Monolithic Materials (monolithic + material)

Distribution by Scientific Domains


Selected Abstracts


Ring-Opening Metathesis Polymerization Based Post-Synthesis Functionalization of Electron Beam Curing Derived Monolithic Media

MACROMOLECULAR RAPID COMMUNICATIONS, Issue 21 2007
Rajendar Bandari
Abstract Monolithic materials were prepared via electron-beam curing from ethyl methacrylate, trimethylolpropane triacrylate, and norborn-5-ene-2-ylmethyl acrylate. Reaction of the norborn-2-ene groups with either RuCl2(PCy3)2(CHPh) (1) or RuCl2(PCy3)(1,3-dimesityl-4,5-dihydroimidazol-2-inylidene)(CHPh) (2) resulted in the surface attachment of the initiators. The extent of initiator immobilization was found to be substantially higher for 1 than for 2. Reaction of the surface immobilized initiators with various monomers resulted in the desired surface modification of EB-derived monoliths. The amounts of grafted monomer were determined by elemental analysis and ICP-OES. [source]


Integrated microdevice for preconcentration and separation of a wide variety of compounds by electrochromatography

ELECTROPHORESIS, Issue 3 2009
Gaelle Proczek
Abstract An integrated microdevice was developed to couple on-chip SPE to separation by channel electrochromatography. An acrylate-based monolith was synthesized within a glass microdevice by photoinitiated polymerization. It was used for both separation and preconcentration by direct injection on the head of the stationary phase or by confining the preconcentration step in a given zone of the stationary phase. The composition of the polymerization mixture was chosen to achieve a monolithic material containing both hydrophobic and charged moieties to ensure an electroosmotic flow for separation. As a consequence the extraction procedure occurs via hydrophobic and ionic interactions. Neutral, ionizable and charged compounds were successfully preconcentrated and separated within the microdevice through electrochromatographic mechanisms, highlighting the versatility of this device. The performance of the integrated microdevice was demonstrated with the preconcentration and separation of a mixture of PAHs for which a signal enhancement factor (SEF) of 270 was achieved within 120,s of preconcentration. In the case of charged and ionizable compounds, according to the electrolyte composition, contributions of both reverse-phase and ion-exchange mechanisms were used to perform effective electrochromatographic preconcentration. A SEF of 250 was obtained for the model-charged compound within 20,s of preconcentration. Finally, the potentials of on-chip preconcentrate and separate both neutral and ionized compounds have been demonstrated using a mixture of model compounds. [source]


Solid phase peptide synthesis on epoxy-bearing methacrylate monoliths

JOURNAL OF PEPTIDE SCIENCE, Issue 12 2004
E. Vlakh
Abstract Monoliths based on a copolymer of glycidyl methacrylate (GMA) and ethylene dimethacrylate (EDMA) can be used directly as sorbents for affinity chromatography after solid phase peptide synthesis. The quality of the synthesized products, the amount of grown peptides on a support and the reproducibility of the process must be considered. A determination of the quantity of the introducing ,-Ala (and, consequently, the total amount of synthesized peptide) was carried out. Three peptides complementary to recombinant tissue plasminogen activator (t-PA) have been synthesized using Fmoc-chemistry on GMA-EDMA disks. The peptidyl ligands were analysed by amino acid analysis, ES-MS and HPLC methods. The affinity binding parameters were obtained from frontal elution data. The results were compared with those established for GMA-EDMA affinity sorbents formed by the immobilization of the same but separately synthesized and purified ligands. The immobilization on GMA-EDMA disks was realized using a one-step reaction between the amino groups of the synthetic ligand and the original epoxy groups of monolithic material. The affinity constants found for two kinds of sorbent did not vary significantly. Finally, the directly obtained affinity sorbents were tested for t-PA separation from a cellular supernatant. Copyright © 2004 European Peptide Society and John Wiley & Sons, Ltd. [source]


Porous polymer monolith for surface-enhanced laser desorption/ionization time-of-flight mass spectrometry of small molecules

