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Alkali
Terms modified by Alkali Selected AbstractsEFFECT OF VARIOUS ANTIOXIDANTS ON THE OXIDATIVE STABILITY OF ACID AND ALKALI SOLUBILIZED MUSCLE PROTEIN ISOLATESJOURNAL OF FOOD BIOCHEMISTRY, Issue 2 2009SIVAKUMAR RAGHAVAN ABSTRACT Protein isolates prepared from cod (Gadus morhua) myofibrillar proteins using acid or alkali solubilization are susceptible to oxidative rancidity. Oxidation could be delayed by the exogenous addition of antioxidants. The objective of this research was to compare the efficacy of antioxidants such as ,-tocopherol, butylated hydroxyanisole (BHA) and propyl gallate, to inhibit oxidation in acid- and alkali- solubilized cod protein isolates. Oxidation was catalyzed using cod hemolysate. Oxidation of lipids was monitored by the measurement of thiobarbituric acid reactive substances and painty odor. Results showed that protein isolates prepared using the acid process was significantly (P < 0.05) more susceptible to lipid oxidation than alkali-solubilized protein isolates. Regardless of pH treatments, the efficacy of various antioxidants decreased in the order propyl gallate > BHA > ,-tocopherol. PRACTICAL APPLICATIONS Research has shown that seafood available for human consumption is rapidly getting depleted and that many fish species may become extinct in the next half-century or so. Acid and alkali solubilization methods are recent but well-known techniques used for preparing protein isolates from under-utilized aquatic species and the by-products of seafood industry. Although numerous researchers have studied the use of acid and alkali processes on several sources of seafood, almost no research has been done on the use of antioxidants to protect protein isolates from lipid oxidation. In our research, we have studied the effect of various antioxidants on the oxidative stability of acid- and alkali-solubilized fish myofibrillar proteins. The results from this work will enable the seafood industry to properly identify the process and the type of antioxidants required for making muscle food products with increased oxidative stability. [source] Clustering of nucleobases with alkali metals studied by electrospray ionization tandem mass spectrometry: implications for mechanisms of multistrand DNA stabilizationJOURNAL OF MASS SPECTROMETRY (INCORP BIOLOGICAL MASS SPECTROMETRY), Issue 7 2002Kim J. Koch Abstract Self-clustering of the five common nucleobases was investigated by electrospray ionization tandem mass spectrometry and shown to provide insight into the non-covalent interactions between identical bases. Alkali and ammonium cations significantly increase self-aggregation of the nucleobases and lead to the formation of uniquely stable magic number clusters. Sodium adducts of guanine, thymine and uracil preferentially take the form of tetrameric (quartet) clusters. This gas-phase result correlates with previously reported solution-phase data on sodium cation stabilized guanosine, thymine and uracil quartet structures believed to be responsible for telomere stabilization. In the presence of potassium, cesium or ammonium cations, pentameric magic number clusters are formed from thymine and uracil, while in solution the nucleoside isoguanosine yields clusters of this favored size. The formation of magic number metaclusters occurs for thymine and uracil in the presence of ammonium cations. These doubly charged 10- and 15-mers are tentatively attributed to the formation of pentamer/ammonium cation/ pentamer sandwich structures. Copyright © 2002 John Wiley & Sons, Ltd. [source] Effect of Calcination Conditions and Excess Alkali Carbonate on the Phase Formation and Particle Morphology of Na0.5K0.5NbO3 PowdersJOURNAL OF THE AMERICAN CERAMIC SOCIETY, Issue 5 2007Pornsuda Bomlai Sodium-potassium niobate [Na0.5K0.5NbO3] powders were prepared following the conventional mixed oxide method. An orthorhombic XRD pattern, consistent with single-phase Na0.5K0.5NbO3, was obtained after calcination at 900°C for 6 h. Introducing 5 mol% excess Na2CO3 and K2CO3 into the starting mixture allowed milder calcination conditions to be used, for example 800°C for 2 h. Primary particles in 5 mol% excess samples were cuboid, with maximum sizes of ,2.5 ,m. Equiaxed 0.3,0.4-,m particles were formed for non-excess powders, and also for powders prepared with 1 and 3 mol% excess alkali carbonates. The results suggest liquid formation during calcination of the excess 5-mol% starting powders. [source] Exploiting Tautomerism for Switching and Signaling,ANGEWANDTE CHEMIE, Issue 42 2009Liudmil Antonov Prof. Gut in Form: Durch Anbringen einer flexiblen Piperidin-Einheit an 4-(Phenyldiazenyl)naphthalin-1-ol