/07/06 06:00 PHST- 2012/04/11 00:00 [received] PHST- 2012/05/17 00:00 [revised] PHST- 2012/05/21 00:00 [accepted] PHST- 2012/07/06 06:00 [entrez] PHST- 2012/07/06 06:00 [pubmed] PHST- 2012/11/14 06:00 [medline] AID - S0021-9673(12)00804-7 [pii] AID - 10.1016/j.chroma.2012.05.072 [doi] PST - ppublish SO - J Chromatogr A. 2012 Aug 24;1252:31-44. doi: 10.1016/j.chroma.2012.05.072. Epub 2012 Jun 15.