Pore structural characteristics, size exclusion properties and column performance of two mesoporous amorphous silicas and their pseudomorphically transformed MCM-41 type derivatives

Highly ordered mesoporous silicas such as, mobile composition of matter, MCM-41, MCM-48, and the SBA-types of materials have helped to a large extent to understand the formation mechanisms of the pore structure of adsorbents and to improve the methods of pore structural characterization. It still remains an open question whether the high order, the regularity of the pore system, and the narrow pore size distribution of the materials will lead to a substantial benefit when these materials are employed in liquid phase separation processes. MCM-41 type 10 microm beads are synthesized following the route of pseudomorphic transformation of highly porous amorphous silicas. Highly porous silicas a…

Pore structural characterization of monolithic silica columns by inverse size-exclusion chromatography

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 …

ChemInform Abstract: Liquid Chromatography - Its Development and Key Role in Life Science Applications

Liquid chromatographic methods cover the broadest range of appli- cations imaginable today. Nowhere is this more evident and relevant than in the life sciences, where identification of target substances relevant in disease mechanisms is performed down to the femtomole level. On the other hand, purification of therapeutic drugs on a multi- ton scale is performed by process LC. The complexity and abundance range of biological systems in combination with the extreme purity requirements for drug manufacturing are the challenges that can be mastered today by chromatography, after more than a century of research and development. However, significant improvement is still required for a better unde…

Flow-through pore characteristics of monolithic silicas and their impact on column performance in high-performance liquid chromatography

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…

Liquid chromatography--its development and key role in life science applications.

Liquid chromatographic methods cover the broadest range of appli- cations imaginable today. Nowhere is this more evident and relevant than in the life sciences, where identification of target substances relevant in disease mechanisms is performed down to the femtomole level. On the other hand, purification of therapeutic drugs on a multi- ton scale is performed by process LC. The complexity and abundance range of biological systems in combination with the extreme purity requirements for drug manufacturing are the challenges that can be mastered today by chromatography, after more than a century of research and development. However, significant improvement is still required for a better unde…

Flüssigkeitschromatographie - ihre Entwicklung und Bedeutung für die Lebenswissenschaften

Flussigkeitschromatographische Methoden umfassen den breitest heute vorstellbaren Anwendungsbereich. Dies wird nirgendwo so deutlich wie in den Lebenswissenschaften, wenn es darum geht, Krankheitsmechanismen aufzuklaren und komplexe Gemische bis in den Femtomol-Bereich zu analysieren. Auf der anderen Seite besteht Bedarf an hochreinen therapeutischen Wirkstoffen, die als Pharmaka auf den Markt kommen und hohen Reinheitsanforderungen genugen mussen. Diese Aufreinigung wird mithilfe der Prozesschromatographie im Tonnenmasstab bewerkstelligt. Die hohe Komplexitat und breiten Konzentrationsbereiche biologischer Systeme in Kombination mit den extremen Reinheitsanforderungen der Arzneimittelprodu…

Characterization of the Pore Structure of Monolithic Silicas

Liquid intrusion and alternative methods for the characterization of macroporous materials (IUPAC Technical Report)

This document deals with the characterization of porous materials having pore widths in the macropore range of 50 nm to 500 μm. In recent years, the development of advanced adsorbents and catalysts (e.g., monoliths having hierarchical pore networks) has brought about a renewed interest in macropore structures. Mercury intrusion–extrusion porosimetry is a well-established method, which is at present the most widely used for determining the macropore size distribution. However, because of the reservations raised by the use of mercury, it is now evident that the principles involved in the application of mercury porosimetry require reappraisal and that alternative methods are worth being listed…

Textural characterization of native and n-alky-bonded silica monoliths by mercury intrusion/extrusion, inverse size exclusion chromatography and nitrogen adsorption

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…

Impact of pore structural parameters on column performance and resolution of reversed-phase monolithic silica columns for peptides and proteins

In this work, monolithic silica columns with the C4, C8, and C18 chemistry and having various macropore diameters and two different mesopore diameters are studied to access the differences in the column efficiency under isocratic elution conditions and the resolution of selected peptide pairs under reversed-phase gradient elution conditions for the separation of peptides and proteins. The columns with the pore structural characteristics that provided the most efficient separations are then employed to optimize the conditions of a gradient separation of a model mixture of peptides and proteins based on surface chemistry, gradient time, volumetric flow rate, and acetonitrile concentration. Bo…

Particle packed columns and monolithic columns in high-performance liquid chromatography-comparison and critical appraisal

The review highlights the fundamentals and the most prominent achievements in the field of high-performance liquid chromatography (HPLC) column development over a period of nearly 50 years. After a short introduction on the structure and function of HPLC columns, the first part treats the major steps and processes in the manufacture of a particle packed column: synthesis and control of particle morphology, sizing and size analysis, packing procedures and performance characterization. The next section is devoted to three subjects, which reflect the recent development and the main future directions of packed columns: minimum particle size of packing, totally porous vs. core/shell particles an…