Search results for "Emt"
showing 10 items of 413 documents
Synthesis of spherical porous silicas in the micron and submicron size range: challenges and opportunities for miniaturized high-resolution chromatog…
2000
Classical silica technology has reached its limit with respect to an ultimate minimum particle size of about 2 microm in diameter. Here, a novel process is presented which allows one to synthesize porous silica beads and control their particle diameter in situ, within the range of 0.2-2.0 microm. As a result, no sizing is required and losses of silica are avoided. Furthermore, the process enables one to control in situ the pore structural parameters and the surface chemistry of the silica beads. Even though surface funtionalized silicas made according to this process can principally be applied in fast HPLC the column pressure drop will be high even for short columns. In addition, the column…
Gas–solid chromatographic separation of hydrogen isotopes: a comparison between two palladium bearing materials – alumina and kieselguhr
1998
The separation of hydrogen isotopes (H, D, T) is performed by displacement gas chromatography on palladium. A large isotopic effect is associated with the reversible adsorption of hydrogen by palladium. Two Pd support materials have been compared: alpha-alumina and kieselguhr. The study includes a physicochemical characterization and a set of functional tests. The Van Deemter model gives a fairly good analysis of the process but to get more information, thermoregulated separations are needed. For both supports, palladium is impregnated as small dispersed particles in the 0.1 to 0.3 μm range diameter. For the same palladium loading, alumina is more efficient than kieselguhr.
Photo-polymerized lauryl methacrylate monolithic columns for CEC using lauroyl peroxide as initiator
2009
Lauryl methacrylate (LMA)-ester based monolithic columns photo-polymerized using lauroyl peroxide (LPO) as initiator were prepared, and their morphological and CEC properties were studied. The composition of the polymerization mixture (i.e. ratios of monomers/porogenic solvents, 1,4-butanediol/1-propanol and LMA/crosslinker) was optimized. The morphological and chromatographic properties of LMA columns were evaluated by means of SEM pictures and van Deemter plots of PAHs, respectively. The polymerization mixture selected as optimal provided a fast separation of a mixture of PAHs with excellent efficiencies (minimum plate heights of 8.9-11.1 μm). Satisfactory column-to-column (RS D < 4.5%) a…
Comparison on photo-initiators for the preparation of methacrylate monolithic columns for capillary electrochromatography.
2010
The synthesis of lauryl methacrylate monoliths for capillary electrochromatography by UV polymerization using several free-radical initiators (alpha,alpha'-azobisisobutyronitrile, 2,2-dimethoxy-2-phenylacetophenone, dibenzoyl peroxide (BPO) and lauroyl peroxide (LPO)) has been investigated. Using a 1,4-butanediol/1-propanol mixture as porogenic solvent, the influence of each initiator and its content on the morphological and electrochromatographical properties of beds was evaluated. Under their respective optimum content, satisfactory separations of a test mixture of PAHs with similar efficiencies (minimum plate heights of 8.0-12.7 microm obtained from Van Deemter plots) were achieved for t…
CEC column behaviour of butyl and lauryl methacrylate monoliths prepared in non-aqueous media
2009
Polymeric monolithic stationary phases for capillary electrochromatography were prepared using two bulk monomers, butyl methacrylate (BMA) and lauryl methacrylate (LMA), by in situ polymerization in non-aqueous media. The effect of 1,4-butanediol/1-propanol ratio on porous properties was investigated separately for each monomer, keeping the proportion of monomers to pore-forming solvents fixed at 40:60 wt:wt. Also, mixtures of BMA and LMA at different 1,4-butanediol/1-propanol ratios were studied for tailoring the morphological features of the monolithic columns. The chromatographic performance of the different columns was evaluated by means of van Deemter plots of polycyclic aromatic hydro…
Adsorbents and columns in analytical high-performance liquid chromatography: A perspective with regard to development and understanding
2012
A brief historical survey is presented on the evaluation of silica adsorbents in analytical HPLC. The theory of analytical HPLC is mostly still being based on the height equivalent to a theoretical plate concept and the van Deemter equation that was derived from gas phase adsorption involving a linear adsorption isotherm and fast mass transfer kinetics. One can obviously wonder whether the use of the van Deemter equation is relevant and valid for the evaluation of the performance of HPLC systems, where most often the liquid solutes involve charged molecules in electrolytes and in very many cases the adsorbates are macromolecules having diffusion coefficients of small magnitude. Instead of t…
Study of the column efficiency using gradient elution based on Van Deemter plots.
2018
Performance of chromatographic columns is of major importance in the development of more efficient separation methods. So far, a common practice is to study the column behavior in isocratic elution by modifying the flow rate and fitting the theoretical plate height values versus the mobile phase linear velocity, according to the Van Deemter equation. In this work, an approach is presented to extend the measurement of efficiency to linear gradient elution, where the mean retention factor is kept constant at each assayed flow. This avoids a possible source of uncertainty due to the change in the distribution equilibria profile, and makes the mean interactions with the stationary phase in grad…
Simultaneous optimization of mobile phase composition, column nature and length to analyse complex samples using serially coupled columns
2013
Abstract The combination of the selectivity of different columns serially coupled improves the separation expectancies with regard to the separation offered by each single column. In the reported approaches, either a pre-selected isocratic mobile phase composition or gradient program, giving rise to acceptable retention, is used. In previous work (JCA 1281 (2013) 94), we showed that the approach succeeds with conventional columns, assembled through zero-dead volume couplers. In this work, the simultaneous interpretive optimization of mobile phase composition and column nature and length, based on a limited number of experimental data, is demonstrated. This approach allows an impressive redu…
Prediction of Peak Shape and Characterization of Column Performance in Liquid Chromatography as a Function of Flow Rate
2015
Traditionally, column performance in liquid chromatography has been studied using information from the elution of probe compounds at different flow rates through van Deemter plots, which relate the column plate height to the linear mobile phase velocity. A more recent approach to characterize columns is the representation of the peak widths (or the right and left peak half-widths) for a set of compounds versus their retention times, which, for isocratic elution, give rise to almost linear plots. In previous work, these plots have been shown to facilitate the prediction of peak profiles (width and asymmetry) with optimization purposes. In this work, a detailed study on the dependence of the …
Femtometer accuracy EXAFS measurements: Isotopic effect in the first, second and third coordination shells of germanium
2009
The analysis of the EXAFS signals from 70Ge and 76Ge has evidenced the low-temperature effect of isotopic mass difference on the amplitude of relative atomic vibrations. This effect is reflected in the difference of the Debye-Waller factors of the first three coordination shells, and on the difference of nearest-neighbour average interatomic distances, evaluated with femtometer accuracy. The experimental results are in agreement with theoretical expectations.