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 13 2004
Dominic S. Peterson
Porous poly(butyl methacrylate- co -ethylene dimethacrylate), poly(benzyl methacrylate- co -ethylene dimethacrylate), and poly(styrene- co -divinylbenzene) monoliths have been prepared on the top of standard sample plates used for matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry and the modified plates were used for laser desorption/ionization mass spectrometry (LDI-MS). The hydrophobic porous surface of these monoliths enables the transfer of sufficient energy to the analyte to induce desorption and ionization prior to TOFMS analysis. Both UV and thermally initiated polymerization using a mask or circular openings in a thin gasket have been used to define spot locations matching those of the MALDI plates. The desorption/ionization ability of the monolithic materials depends on the applied laser power, the solvent used for sample preparation, and the pore size of the monoliths. The monolithic matrices are very stable and can be used even after long storage times in a typical laboratory environment without observing any deterioration of their properties. The performance of the monolithic material is demonstrated with the mass analysis of several small molecules including drugs, explosives, and acid labile compounds. The macroporous spots also enable the archiving of samples. Copyright © 2004 John Wiley & Sons, Ltd. [source]


Multi-Criteria Material Selection of Monolithic and Multi-Materials in Engineering Design

ADVANCED ENGINEERING MATERIALS, Issue 1-2 2006
P. Sirisalee
Multi-materials are combinations of monolithic materials in a chosen configuration and scale. They can help populate the material property space and fill areas monolithic materials cannot reach. This paper presents a novel approach to compare the performance of monolithic materials and multi-materials in multi-criteria design problems, with the results being visualised through exchange constant charts. In this paper, a particular type of multi-materials, sandwich panels, is selected to demonstrate the approach. [source]


Aryl acrylate based high-internal-phase emulsions as precursors for reactive monolithic polymer supports

JOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 2 2005
Peter Krajnc
Abstract Water-in-oil high-internal-phase emulsions (HIPEs), containing 4-nitrophenyl acrylate and 2,4,6-trichlorophenyl acrylate as reactive monomers, were prepared and polymerized, and highly porous monolithic materials resulted. The novel materials were studied by combustion analysis, Fourier transform infrared spectroscopy scanning electron microscopy, mercury porosimetry, and N2 adsorption/desorption analysis. With both esters, cellular macroporous monolithic polymers were obtained; the use of 4-nitrophenyl acrylate resulted in a cellular material with void diameters between 3 and 7 ,m and approximately 3-,m interconnects, whereas the use of 2,4,6-trichlorophenyl acrylate yielded a foam with void diameters between 2 and 5 ,m, most interconnects being around 1 ,m. The resulting monoliths proved to be very reactive toward nucleophiles, and possibilities of functionalizing the novel polymer supports were demonstrated via reactions with amines bearing additional functional groups and via the synthesis of an acid chloride derivative. Tris(hydroxymethyl)aminomethane and tris(2-aminoethyl)amine derivatives were obtained. The hydrolysis of 4-nitrophenylacrylate removed the nitrophenyl group, yielding a monolithic acrylic acid polymer. Furthermore, functionalization to immobilized acid chloride was performed very efficiently, with more than 95% of the acid groups reacting. The measurement of the nitrogen content in 4-nitrophenyl acrylate poly(HIPE)s after various times of hydrolysis showed the influence of the total pore volume of the monolithic polymers on the velocity of the reaction, which was faster with the more porous polymer. © 2004 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 296,303, 2005 [source]


Macroporous molecularly imprinted monolithic polymer columns for protein recognition by liquid chromatography

JOURNAL OF SEPARATION SCIENCE, JSS, Issue 17-18 2010
Jinxiang Liu
Abstract Macroporous cytochrome c (cyc)-imprinted monolithic polyarylamide columns were prepared, and applied for the template protein recognition by HPLC. With cyc (18.8,mg) as template, the imprinted monolithic materials were in situ polymerized in an HPLC column tube, with methacrylamide (450,mg), methacrylic acid (15.8,mg), piperazine diacrylamide (720,mg) and ammonium sulfate (390,mg) dissolved in 5,mL of phosphate buffer (pH 7.4), initiated by ammonium persulfate and TEMED. After the reaction, cyc was removed with acetic acid (10%, v/v) containing 10%,w/v SDS. The non-imprinted monolithic column was prepared under the same procedure except without cyc. Retention of cyc and its competitive protein, lysozyme (lys), on molecular-imprinting polymer (MIP) and non-imprinted polymer columns was studied. When the pH value of mobile phase was 4.0, on MIP column, the retention factors of cyc and lys were 2.0 and 1.3, respectively. However, those on non-imprinted polymer column were very similar, both as 1.1. Even in competitive environment, a mixture of cyc and lys could be separated on MIP column under gradient elution, with resolution as 1.2. These results indicate that protein-imprinted monolithic polymer columns could offer obvious affinity and specific recognition to the template protein. [source]


Bioaffinity chromatography on monolithic supports

JOURNAL OF SEPARATION SCIENCE, JSS, Issue 3 2010
Kishore K. R. Tetala
Abstract Affinity chromatography on monolithic supports is a powerful analytical chemical platform because it allows for fast analyses, small sample volumes, strong enrichment of trace biomarkers and applications in microchips. In this review, the recent research using monolithic materials in the field of bioaffinity chromatography (including immunochromatography) is summarized and discussed. After giving an introduction into affinity chromatography, information on different biomolecules (antibodies, enzymes, lectins, aptamers) that can act as ligands in bioaffinity chromatography is presented. Subsequently, the history of monoliths, their advantages, preparation and formats (disks, capillaries and microchips) as well as ligand immobilization techniques are mentioned. Finally, analytical and preparative applications of bioaffinity chromatography on monoliths are presented. During the last four years 37 papers appeared. Protein A and G are still most often used as ligands for the enrichment of immunoglobulins. Antibodies and lectins remain popular for the analysis of mainly smaller molecules and saccharides, respectively. The highly porous cryogels modified with ligands are applied for the sorting of different cells or bacteria. New is the application of aptamers and phages as ligands on monoliths. Convective interaction media (epoxy CIM disks) are currently the most used format in monolithic bioaffinity chromatography. [source]


Preparation and HPLC applications of rigid macroporous organic polymer monoliths

JOURNAL OF SEPARATION SCIENCE, JSS, Issue 10-11 2004
Frantisek Svec
Abstract Rigid porous polymer monoliths are a new class of materials that emerged in the early 1990s. These monolithic materials are typically prepared using a simple molding process carried out within the confines of a closed mold. For example, polymerization of a mixture comprising monomers, free-radical initiator, and porogenic solvent affords macroporous materials with large through-pores that enable applications in a rapid flow-through mode. The versatility of the preparation technique is demonstrated by its use with hydrophobic, hydrophilic, ionizable, and zwitterionic monomers. Several system variables can be used to control the porous properties of the monolith over a broad range and to mediate the hydrodynamic properties of the monolithic devices. A variety of methods such as direct copolymerization of functional monomers, chemical modification of reactive groups, and grafting of pore surface with selected polymer chains is available for the control of surface chemistry. Since all the mobile phase must flow through the monolith, the convection considerably accelerates mass transport within the molded material, and the monolithic devices perform well, even at very high flow rates. The applications of polymeric monolithic materials are demonstrated mostly on the separations in the HPLC mode, although CEC, gas chromatography, enzyme immobilization, molecular recognition, advanced detection systems, and microfluidic devices are also mentioned. [source]