wurde ein molekularer Schalter erhalten, der über ein Tautomerengleichgewicht mit Protonierung/Deprotonierung gesteuert werden kann (siehe Bild). Der Schalter, der kleine Alkali- und Erdalkalimetallionen komplexiert, könnte eine Basis für die Entwicklung effektiver molekularer Sensoren bieten. [source] Alkali-based AFEX pretreatment for the conversion of sugarcane bagasse and cane leaf residues to ethanolBIOTECHNOLOGY & BIOENGINEERING, Issue 3 2010Chandraraj Krishnan Abstract Sugarcane is one of the major agricultural crops cultivated in tropical climate regions of the world. Each tonne of raw cane production is associated with the generation of 130,kg dry weight of bagasse after juice extraction and 250,kg dry weight of cane leaf residue postharvest. The annual world production of sugarcane is ,1.6 billion tones, generating 279 MMT tones of biomass residues (bagasse and cane leaf matter) that would be available for cellulosic ethanol production. Here, we investigated the production of cellulosic ethanol from sugar cane bagasse and sugar cane leaf residue using an alkaline pretreatment: ammonia fiber expansion (AFEX). The AFEX pretreatment improved the accessibility of cellulose and hemicelluloses to enzymes during hydrolysis by breaking down the ester linkages and other lignin carbohydrate complex (LCC) bonds and the sugar produced by this process is found to be highly fermentable. The maximum glucan conversion of AFEX pretreated bagasse and cane leaf residue by cellulases was ,85%. Supplementation with hemicellulases during enzymatic hydrolysis improved the xylan conversion up to 95,98%. Xylanase supplementation also contributed to a marginal improvement in the glucan conversion. AFEX-treated cane leaf residue was found to have a greater enzymatic digestibility compared to AFEX-treated bagasse. Co-fermentation of glucose and xylose, produced from high solid loading (6% glucan) hydrolysis of AFEX-treated bagasse and cane leaf residue, using the recombinant Saccharomyces cerevisiae (424A LNH-ST) produced 34,36,g/L of ethanol with 92% theoretical yield. These results demonstrate that AFEX pretreatment is a viable process for conversion of bagasse and cane leaf residue into cellulosic ethanol. Biotechnol. Bioeng. 2010;107: 441,450. © 2010 Wiley Periodicals, Inc. [source] ChemInform Abstract: Prediction and Characterization of a New Kind of Alkali,Superhalogen Species with Considerable Stability: MBeX3 (M: Li, Na; X: F, Cl, Br).CHEMINFORM, Issue 6 2008Song-Hua Cui Abstract ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a "Full Text" option. The original article is trackable via the "References" option. [source] Study of the Behavior of p-Bis{3-[N,N-dialkyl-N-(4-hydroxybut-2-ynyl)ammonio] prop-2-ynyl}-benzene Dichlorides in Relation to Aqueous Alkali.CHEMINFORM, Issue 21 20072-dialkyl-4-hydroxymethyl)isoindolinium Dichlorides., Double Intramolecular Recyclization of Benzo[, c]di( Abstract ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 200 leading journals. To access a ChemInform Abstract, please click on HTML or PDF. [source] Reaction of Aldehydes with Hydrazine in the System Sulfur,Alkali.CHEMINFORM, Issue 19 2003N. V. Russavskaya Abstract For Abstract see ChemInform Abstract in Full Text. [source] ChemInform Abstract: Novel Ring Contraction of 3-Hydroxy-2,4(1H,3H)-quinolinediones in Aqueous Alkali.CHEMINFORM, Issue 5 2002The First Convenient Route to 2-Hydroxyindoxyls. Abstract ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a "Full Text" option. The original article is trackable via the "References" option. [source] ChemInform Abstract: Solid-Phase Oxidation of 2,4-Di-tert-butylphenol and 3,6-Di-tert-butylpyrocatechol in the Presence of Alkali and Alkaline Earth Metal Halides under Elastic Deformation.CHEMINFORM, Issue 16 2001V. B. Vol'eva Abstract ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a "Full Text" option. The original article is trackable via the "References" option. [source] Effect of Cross Linking Agent on Alkali/Surfactant/PolymerCHINESE JOURNAL OF CHEMISTRY, Issue 1 2008Ke ZHANG Abstract Alkali/surfactant/polymer (ASP) multisystem flooding technique, which has an expansive application prospect, is one of the enhancing oil recovery (EOR) methods. By adding the organic chromium to the ASP, the molecular structure of polymer was made to change, and the capability of controlling mobility coefficient of ASP was improved. The results showed that multisystem could still keep ultra-low interfacial tension between the multisystem and crude oil after addition of Cr3+. The resistance factor and residual resistance factor, the indicator which describes the capability of controlling mobility, upgraded strikingly. However its storage modulus and loss modulus, the indicator which describes viscoelasticity, increased. The results of physical simulation experiment indicated that this type of improved ASP could increase the recovery ratio by 4.3% compared to common ASP multisystem. [source] Synthesis, crystal structure and vibrational characterization of bis-,-peroxo-hexacarbonatodicerate(IV) complexes of rubidium and cesiumCRYSTAL RESEARCH AND TECHNOLOGY, Issue 11 2008N.