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PubMedDate not supplied

A research on determination of explosive gases utilizing cataluminescence sensor array.

In this paper, we propose a model of a sensor array system, which consists of three cataluminescence sensors based on nanosized SrCO3, gamma-Al2O3 and BaCO3 as catalysts, for quantitative analysis of the explosive gases of propane, n-butane and iso-butane in a mixture. Six linear regression equations of the cataluminescence intensity vs. the gas concentrations in the range 2000-10,000 ppm were established from the sensor array system at two working temperatures, as the explosive gases show different sensitivity to the three sensors. The least squares method was employed for solving the simultaneous equations and quantifying the concentrations of the three components. The detection limits (3sigma) of propane, n-butane and iso-butane on SrCO3, gamma-Al2O3 and BaCO3 sensors are 50, 40 and 20 ppm, 80, 60 and 40 ppm, and 20, 10 and 5 ppm, respectively. The concentrations of two artificial samples containing the tertiary mixture were analysed with satisfactory results.

Aluminum Oxide↗
PubMed2002

Low-temperature electron microscopy for the study of polysaccharide ultrastructures in hydrogels. I. Theoretical and technical considerations.

The high-pressure freezing (HPF) technique was applied to the cryo-immobilization of alginate gels and the quality of the freezing analyzed on a TEM by comparison of the segregation pattern of samples of decreasing thickness. Dynamic simulations of heat transfer within an idealized slab of pure water surrounded by two walls of aluminium were performed to illustrate the effect of the heat-transfer coefficient by convection on the cooling rate of the sample. Heat-transfer coefficients in liquid nitrogen and liquid propane at ambient pressure were measured using a carefully characterized thermocouple and the values incorporated as parameters in heat-transfer simulations to compare the efficiency of the plunge-freezing technique with the high-pressure freezing technique. Values of the heat-transfer coefficient in liquid nitrogen and liquid propane, calculated between 273 K and 173 K were 670 and 18420 W/m(2)/K, respectively. Based on TEM observations and the results of heat-transfer simulations, the HPF technique was adapted to the cryo-fixation of 50-microm-thick alginate gels. The occurrence of artifacts was rejected because no differences were observed in the pattern of cryo-fixed and freeze-substituted samples of various thickness, with and without ethanol as cryo-protectant. A sample thickness of 50 microm was found to ensure an adequate preservation of structures as small as a few nanometers, as verified by TEM and SEM observations. Finally, DSC measurements on alginate solutions and alginate beads revealed that under the experimental conditions (0-3%), alginate cannot be considered to be an efficient cryo-protectant.

Alginates↗
PubMed2005

A density functional study on a biomimetic non-heme iron catalyst: insights into alkane hydroxylation by a formally HO-FeV=O oxidant.

The reactivity of [HO-(tpa)Fe(V)=O] (TPA=tris(2-pyridylmethyl)amine), derived from O-O bond heterolysis of its [H(2)O-(tpa)Fe(III)-OOH] precursor, was explored by means of hybrid density functional theory. The mechanism for alkane hydroxylation by the high-valent iron-oxo species invoked as an intermediate in Fe(tpa)/H(2)O(2) catalysis was investigated. Hydroxylation of methane and propane by HO-Fe(V)=O was studied by following the rebound mechanism associated with the heme center of cytochrome P450, and it is demonstrated that this species is capable of stereospecific alkane hydroxylation. The mechanism proposed for alkane hydroxylation by HO-Fe(V)=O accounts for the experimentally observed incorporation of solvent water into the products. An investigation of the possible hydroxylation of acetonitrile (i.e., the solvent used in the experiments) shows that the activation energy for hydrogen-atom abstraction by HO-Fe(V)=O is rather high and, in fact, rather similar to that of methane, despite the similarity of the H-CH(2)CN bond strength to that of the secondary C-H bond in propane. This result indicates that the kinetics of hydrogen-atom abstraction are strongly affected by the cyano group and rationalizes the lack of experimental evidence for solvent hydroxylation in competition with that of substrates such as cyclohexane.

Algorithms↗
PubMed2004

EPR studies of amine radical cations, part 1: thermal and photoinduced rearrangements of n-alkylamine radical cations to their distonic forms in low-temperature freon matrices.

The thermal and photochemical transformations of primary amine radical cations (n-propyl 1.+, n-butyl 5.+) generated radiolytically in freon matrices have been investigated by using low-temperature EPR spectroscopy. Assignment of the spectra was facilitated by parallel studies on the corresponding N,N-dideuterioamines. The identifications were supported by quantum chemical calculations on the geometry, electronic structure, hyperfine splitting constants and energy levels of the observed transient radical species. The rapid generation of the primary species by a short exposure (1-2 min) to electron-beam irradiation at 77 K allowed the thermal rearrangement of 1.+ to be monitored kinetically as a first-order reaction at 125-140 K by the growth in the well-resolved EPR signal of the distonic radical cation .C(2CH2CH2NH3+. By comparison, the formation of the corresponding .CH2CH2CH2CH2NH3+ species from 5.+ is considerably more facile and already occurs within the short irradiation time. These results directly verify the intramolecular hydrogen-atom migration from carbon to nitrogen in these ionised amines, a reaction previously proposed to account for the fragmentation patterns observed in the mass spectrometry of these amines. The greater ease of the thermal rearrangement of 5.+ is in accordance with calculations on the barrier heights for these intramolecular 1,5- and 1,4-hydrogen shifts, the lower barrier for the former being associated with minimisation of the ring strain in a six-membered transition state. For 1.+, the 1,4-hydrogen shift is also brought about directly at 77 K by exposure to approximately 350 nm light, although there is also evidence for the 1,3-hydrogen shift requiring a higher energy. A more surprising result is the photochemical formation of the H2C=N. radical as a minor product under hard-matrix conditions in which diffusion is minimal. It is suggested that this occurs as a consequence of the beta-fragmentation of 1.+ to the ethyl radical and the CH2=NH2+ ion, followed by consecutive cage reactions of deprotonation and hydrogen transfer from the iminonium group. Additionally, secondary ion-molecule reactions were studied in CFCl2CF2Cl under matrix conditions that allow diffusion. The propane-1-iminyl radical CH3CH2CH=N. was detected at high concentrations of the n-propylamine substrate. Its formation is attributed to a modified reaction sequence in which 1.+ first undergoes a proton transfer within a cluster of amine molecules to yield the aminyl radical CH3CH2CH2N.H. A subsequent disproportionation of these radicals can then yield the propane-1-imine precursor CH3CH2CH=NH, which is known to easily undergo hydrogen abstraction from the nitrogen atom. The corresponding butane-1-iminyl radical was also observed.

Journal Article↗
PubMed2006

Clean diesel power via microwave susceptible oxidation catalysts.

The problem of soot emissions from diesel engines is introduced and the possible solution of combining doped perovskites and microwave (mw) irradiation to "clean up" diesel soot filters is outlined. Eighteen doped perovskite catalysts are synthesized and tested for propane and CO oxidation, which are taken as model components for soot. The activity, selectivity, and SO2 tolerance are compared under conventional heating and mw irradiation. By combining mw irradiation and doped perovskites, one can create "hot spots" on the catalyst, resulting in efficient and selective heating of the active site, as well as less poisoning. Sr-doped and Ce-doped manganese perovskites show the highest activity. These catalysts are also the most selective, and have a high mw susceptibility. Optimal SO2 tolerance is displayed by Cr perovskites, from which the La0.8Ca0.2CrO3 combination uniquely converts propane before CO, and therefore can be used to remove >C2 hydrocarbons from a mix with CO. Possible mechanistic scenarios are presented and discussed.

Journal Article↗
PubMed1997

Effect of zwitterionic surfactants on the separation of proteins by capillary electrophoresis.

The effect of zwitterionic surfactants on capillary electrophoretic separation of proteins was investigated using an uncoated silica capillary column and different buffers containing zwitterionic surfactants. The effects of N-alkyl-N,N-dimethyl ammonio-1-propane-sulfonates on the electrophoretic mobility of three different proteins, namely albumin, lysozyme and myoglobin, were examined. The addition of N-alkyl-N,N-dimethylammonio-1-propane sulfonate in phosphate saline buffer is important in minimizing protein-capillary wall interactions, and facilitated an efficient electrophoretic mobility of myoglobin and lysozyme. The separation efficiency of proteins also depends on the injection pressure for the control of migration time and the peak sharpness. The electrophoretic conditions were applied to evaluate the separation of lysozyme, myoglobin and albumin. The zwitterion surfactants can form a dynamic coating on the capillary surface, thereby reducing the number of adsorption sites to which proteins may adsorb.

