Search results for "lithic"
showing 10 items of 392 documents
Study of elution behaviour with gradient voltage in CEC using methacrylate monolithic columns.
2010
A theoretical study on the retention behaviour and chromatographic performance of neutral solutes using a lauryl methacrylate-based monolithic column under voltage gradient mode in CEC was carried out. Through a flexible mathematical function based on a modified Gaussian model, the peak shape of compounds was firstly fitted under constant and gradient voltage. Using the peak shape parameters and retention time, the estimation of global chromatographic performance, efficiency and peak capacity under several voltage conditions was performed. The influence of voltage gradient on the separation efficiency is discussed and simple equations are presented to calculate retention and peak widths und…
Development of Methods for the Determination of Ts, T3s and Sterols in Vegetable Oils
2012
In this work, a CEC method using methacrylate ester-based monolithic columns was developed to determine Ts and T3s present in edible oils. The potential of this method to evaluate olive oil adulteration with lower-cost oils of a different botanical origin was also investigated. For these purposes, the following vegetable oils were used: soybean, sunflower, grapeseed, EVOO (Coosur), hazelnut (Guinama), corn (Hacendado) and red palm (Blue Bay).
Monolithic silica columns of various format in automated sample clean-up/multidimensional liquid chromatography/mass spectrometry for peptidomics.
2007
The following particulate and monolithic silica columns were implemented in a fully automated and flexible multidimensional LC/MS system with integrated sample clean-up, to perform the analysis of endogeneous peptides from filtered urine and plasma samples: restricted access sulphonic acid strong cation-exchanger (RAM-SCX) for sample clean-up, RP 18 Chromolith guard columns as trap columns and 100 microm I.D. monolithic RP 18 fused silica capillary columns as last LC dimension. The results show sufficient overall system reproducibility and repeatability. Implementation of monolithic silica columns added an additional flexibility with respect to flow rate variation and adjustment due to the …
Flow-through pore characteristics of monolithic silicas and their impact on column performance in high-performance liquid chromatography
2008
Abstract In order to elucidate the role of the flow-through characteristics with regard to the column performance in high-performance liquid chromatography (HPLC) native and n -octadecyl bonded monolithic silica rods and columns, respectively of 100 mm length and 4.6 mm ID with mesopores in the range between 10 and 25 nm and macropores in the range between 0.7 and 6.0 μm were examined by mercury intrusion/extrusion, scanning electron microscopy, image analysis and permeability. The obtained data of the flow-through pore sizes and porosity values as well as surface-to-volume ratio of the stationary phase skeleton enabled to predict their influence to the chromatographic separation efficiency…
Comprehensive pore structure characterization of silica monoliths with controlled mesopore size and macropore size by nitrogen sorption, mercury poro…
2005
The porosity of monolithic silica columns is measured by using different analytical methods. Two sets of monoliths were prepared with a given mesopore diameter of 10 and 25 nm, respectively and with gradated macropore diameters between 1.8 and 7.5 microm. After preparing the two sets of monolithic silica columns with different macro- and mesopores the internal, external and total porosity of these columns are determined by inverse size-exclusion chromatography (ISEC) using polystyrene samples of narrow molecular size distribution and known average molecular weight. The ISEC data from the 4.6 mm analytical monolithic silica columns are used to determine the structural properties of monolithi…
Pore structural characterization of monolithic silica columns by inverse size-exclusion chromatography
2007
In this work, a parallel pore model (PPM) and a pore network model (PNM) are developed to provide a state-of-art method for the calculation of several characteristic pore structural parameters from inverse size-exclusion chromatography (ISEC) experiments. The proposed PPM and PNM could be applicable to both monoliths and columns packed with porous particles. The PPM and PNM proposed in this work are able to predict the existence of the second inflection point in the experimental exclusion curve that has been observed for monolithic materials by accounting for volume partitioning of the polymer standards in the macropores of the column. The appearance and prominence of the second inflection …
Textural characterization of native and n-alky-bonded silica monoliths by mercury intrusion/extrusion, inverse size exclusion chromatography and nitr…
2008
Native and n-alkyl-bonded (n-octadecyl) monolithic silica rods with mesopores in the range between 10 and 25 nm and macropores in the range between 1.8 and 6.0 microm were examined by mercury intrusion/extrusion, inverse size exclusion chromatography (ISEC) and nitrogen sorption. Our results reveal very good agreement for the mesopore size distribution obtained from nitrogen adsorption (in combination with an advanced NLDFT analysis) and ISEC. Our studies highlight the importance of mercury porosimetry for the assessment of the macropore size distribution and show that mercury porosimetry is the only method which allows obtaining a combined and comprehensive structural characterization of m…
Spherical ordered mesoporous silicas and silica monoliths as stationary phases for liquid chromatography
2006
Ordered mesoporous silicas such as micelle-templated silicas (MTS) feature unique textural properties in addition to their high surface area (approximately 1000 m2/g): narrow mesopore size distributions and controlled pore connectivity. These characteristics are highly relevant to chromatographic applications for resistance to mass transfer, which has never been studied in chromatography because of the absence of model materials such as MTS. Their synthesis is based on unique self-assembly processes between surfactants and silica. In order to take advantage of the perfectly adjustable texture of MTS in chromatographic applications, their particle morphology has to be tailored at the microme…
Development of Methods for the Classification of EVOOs According to Their Geographical Origin
2012
The aim of this work was to obtain the phenolic profiles of EVOOs by using a CEC method, and to evaluate the use of these profiles in the prediction of the geographical origin of these EVOO samples. For this purpose, monolithic columns containing LA and BDDA monomers were constructed.
Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography
2017
[EN] In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch®), or mixtures of H2O2 and H2SO4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification…