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1.
Preparation of enantiomers using high pressure technologies
Paul Thorey, 2010, dissertation

Abstract: The study of two different methods of obtaining chiral alcohols is proposed herein. The requirement of the relatively new paradigm of green chemistry associated with clean technologies such as biocatalysis or non-conventional solvents, dense gases, was focused at. Indeed, the two methods of production of chiral alcohols were: - the conversion of acetophenone into (R)-1-phenylethanol in dense gases catalysed by Lactobacillus brevis alcohol dehydrogenase and its coenzyme, NADP/H; - the resolution of (±)-trans-1,2-cyclohexanediol by cocrystal formation with tartaric acid followed by supercritical extraction. In both cases high enantiopurities were achieved (ee>99%).
Keywords: High-pressure technologies, enantiomers, green chemistry, R-1-phenylethanol, Lactobacillus brevis, alcohol dehydrogenase, NADP, liquid propane, enzyme deactivation, resolution, trans-1, 2-cyclohexanediol, tartaric acid, cocrystal, supercritical carbon dioxide, extraction, X-ray diffraction, differential scanning calorimetry
Published: 02.02.2011; Views: 2004; Downloads: 64
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2.
Highly porous open-cellular monoliths from 2-hydroxyethyl methacrylate based high internal phase emulsions (HIPEs) : preparation and void size tuning
Sebastijan Kovačič, Dejan Štefanec, Peter Krajnc, 2007, original scientific article

Abstract: Preparation of highly porous (up to 80% pore volume) open-cellular monolithic cross-linked polymers from 2-hydroxyethyl methacrylate is reported. Oil-in-water and water-in-oil high internal phase emulsions are applied as porosity templates, resulting in an interconnected porous structure with void diameters between 550 nm and 18 m. Significantly larger voids were obtained inthe case of oil-in-water emulsions (between 5 and 18 m) as opposed to water in oil emulsions (approx 600 nm). Controlled coarsening exploiting limited kinetical stability of emulsions was used to obtain monoliths with larger voids, diameters being enlarged 3-fold.
Keywords: organic chemistry, polymerization, monolithic polymers, HIPE, emulsions, porous materials, methacrylates
Published: 31.05.2012; Views: 1185; Downloads: 25
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3.
Evaluation of analytical methods for the determination of free formaldehyde on textile substrate
Bojana Vončina, Alenka Majcen Le Marechal, Darinka Brodnjak-Vončina, 2007, original scientific article

Abstract: Release of formaldehyde from durable press-treated fabrics is a problem for human health and safety because formaldehyde is suspected to be carcinogenic. The accuracy of the standard test method for the free formaldehyde determination, Japan Law 112, depends on the formaldehyde content of the sample. The detection of low formaldehyde contents is particularly important in fields, like children clothing, so the application of high-performance liquid chromatography was evaluated. The results obtained by the standard testmethod, Japan Law 112, where UV/Vis spectrometer was used, were compared with the results obtained by HPLC method in which separation was performed on an RP C18 column with water-methanol as a mobile phase. It was shown that the detection limit and limit of quantification were improved using the HPLC method.
Keywords: analizna kemija, formaldehid, določevanje formaldehida, celulozna vlakna, HPLC, UV/VIS, analytical chemistry, formaldehyde, determination of formaldehyde, cellulose fibres, HPLC, UV/VIS
Published: 31.05.2012; Views: 1515; Downloads: 35
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4.
Oil-in-water high internal phase emulsions for porous monolithic polymers
Peter Krajnc, Dejan Štefanec, 2005, published scientific conference contribution abstract

Abstract: Porous monolithic polymers are objects of many studies recently due to their wide applicability. Especially in separation methods use of monoliths is growing. Usually, porous monoliths are prepared by bulk polymerisation with the use of porogenic solvents. An alternative way of preparation is to polymerise the continuous phase of an emulsion. When the volume fraction of the internal phase exceeds 74%, the emulsion is called a HIPE (high internal phase emulsion), and a polymer derived from it, a PolyHIPE. PolyHIPEs of styrene, vinylbenzyl chloride and acrylate chemistry have been prepared from awater in oil emulsion system, where monomers are dissolved in the organic phase. We describe the reversed procedure, an oil in water high internal phaseemulsion, where monomers are water soluble. Porous polymers based on acrylic acid and crosslinked with methylenebisacrylamide were prepared by using a high internal phase emulsion with toluene as the oil phase. The influence of initiator and surfactant on the morphology was studied.
Keywords: organic chemistry, porous monolith polymers, polymer supports, preparation, emulsion polymerization, HIPE
Published: 01.06.2012; Views: 1454; Downloads: 47
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5.
Aryl acrylate based high-internal-phase emulsions as precursors for reactive monolithic polymer supports
Peter Krajnc, Dejan Štefanec, Jane F. Brown, Neil R. Cameron, 2005, original scientific article

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 approximately3-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 thenitrophenyl 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 themore porous polymer.
Keywords: organic chemistry, macroporous polymers, monolithic polymer supports, emulsion polymerisation, foams, functionalization of polymers, high-internal-phase emulsions
Published: 01.06.2012; Views: 1078; Downloads: 32
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6.
Preparation and characterization of poly(high internal phase emulsion) methacrylate monoliths and their application as separation media
Peter Krajnc, Nermina Leber, Dejan Štefanec, Sandra Kontrec, Aleš Podgornik, 2005, original scientific article

Abstract: Poly(glycidyl methacrylate-co-ethyleneglycol dimethacrylate) monolithic supports were prepared by radical polymerisation of the continuous phase of water in oil high internal phase emulsions. Morphology of monolithic materialswas studied by scanning electron microscopy and mercury intrusion porosimetry. The ratio of phase volume and the degree of crosslinking influenced the void size and pore size distribution of resulting polymers. Void sizes between 1 and 10 m were observed and average pore sizes around 100nm. Polymers with 60, 75, 80 and 90% pore volume were prepared and even samples with highest pore volume showed good mechanical stability. They were modified to bear weak-anion exchange groups and tested on the separation of standard protein mixture containing myoglobin, conalbumine and trypsin inhibitor. Good separation was obtained in a very short time similar to the separation obtained by commercial methacrylate monoliths. However, higher dispersion was observed. Bovine serum albumin dynamic binding capacity for monolith with 90% porosity was close to 9 mg/ml.
Keywords: organic chemistry, methacrylate monoliths, preparation, emulsion polymerization, high porosity, high mechanical stability, polymer chromatographic supports, monolithic methacrylate supports, protein separation
Published: 01.06.2012; Views: 1252; Downloads: 23
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7.
Sol-gel-based optical sensor for the detection of aqueous amines
Špela Korent Urek, Aleksandra Lobnik, Gerhard J. Mohr, 2007, original scientific article

Abstract: We present an optical sensor for the detection of aqueous amines obtained by incorporating chromoionophore XV (ETHT 4001) into sol-gel thin films. Acid- and base-catalyzed sol-gel processes were studied to prepare stable ormosil layers using various amounts of organically modified sol-gel precursor such asmethyltriethoxysilane (MTriEOS). The sensor layers were coated with a protective layer of microporous white polytetrafluoroethylene (PTFE) in order to prevent interference from ions and ambient light. The measurements were carried out in a flow-through cell in the reflection mode. Acid-catalyzed ormosil layers (pH 1) based on the copolymerization of tetraethoxysilane (TEOS) and MTriEOS did not show any change in signal upon exposure to aqueous amine solutions, while base-catalyzed sensor layers (pH 3 and 13) showed significant changes in signal. The response time (t100) for the base-catalyzedsensor layer L3 (pH 13) upon exposure to different solutions containing 0-608 mmol L-1 aqueous propylamine was 20-30 s, the regeneration time was 70 s and the detection limit was 0.1 mmol L-1. The sensor response was reproducible and reversible. The porous ormosil layers permit dry sensor storage conditions.
Keywords: analytical chemistry, optical sensors, sol-gel technology, determination of amines, fluorimetry
Published: 01.06.2012; Views: 1454; Downloads: 30
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8.
Hydroxylammonium fluorogermanates
Irena Ban, Matjaž Kristl, Mihael Drofenik, Arkadije Popović, 2004, original scientific article

Abstract: A new hydroxylammonium compound (NH3OH)2GeF6, has been synthesized by the addition of solid NH3OHF to a solution of GeO2 dissolved in 20% HF. The compound was characterized by chemical analysis and X-ray powder diffraction, the thermal decomposition was studied by thermal analysis and mass spectrometry. (NH3OH)2GeF6 crystallizes monoclinic. Two endothermic and two exothermic peaks have been observed on the DSC curve, the decomposition product at 500 °C is GeO2.
Keywords: inorganic chemistry, synthesis, characterisation, hydroxylammonium fluorogermanates, x-ray powder diffraction, mass spectroscopy, thermal analysis
Published: 01.06.2012; Views: 1162; Downloads: 22
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9.
Experiential learning - a case on diapers' polymers
Nika Golob, 2012, original scientific article

Abstract: The development of science competences requires establishing a link between theory and real world experience. Experiential learning offers the possibility for developing effective science competences as well as specific chemical competences at different stages of the educational vertical. The experiential learning strategy was implemented through experimental work and the cooperative learning method. Students studied diapers' polymers during chemistry class. The results of the case study analysis confirm better motivation for studying chemistry when material from everyday life is used as an educational prop. In order to monitor development levels of individual student competences, a set of instruments which includes monitoring dialogic teaching should be further developed.
Keywords: education, chemistry, experiential learning, science competences, experimental work
Published: 07.06.2012; Views: 836; Downloads: 22
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10.
Chiral discrimination in mobile phases for HPLC
Renato Lukač, Andrew J. Clark, Syma Khalid, Alison Rodger, Alan Snedden, P. Mark Rodger, 2002, original scientific article

Abstract: In this paper we present an algorithm and some preliminary results of a computer simulation study designed to elucidate the molecular interaction mechanisms associated with chiral discrimination in chiral high performance liquid chromatography (HPLC). Molecular dynamics simulations have been performed on a novel active stationary phase constituent based on disaccharides and a model analyte in a typical solvent used as mobile phase in chiral HPLC. The results are interpreted in terms of typical binding geometries and energies found from the simulations. This paper provides basic algorithms for predicting enantiometric selectivity and for investigating the implications for choice of parameters such as solvent polarity and temperature for optimising chiral HPLC separations
Keywords: physical chemistry, liquid crystals, liquid chromatography, computer simulations, spectroscopy
Published: 07.06.2012; Views: 715; Downloads: 8
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