Albumins↗
PubMedDate not supplied

Sensitivity evaluation of the Daphtoxkit and Thamnotoxkit microbiotests on blind samples.

At the Oregon State University Workshop we utilized two "culture/maintenance-free" microbiotests, the Thamnotoxkit F with the anostracan crustacean Thamnocephalus platyurus and the Daphtoxkit F magna with the cladoceran crustacean Daphnia magna, to determine the toxicity of water samples in a blind format. The Thamnotoxkit was applied to 7 samples and the Daphtoxkit to 12 samples. The chemical composition of the water samples to which the Toxkit microbiotests had been applied was disclosed a posteriori by the organizers and appeared to contain chlordimeform, colchicine, phosdrin, mercuric chloride, sodium arsenite, metham sodium, sodium cyanide, trimethylol propane phosphate, p-chlorophenol and a natural sediment sample containing mercury. Three of the water samples were blanks that had not been spiked with chemicals. No false positives were obtained with the two Toxkits and all the toxic waters were earmarked as such by the microbiotests, except trimethylol propane phosphate, which was not found to induce acute effects in Daphnia magna in the non-diluted water sample containing 100 mg l(-1) of this compound.

Animals↗
PubMed2007

Biodegradation of high-toughness double network hydrogels as potential materials for artificial cartilage.

This study evaluated biodegradation properties of four novel high-toughness double network (DN) hydrogels as potential materials for artificial cartilage. Concerning each DN gel material, a total of 12 specimens were prepared, and 6 of the 12 specimens were examined to determine the mechanical properties without any treatments. The remaining 6 specimens were implanted into the subcutaneous tissue, using 6 mature female rabbits. At 6 weeks after implantation, the mechanical properties and the water content of the implanted specimens were measured. In the poly(2-acrylamide-2-methyl-propane sulfonic acid)/poly(N,N'-dimethyl acrylamide) DN gel, the ultimate stress and the tangent modulus were significantly increased from 3.10 and 0.20 MPa, respectively, to 5.40 and 0.37 MPa, respectively, with a significant reduction of the water content after implantation (94 to 91%). In the poly(2-acrylamide-2-methyl-propane sulfonic acid)/polyacrylamide DN gel and the cellulose/poly(dimethyl acrylamide) DN gel, the stress (11.4 and 1.90 MPa, respectively) and the modulus (0.30 and 1.70 MPa, respectively) or the water content rarely changed after implantation (90 and 85%, respectively). In the bacterial cellulose/gelatin DN gel, the ultimate stress was dramatically reduced from 4.30 to 1.98 MPa with a significant increase of the water content after implantation (78 to 86%). This study implied that these DN gels except for the cellulose/gelatin DN gel are potential materials that may meet the requirements of artificial cartilage.

Absorbable Implants↗
PubMed2004

A new resin matrix for dental composite having low volumetric shrinkage.

The applications of dental restorative composite resins containing 2,2 bis [4-(2-hydroxy-3-methacryloyloxy propoxy) phenyl] propane (Bis-GMA), as a base resin, and triethylene glycol dimethacrylate (TEGDMA), as a diluent, are often limited in dentistry due to the relatively large amount of volumetric shrinkage that occurs during the curing reaction. In this study, various new resin matrices were examined for use as dental composites in order to reduce the amount of volumetric shrinkage that occurs in dental composites as a result of curing. Bis-GMA derivatives were synthesized by substituting methyl groups for hydrogen on the phenyl ring. The derivatives of TEGDMA with different chain lengths or reactive groups were also examined. The molecular structural changes in the TEGDMA derivatives were not effective in reducing the level of volumetric shrinkage. The resin matrix containing a Bis-GMA derivative and TEGDMA showed a reduced amount of volumetric shrinkage in proportion to the number of methyl groups on the phenyl rings. Polymerization with a mixture of Bis-GMA, its derivatives and a diluent is a promising strategy for obtaining a polymer with a low amount of volumetric shrinkage. A comparison of the volumetric shrinkage of dental composites containing Bis-GMA, TMBis-GMA (2,2-bis[3,5-dimethyl, 4-(2-hydroxy-3-methacryloyloxy propoxy) phenyl] propane)), and TEGDMA with that prepared from a Bis-GMA and TEGDMA mixture showed that the volumetric shrinkage reduction in the new resin was approximately 50%. Furthermore, the mechanical strength of the former was higher than that of the latter.

Biocompatible Materials↗
PubMed2002

Ab initio conformational studies on diols and binary diol-water systems using DFT methods. Intramolecular hydrogen bonding and 1:1 complex formation with water.

Studies on the conformational equilibrium for the following diols, ethane-1,2-diol (12EG, CAS 107-21-1), 2R-D-(-)-propane-1,2-diol (12PG, CAS 4254-14-2), (2S,3S)-L-(+)-butane-2,3-diol (L23BD, CAS 19132-06-0), and (2S,3R)-meso-butane-2,3-diol (m23BD, CAS 5341-95-7), are described using Gaussian ab initio calculations involving density functional theory (DFT) methods. We also report in this article results on the stability and conformation for the 1:1 water-diol complex formed by ethane-1,2-diol, propane-1,2-diol, and L- and meso-butane-2,3-diol. The relative stability of the intramolecular (internal) hydrogen bond in a range of diols (n = 2 to 6), based on ab initio geometry optimization and determination of the -O...H- distance, dOH, and -O-H...O- angle, theta, increases through the sequence 1,2 approximately equals 2,3 < 1,3 < 1,4 approximately equals 1,5 approximately equals 1,6, as judged from the bond linearity and -O...H- separation. Quantum mechanical and topological analysis of possible intramolecular hydrogen bonding in this complete series of diols provides convincing evidence for this in diols in which the hydroxyl groups are separated by three or more carbon atoms, that is, in (n, n+m) diols for m > or = 2, but not for ethane-1,2-diol or other vicinal diols, which do not satisfy Popelier's topological and electron density criteria based on the AIM theory of Bader. Based on these criteria it is unlikely that vicinal diols are in fact capable of forming an intramolecular hydrogen bond, in spite of geometric and spectroscopic data in the literature suggesting otherwise.

Journal Article↗
PubMed2005

Estimation of the absolute internal-rotation entropy of molecules with two torsional degrees of freedom from stochastic simulations.

A method of statistical estimation is applied to the problem of evaluating the absolute entropy of internal rotation in a molecule with two torsional degrees of freedom. The configurational part of the entropy is obtained as that of the joint probability density of an arbitrary form represented by a two-dimensional Fourier series, the coefficients of which are statistically estimated using a sample of the torsional angles of the molecule obtained by a stochastic simulation. The internal rotors in the molecule are assumed to be attached to a common frame, and their reduced moments of inertia are initially calculated as functions of the two torsional angles, but averaged over all the remaining internal degrees of freedom using the stochastic-simulation sample of the atomic configurations of the molecule. The torsional-angle dependence of the reduced moments of inertia can be also averaged out, and the absolute internal-rotation entropy of the molecule is obtained in a good approximation as the sum of the configurational entropy and a kinetic contribution fully determined by the averaged reduced moments of inertia. The method is illustrated using Monte Carlo simulations of isomers of stilbene and halogenated derivatives of propane. The two torsional angles in cis-stilbene are found to be much more strongly correlated than those in trans-stilbene, while the degree of the angular correlation in propane increases strongly on substitution of hydrogen atoms with chlorine.

Journal Article↗
PubMed2004

Preparation and crystal characterization of a polymorph, a monohydrate, and an ethyl acetate solvate of the antifungal fluconazole.

The preparation and solid-state characterization of three crystalline modifications of the antifungal agent fluconazole [2-(2,4-difluorophenyl)-1,3-bis-(1H-124-triazol-1-yl)-propan-2-ol] are reported. Recrystallization of fluconazole from propan-2-ol yielded a polymorph (Form III), whereas the solvents water and ethyl acetate yielded the solvated products fluconazole monohydrate and fluconazole. (ethyl acetate)(0.25), respectively. These species were analyzed by thermogravimetry (TGA), differential scanning calorimetry (DSC), FTIR spectroscopy, powder X-ray diffractometry (PXRD), and single crystal X-ray diffraction. Availability of the hitherto unknown crystal structures facilitated interpretation of the thermal data and clarified previous findings relating to the polymorphism of this compound. Fluconazole was found to exist as a centrosymmetric hydrogen bonded dimer in Form III. For the solvated phases, the solvent locations within the drug host matrices were established as isolated sites for water molecules and constricted channels for ethyl acetate molecules. Desolvation of the monohydrate and ethyl acetate solvate yielded polymorphic Form I. Reference PXRD patterns computed from the refined single-crystal X-ray data for the title compounds are presented.

Acetates↗
PubMed1987

Microbiological systems in organic synthesis: preparation of racemic prenalterol utilizing Cunninghamella echinulata.

The fungal microorganism Cunninghamella echinulata was utilized to para-hydroxylate the synthetic substrate (+/-)-1-isopropylamino-3-phenoxy-propan-2-ol (1). The resulting product, (+/-)-1-(4-hydroxyphenoxy)-3-isopropylamino-propan-2-ol, or (+/-)-prenalterol, (2) was formed in greater than 85% yield. Extracts from incubates were derivatized with trifluoroacetic anhydride and the concentrations of 1 and 2 were determined by GC on a fused silica methyl silicone capillary column with nitrogen-phosphorus detection. At substrate concentrations of 100 and 200 mg/L, the biotransformation proceeds with apparent first-order kinetics. With higher concentrations, the kinetics of prenalterol formation and substrate uptake appear to be nonlinear with a Km value of 427.8 micrograms/mL and a Vmax value of 232.3 micrograms/mL/d. This suggests that the biotransformation may proceed through a single-capacity limited pathway. The microbial product was isolated and identified as (+/-)-prenalterol by comparison (mp, IR, MS, 1H NMR) with an authentic specimen.

Biotransformation↗
PubMed1993

Quaternary salts of 3,3'-bis-pyridinium monooximes: synthesis and biological activity.

Two new series of asymetrically substituted 3,3'-bis-pyridinium monooximes bridged by oxopropane and propane groups were synthesized and characterized by spectral data and acid dissociation constants (pKas). Both the in vitro reactivation potency, in experiments with lyophilized electric eel acetylcholinesterase (AChE) inhibited by diisopropylfluorophosphate, and in vivo protection efficacy against diisopropylfluorophosphate intoxication in mice of these compounds were evaluated and compared with those of trimedoxime and 2-pyridine-aldoxime methiodide. The compounds were also evaluated for in vitro inhibition of AChE. The compounds with the oxopropane link were stronger inhibitors and weaker reactivators than the corresponding propane derivatives. No significant correlation was observed among pKa, oxime inhibition of AChE, reactivation of inhibited AChE, and protection index. Changing substituents in pyridine rings or altering linking groups between pyridine rings did not improve antidotal efficacy compared with trimedoxime and 2-pyridine-aldoxime methiodide.

Animals↗
PubMed2004

Fermentative production of chemicals that can be used for polymer synthesis.

The fermentative production of chemicals that can be used as monomers for the synthesis of polymers has become an important topic in biotechnology research because of the limited nature of petroleum and environmental issues. In particular, the fermentative production of metabolites such as dicarboxylic acids, amino acids, and diols, which are suitable as building blocks for subsequent polymerization, has attracted much attention. Various wild-type and metabolically engineered microorganisms have been developed for the efficient production of these chemicals from renewable resources. In addition, the development of fermentation strategies to achieve the highest possible productivities has been another focus of research, considering that these monomers should be produced at costs low enough to compete with petroleum-derived ones. In this paper, the metabolic pathways leading to the synthesis of such important monomers including succinic acid, lactic acid, fumaric acid, propan-1,2-diol, and propan-1,3-diol are reviewed. In addition, the metabolic engineering and fermentation strategies for their production are reviewed.

Biotechnology↗
PubMed2003

Optimizing protein solubility for two-dimensional gel electrophoresis analysis of human myocardium.

