Skip to Content
Merck
  • Estimation of the effects of longitudinal temperature gradients caused by frictional heating on the solute retention using fully porous and superficially porous sub-2μm materials.

Estimation of the effects of longitudinal temperature gradients caused by frictional heating on the solute retention using fully porous and superficially porous sub-2μm materials.

Journal of chromatography. A (2014-07-30)
Szabolcs Fekete, Jenő Fekete, Davy Guillarme
ABSTRACT

In this study, the retention changes induced by frictional heating were evaluated for model small compounds (150-190Da) and a small protein, namely insulin (5.7kDa). For this purpose, the effect of longitudinal temperature gradient caused by frictional heating was experimentally dissociated from the combined effect of pressure and frictional heating, by working either in constant and variable inlet pressure modes. Various columns packed with core-shell and fully porous sub-2μm particles were tested. It appears that frictional heating was less pronounced on the column packed with smallest core-shell particles (1.3μm), compared to the ones packed with core-shell and fully porous particles of 1.7-1.8μm. This observation was attributed to the low permeability of this material and the fact that it can only be employed in a restricted flow rate range, thus limiting the generated heat power. In addition, the thermal conductivity of the solid silica core of superficially porous particles (1.4W/m/K) is known to be much larger than that of fully porous silica. Then, the heat dissipation is improved. However, if systems with higher pressure capability would be available and the mechanical stability of 1.3μm core-shell material was extended to e.g. 2000bar, the retention would be more severely impacted. At 2000bar, ∼4.4W heat power and +30°C increase at column outlet temperature is expected. Last but not least, when analyzing large molecules, the impact of pressure overcomes the frictional heating effects. This was demonstrated in this study with insulin (∼5.7kDa).

MATERIALS
Product Number
Brand
Product Description

Supelco
Ethylparaben, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Methylparaben, Pharmaceutical Secondary Standard; Certified Reference Material
Ethyl parahydroxybenzoate, European Pharmacopoeia (EP) Reference Standard
Supelco
Methyl Paraben, PESTANAL®, analytical standard
Butyl parahydroxybenzoate, European Pharmacopoeia (EP) Reference Standard
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Methyl parahydroxybenzoate, European Pharmacopoeia (EP) Reference Standard
USP
Methylparaben, United States Pharmacopeia (USP) Reference Standard
USP
Ethylparaben, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Ultrapure Acetonitrile
Fluorouracil impurity C, European Pharmacopoeia (EP) Reference Standard
Supelco
Uracil, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrile, ReagentPlus®, 99%
Sigma-Aldrich
Trifluoroacetic acid, ≥99%, for protein sequencing
Sigma-Aldrich
Acetonitrile, suitable for DNA synthesis, ≥99.9% (GC)
Sigma-Aldrich
Acetonitrile, ACS reagent, ≥99.5%
Sigma-Aldrich
Acetonitrile, biotech. grade, ≥99.93%
Sigma-Aldrich
Acetonitrile, ≥99.5% (GC)
Supelco
Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Supelco
Butylparaben, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetonitrile, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Butyl 4-hydroxybenzoate, ≥99%
Sigma-Aldrich
Methyl 4-hydroxybenzoate, ≥99%, FCC
Supelco
Trifluoroacetic acid, analytical standard
Supelco
Acetonitrile, analytical standard
Sigma-Aldrich
Methyl 4-hydroxybenzoate, tested according to Ph. Eur.
Sigma-Aldrich
Methyl 4-hydroxybenzoate, ReagentPlus®, ≥99.0%, crystalline
Sigma-Aldrich
Methyl 4-hydroxybenzoate, analytical standard
Sigma-Aldrich
Methyl 4-hydroxybenzoate, BioXtra, ≥99.0% (titration)