Preface: phys. stat. sol. (b) 245/3

PHYSICA STATUS SOLIDI (B) BASIC SOLID STATE PHYSICS, Issue 3 2008
Christopher W. Smith
This is the third Special Issue of physica status solidi (b) focusing on materials with a negative Poisson's ratio or other ,anomalous' physical properties. This issue contains selected papers from the First International Conference on Auxetics and Anomalous Systems held at the University of Exeter, UK, on 4,6 September 2006. Around 50 participants from all over the world as well as from a wide range of scientific and engineering disciplines contributed to what was a highly successful conference. This conference follows in the footsteps of two previous workshops held at the Mathematical Research and Conference Centre in B,dlewo near Pozna,, Poland, in 2004 and 2005 [1, 2]. The papers selected for this issue publish recent results obtained for ,anomalous systems' in experiment, theory and computer simulations. In the following we summarize very briefly their contents. Alderson and Coenen compare the performance of auxetic composites to similar systems with conventional positive Poisson's ratios. They find that there are indeed differences which appear to arise from the change of the overall Poisson's ratio of the composite, some beneficial like a rise in impact tolerance at low impact rates, and others deleterious such as the reduced tolerance at higher impact rates. This is one of the first investigations of possible applications for auxetic materials. The two papers by Gaspar and Koenders both examine the effects of disorder upon anomalous properties, especially negative Poisson's ratio. In the first one Gaspar demonstrates how a mean strain estimate fails to predict negative values of Poisson's ratio because of an inability to account for local fluctuations in elastic properties. For instance it is shown that the volume fraction of auxetic regions in an globally auxetic material (measured experimentally) are smaller than a mean strain homogenisation would require. Koenders and Gaspar explore the elastic properties, and especially Poisson's ratio, of a heterogeneous 2D network of bending beams. They predict auxetic behaviour arising from localised disorder in the packing, and therefore effective locally aggregated elastic properties of the beams. In the three articles by Gatt et al. and Grima et al. models based on simple geometry are used to explain the behaviour of seemingly disparate systems, i.e. 2D honeycombs systems and zeolite SiO2 networks. Two papers concerning honeycombs demonstrate relationships between elastic properties and structure and the bounds for auxetic behaviour. The paper concerning the zeolite Natrolite uses numerical force field based energy minimisation methods to simulate the response of this particular zeolite to applied forces and then simplifies the predicted properties even further by considering structural units as rigid 2D polyhedra linked by flexible hinges. In a similar vein, though using a different approach and concerning a very different form of matter, Heyes shows how the heterogeneity in an assembly of particles in a liquid can affect the elastic properties of a liquid and notably the infinite frequency Poisson's ratio. Heyes uses the Molecular Dynamics approach to simulate a Lennard,Jones fluid under various pressures, notably comparing behaviour under positive and negative pressures. In their first paper Jasiukiewicz and co-authors derive elastic constants of 2D crystals for all four classes of 2D crystalline solids: hexagonal (isotropic), quadratic, rectangular, and oblique systems. In their second paper they demonstrate conditions required for auxetic behaviour of 2D crystals. Auxetic solids are further divided into those with some negative Poisson's ratios (auxetic), all negative Poisson's ratios (completely auxetic) and no negative Poisson's ratios (non-auxetic). Lakes and Wojciechowski consider counterintuitive properties of matter, like negative compressibility, negative Poisson's ratio, negative thermal expansion, negative specific heat, and negative pressure. They present and interpret experimental observations of negative bulk modulus in pre-strained foams. They propose also a constrained microscopic model which exhibits negative compressibility. Finally, they solve a very simple thermodynamic model with negative thermal expansion. Martin et al. take a long stride toward a real world application of auxetic materials with a wide ranging study starting with numerical modelling of a wingbox section to experimental testing in a wind tunnel. They show that an auxetic core in a wing box section can allow a passive aero-elastic response which can be tailored by careful design of the core so that camber, and thus drag, is reduced with increasing airspeed but without sacrificing structural integrity. Miller et al. consider another anomalous physical property, negative thermal expansivity, and its application in the form of particulate composites for amelioration of stresses arising from thermal mismatch. They show via experiments that particles with a negative coefficient of thermal expansion may be used as a composite reinforcer to reduce overall thermal expansion and behave according to the standard volume fraction based models. Narojczyk and Wojciechowski examine the effects of disorder upon the bulk elastic properties of 3D fcc soft sphere systems in terms of particle size. Systems, such as colloids, can be thought of in such terms. The study shows that higher order moments of probability distribution do not influence the bulk elastic properties much, but that lower moments such as the standard deviation of particle size influence the elastic properties greatly. The "hardness" of the particle interaction potential is also important in this context. In general, it is shown that the effect of increasing polydispersity is to increase the Poisson's ratio, except the [110] [10] directions. Scarpa and Malischewsky in their paper on Rayleigh waves in auxetic materials show how the Rayleigh wave speed is affected by the Poisson's ratio. The behaviour is complex and depends upon the homogeneity within the material, for instance slowing with decreasing Poisson's ratio in isotropic solids, but showing the reverse trend and increased sensitivity to Poisson's ratio in laminate composites. Scarpa et al. explore the buckling behaviour of auxetic tubes via three types of model, a simple beam mechanics and Eulerian buckling model, a 3D linear elastic FE model and a bespoke non-linear continuum model. The more sophisticated models provide increasing insight into the buckling behaviour though the simple beam model predicts reasonably well in the pre-buckling linear region. Some unexpected and interesting behaviour is predicted by the continuum model as the Poisson's ratio approaches the isotropic limit of ,1, including increasing sensitivity to Poisson's ratio and rapid mode jumping between integer wave numbers. The paper by Shilko et al. presents an analysis of a particular kind of friction joint, a double lap joint, and explores the effects of altering the elastic properties of one component, in particular it's Poisson's ratio. The manuscript introduces the evolution of smart materials from monolithic materials, and the classification of composites exhibiting negative Poisson's ratios. The paper then presents the case of a double lap joint and performs a sensitivity type study, via a 2D FE model, of the effects of changing the elastic properties and degree of anisotropy of one section of the model on various parameters defining the limits of functionality of the joint. The main finding is that an enhanced shear modulus, via a negative Poisson's ratio, can endow such a friction joint with superior performance. Manufacturing of auxetic materials on a commercial scale has proved to be the largest obstacle to their fuller exploitation. The paper by Simkins et al. explores one route for post processing of auxetic polymers fibres produced by a conventional melt extrusion route. Simkins et al. showed that a post process thermal annealing treatment, with carefully optimised parameters, was able to even out otherwise inhomogenous auxetic properties, and moreover improve other elastic and fracture properties often sacrificed for auxetic behaviour. We gratefully acknowledge the support given by the sponsors of the conference, namely the EPSRC of the UK and Auxetic Technologies Ltd. (UK). We also thank the Scientific Committee, the Organising Committee, and all the participants of the conference. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source]


Porous polymer monolith for surface-enhanced laser desorption/ionization time-of-flight mass spectrometry of small molecules

RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 13 2004
Dominic S. Peterson
Porous poly(butyl methacrylate- co -ethylene dimethacrylate), poly(benzyl methacrylate- co -ethylene dimethacrylate), and poly(styrene- co -divinylbenzene) monoliths have been prepared on the top of standard sample plates used for matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry and the modified plates were used for laser desorption/ionization mass spectrometry (LDI-MS). The hydrophobic porous surface of these monoliths enables the transfer of sufficient energy to the analyte to induce desorption and ionization prior to TOFMS analysis. Both UV and thermally initiated polymerization using a mask or circular openings in a thin gasket have been used to define spot locations matching those of the MALDI plates. The desorption/ionization ability of the monolithic materials depends on the applied laser power, the solvent used for sample preparation, and the pore size of the monoliths. The monolithic matrices are very stable and can be used even after long storage times in a typical laboratory environment without observing any deterioration of their properties. The performance of the monolithic material is demonstrated with the mass analysis of several small molecules including drugs, explosives, and acid labile compounds. The macroporous spots also enable the archiving of samples. Copyright © 2004 John Wiley & Sons, Ltd. [source]