In order to maximize the myocardial proteome observed by two-dimensional gel electrophoresis (2-DE), the effect of (1) either an ionic or different zwitterionic detergents during tissue homogenization and (2) altering the "standard" detergent for isoelectric focusing (3-[(3-cholamidopropyl)dimethylamino]-1-propane sulfonate (CHAPS)) to either the zwitterionic detergent amidosulfobetaine-14 (ASB-14) or N-decyl-N-N'-dimethyl-3-ammonio-1-propane sulfonate (SB3-10) was investigated. Sodium dodecyl sulfate was shown to be a superior detergent for extraction of proteins during homogenization of cardiac tissue compared to the detergents ASB-14, SB3-10 or CHAPS. Additionally, both ASB-14 and SB3-10 exhibited better extraction than CHAPS for distinct regions of two-dimensional gels. In most cases, the best combination of homogenization and focusing conditions did not involve the use of the same detergent. Specifically, it was found that the ability to mix homogenization and focusing conditions can allow one to obtain an optimum balance between the resolution and number of protein spots obtained in 2-DE analysis of cardiac tissue. An excellent initial combination of buffers to utilize for the general examination of cardiac proteins was determined to be initial homogenization in a buffer containing ASB-14 followed by focusing in a buffer containing CHAPS.

Buffers↗
PubMed2003

An efficient solubilization buffer for plant proteins focused in immobilized pH gradients.

The solubilization of a large array of proteins before electrophoresis itself is a very critical point for proteomic analyses. We compared the efficiency of several different solubilization buffers. From this work, we defined a very efficient solubilization buffer, including two chaotropes, two reducing agents (R2), two detergents (D2), and two kinds of carrier ampholytes in combination. This so-called R2D2 buffer (5 M urea, 2 M thiourea, 2% 3-[(3-cholamidopropyl) dimethyl-ammonio]-1-propane-sulfonate, 2% N-decyl-N,N-dimethyl-3-ammonio-1-propane-sulfonate, 20 mM dithiothreitol, 5 mM Tris(2-carboxyethyl) phosphine, 0.5% carrier ampholytes 4-6.5, 0.25% carrier ampholytes 3-10) proved to be very efficient for a large range of different samples and allowed us to obtain two-dimensional gels of high resolution and quality.

Buffers↗
PubMed2000

A study on the reactions of plant copper amine oxidase with C3 and C4 aliphatic diamines.

The paper reports a study on the reactions of grass pea (Lathyrus sativus) amine oxidase (GPAO) with several aliphatic diamines. The influence of the chain length and of unsaturations in the molecules was examined. Kinetic measurements confirmed that trans-, i.e., (E)-2-butene-1,4-diamine (TDABE) and cis-, i.e., (Z)-2-butene-1,4-diamine (CDABE) could be classified as good substrates. Propane-1,3-diamine (DAP) and propene-1,3-diamine (DAPE) were only weakly oxidized, whereas 1,3-diamino-2-propanol (DAPL) was not utilized as a substrate. Contrary to the inactivator 2-butyne-1,4-diamine (DABI), DAPE was shown to be only a competitive inhibitor. DAP itself did not inhibit the catalytic activity. Irreversible inhibition of the activity occurred only after the incubation of GPAO with DABI; other diamines were without this effect. Differential pulse polarography and chromatofocusing confirmed that the aminoaldehyde product of DABI oxidation binds to the enzyme. Activity assay of pea aminoaldehyde dehydrogenase enabled us to detect the products of the oxidation of TDABE, CDABE, and DAP by GPAO. As the product of DAP oxidation, 3-amino-propanal (APAL) was detected by mass spectrometry and confirmed to be a potent noncompetitive inhibitor of GPAO. The absorption changes that occurred in the course of the reaction of GPAO with the diamines were investigated using rapid-scanning spectrophotometry. DABI, TDABE, CDABE, DAP, and DAPE reacted with GPAO providing characteristic maxima of the Cu(I)-semiquinolamine species that is formed in the catalytic cycle. The results presented here confirm that with the exception of DAPL, all the studied diamines could be classified as GPAO substrates, but only DABI can be considered as a mechanism-based inhibitor.

Aldehyde Dehydrogenase↗