-P. Pook Abstract The new compounds Rb8[Ce(O2)(CO3)3]2 · 12 H2O (1) and Cs8[Ce(O2)(CO3)3]2 · 10 H2O (2) were obtained from the reaction of hydrogen peroxide and Ce(III) in saturated alkali carbonate solutions. The crystal structures and the unit cell parameters of (1) triclinic, P-1 with a = 8.973(2) Å, b = 10.815(2) Å, c = 11.130(3) Å, , = 66.992(2)°, , = 68.337(2)°, , = 74.639(2)°, VEZ = 914.7(4) Å3, Z = 2, and (2) orthorhombic, Pbca, a = 19.3840(16) Å, b = 18.528(2) Å, c = 10.487(3) Å, VEZ = 3766.4(13) Å3, Z = 8, were determined. Both compounds contain the bis-µ-peroxo-hexacarbonatodicerate(IV)-ion, [(CO3)3Ce(O2)2Ce(CO3)3]8- . IR and Raman spectra were measured and discussed. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Radiation induced modification of impurity-related point defects in crystalline quartz , a reviewCRYSTAL RESEARCH AND TECHNOLOGY, Issue 7 2006Harish Bahadur Abstract This article presents a short review of impurity-related point defects in crystalline quartz and their radiation induced modifications. In particular, a discussion has been presented on some of the prominent aluminum related alkali and proton compensated centers. (© 2006 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] "My Two-week-old Daughter Is Throwing up Blood"ACADEMIC EMERGENCY MEDICINE, Issue 8 2005M.H. Moustafa MD Abstract Swallowed maternal blood at the time of delivery or from cracked nipples during breastfeeding is the most common cause of suspected gastrointestinal bleeding in the neonate. In this case, the Apt,Downey test is a useful diagnostic tool. The Apt,Downey test can effectively differentiate neonatal from maternal hemoglobin based on the conversion of oxyhemoglobin to alkaline globin hematin when mixed with alkali. [source] Lead(II) Potentiometric Sensor Based on 1,4,8,11-Tetrathiacyclotetradecane Neutral Carrier and Lipophilic AdditivesELECTROANALYSIS, Issue 11 2008Mohamed Abstract A potentiometric sensor for lead(II) ions based on the use of 1,4,8,11-tetrathiacyclotetradecane (TTCTD) as a neutral ionophore and potassium tetrakis-(p -chlorophenyl)borate as a lipophilic additive in plasticized PVC membranes is developed. The sensor exhibits linear potentiometric response towards lead(II) ions over the concentration range of 1.0×10,5,1.0×10,2,mol L,1 with a Nernstian slope of 29.9,mV decade,1 and a lower limit of detection of 2.2×10,6,mol L,1 Pb(II) ions over the pH range of 3,6.5. Sensor membrane without a lipophilic additive displays poor response. The sensor shows high selectivity for Pb(II) over a wide variety of alkali, alkaline earth and transition metal ions. The sensor shows long life span, high reproducibility, fast response and long term stability. Validation of the method by measuring the lower limit of detection, lower limit of linear range, accuracy, precision and sensitivity reveals good performance characteristics of the proposed sensor. The developed sensor is successfully applied to direct determination of lead(II) in real samples. The sensor is also used as an indicator electrode for the potentiometric titration of Pb(II) with EDTA and potassium chromate. The results obtained agree fairly well with data obtained by AAS. [source] A Novel Al(III)-Selective Electrochemical Sensor Based on N,N,-Bis(salicylidene)-1,2-phenylenediamine ComplexesELECTROANALYSIS, Issue 16 2006B. Gholivand Abstract A polyvinylchloride membrane sensor based on N,N,-bis(salecylidene)-1,2-phenylenediamine (salophen) as membrane carrier was prepared and investigated as a Al3+ -selective electrode. The sensor exhibits a Nernstian response toward Al(III) over a wide concentration range (8.0×10,7,3.0×10,2,M), with a detection limit of 6.0×10,7,M. The potentiometric response of the sensor is independent of the pH of the test solution in the pH range 3.2,4.5. The electrode possesses advantages of very fast response and high selectivity for Al3+ in comparison with alkali, alkaline earth and some heavy metal ions. The sensor was used as an indicator electrode, in the potentiometric titration of aluminum ion and in determination of Al3+ contents in drug, water and waste water samples. [source] Potentiometric Ag+ Sensors Based on Conducting Polymers: A Comparison between Poly(3,4-ethylenedioxythiophene) and Polypyrrole Doped with Sulfonated CalixarenesELECTROANALYSIS, Issue 18 2005Zekra Mousavi Abstract Potentiometric Ag+ sensors were prepared by galvanostatic electropolymerization of 3,4-ethylenedioxythiophene (EDOT) and pyrrole (Py) on glassy carbon electrodes by using sulfonated calixarenes as doping ions. Poly(3,4-ethylenedioxythiophene) (PEDOT) and polypyrrole (PPy) doped with p -sulfonic calix[4]arene (C4S), p -sulfonic calix[6]arene (C6S) and p -sulfonic calix[8]arene (C8S) were compared. PEDOT and PPy doped with poly(styrene sulfonate) (PSS) were also included for comparison. The analytical performance of the conducting polymer-based Ag+ sensors was studied by potentiometric measurements. All conducting polymer and dopant combinations showed sensitivity and selectivity to Ag+ compared to several alkali, alkaline-earth, and transition-metal cations. The type of the conducting polymer used for the fabrication of the electrodes was found to have a more significant effect on the selectivity of the electrodes to Ag+ than the ring size of the sulfonated calixarenes used as dopants. Selected conducting polymer-based sensors were studied by cyclic voltammetry (CV) and energy dispersive analysis of X-rays (EDAX) measurements. Results from the EDAX measurements show that both PEDOT- and PPy-based membranes accumulate silver. [source] Asymmetrical Schiff Bases as Carriers in PVC Membrane Electrodes for Cadmium (II) IonsELECTROANALYSIS, Issue 8 2005Hossein Mashhadizadeh, Mohammad Abstract 5-[((4-Methyl phenyl) azo)- N -(6-amino-2-pyridin) salicylaldimine] (S1), and 5-[((4-methyl phenyl) azo)- N -(2-diamino-2-cyano-1-ethyl cyanide) salicylaldehyde] (S2) with N and O donor atoms are effective ionophores to make Cd2+ -selective membrane electrodes. The electrodes based on S1 and S2 exhibits a Nernstian or near-Nernstian response for cadmium ion over a wide concentration range 1.5×10,1,7.5×10,7 with a slope of 28 and 2.0×10,1,4.0×10,7 with a slope of 22, respectively. They have quick response and can be used for three or four months without any divergence in potential. The proposed sensors show fairly good selectivity over some alkali, alkaline earth, transition and heavy metal ions. The electrodes based on S1 and S2 can be used in the pH range 3.5,9. These electrodes were used as an indicator electrode in potentiometric titration of cadmium ion with EDTA and in the direct determination of cadmium ion in aqueous solutions. [source] Copper Ion Selective Membrane Electrodes Based on Some Schiff Base DerivativesELECTROANALYSIS, Issue 15-16 2003S. Sadeghi Abstract A series of Schiff base derivatives were studied to characterize their abilities as a copper ion carrier in PVC membrane electrodes. The electrode based on 2,2,-[4,4,diphenyl-methanebis(nitrilomethylidyne)]-bisphenol exhibits a Nernstian response for copper ions over the activity range 8.0×10,6,1.0×10,1 mol L,1 with detection limit of about , mol L,1 of copper ion in comparison with two other Schiff bases. The response time, pH effect and other characteristics of the electrodes were studied in a static mode. The effect of the methyl group substitute on Schiff base structure with SO2 bridging group in different positions with respect to OH group was studied. The results show that behavior of the electrodes is not considerably influenced by the position of methyl substitute. The selectivity coefficients were determined with modified fixed interference method (FIM) and matched potential method (MPM). The proposed electrodes comparatively show good selectivity with respect to alkali, alkaline earth and some transition metal ions. The electrodes were used for the determination of copper in black tea, multivitamin and mineral capsule and as an indicator electrode in potentiometric titration of copper ion. [source] Synthesis and Photochromism of Novel Chromene Derivatives Bearing a Monoazacrown Ether MoietyEUROPEAN JOURNAL OF ORGANIC CHEMISTRY, Issue 13 2003Saleh A. Ahmed Abstract Crowned chromenes , four novel naphthopyrans (chromenes) bearing monoaza-12-crown-4, -15-crown-5, -18-crown-6, and a noncyclic analogue at the 5-position , were synthesized, and their photochromism in acetonitrile was examined in the presence of alkali and alkaline-earth metal ions. Incorporation of crown ether units to chromene moieties facilitated to a great extent both the thermal isomerization and photoisomerization of the chromene moiety, reflecting the metal-ion-binding ability of the crown ether moiety. Comparison of the crowned chromenes with the corresponding crowned spirobenzopyrans reveals that photochromism of the crowned chromene reflects an interaction between the metal ion and the crown ether moiety that is stronger than that of the crowned spirobenzopyran, and shows only positive photochromism with significant red-shifts in the UV/Vis absorption spectra, in contrast to the crowned spirobenzopyrans reported previously. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2003) [source] Patterned Synthesis of Pd4S: Chemically Robust Electrodes and Conducting Etch MasksADVANCED FUNCTIONAL MATERIALS, Issue 6 2010Boya Radha Abstract A simple, one-step process to synthesize Pd4S films is reported here along with their characterization using X-ray diffraction, electron microscopy, and electrical measurements. The synthesis involves thermolysis of a single-source precursor, namely palladium alkanethiolate, in H2 atmosphere at 250,°C for 3,h. The films are highly conducting and resistant to strong acidic, alkali, and oxidizing environments. The precursor allows patterning of the Pd4S films by electron beam lithography and micromolding, an attribute that has been employed in making chemically resistant electrodes and etch masks. The conversion of palladium thiolate to other sulfide phases is also achieved. [source] Chemical modification of pyroclastic rock by hot water: an experimental investigation of mass transport at the fluid,solid interfaceGEOFLUIDS (ELECTRONIC), Issue 1 2009J. HARA Abstract Hydrothermal water,(pyroclastic) rock interactions were examined using flow-through experiments to deduce the effect of mass transport phenomena on the reaction process. A series of experiments were conducted over the temperature range 75,250°C, with a constant temperature for each experiment, and at saturated vapour pressure, to estimate the apparent rate constants as a function of temperature. Based on the chemistry of analysed solutions, the water,rock interaction in the experiments was controlled by diffusion from the reaction surface and by the existence of a surface layer at the rock,fluid interface, which regulated the chemical reaction rate. The reaction progress depended to a high degree on flow velocity and temperature conditions, with element abundances in the fluid significantly affected by these factors. Mass transport coefficients for diffusion from the rock surface to the bulk solution have been estimated. Ca is selectively depleted under lower temperature conditions (T < 150°C), whereas Na is greatly depleted under higher temperature conditions (T > 150°C), and K reaction rates are increased when flow velocity increases. Using these conditions, specific alkali and alkali earth cations were selectively leached from mineral surfaces. The ,surface layer' comprised a 0.5,1.8 mm boundary film on the solution side (the thickness of this layer has no dependence on chemical character) and a reaction layer. The reaction layer was composed of a Si, Al-rich cation-leached layer, whose thickness was dependent on temperature, flow velocity and reaction length. The reaction layer varied in thickness from about 10,4 to 10,7 mm under high temperature/low fluid velocity and low temperature/high fluid velocity conditions, respectively. [source] An experimental and modeling study of Na-rich hydrothermal alterationGEOFLUIDS (ELECTRONIC), Issue 4 2005J. HARA Abstract Sodic alteration assemblages including clinoptilolite, mordenite, analcime and Na-montmorillonite were locally observed in sediments in the eastern part of the Hachimantai geothermal region, northeast Japan. This study investigated the mechanisms of sodic enrichment in the sediments during alteration. Kinetic results for water/rock interaction experiments are reported here. Batch-type experiments were conducted at 150,250°C under saturated vapor pressure. Pyroclastic rocks dissolved incongruently in these experiments, and the solubility and dissolution rates among elements varied as follows: the apparent steady-state concentrations of major elements are Si > Na , K > Ca > Al and the order of the dissolution rates is Si > Al > Na , K > Ca. Na had the highest steady-state concentration and fastest dissolution rate of the alkali and alkali earth metal ions. Based on surface analysis of plagioclase, dissolution was effected via a reaction layer of Na-montmorillonite on the mineral surface. Additionally, a reaction model constructed based on the experimentally observed reaction mechanism quantitatively explains the dissolution behavior. These results show that Na-montmorillonite can be precipitated by pyroclastic rock/meteoric water interactions without seawater involvement: the Na is derived from the host rocks. [source] Direct Current Plasma Emission Spectrometric Determination of Major, Minor and Trace Elements in Microwave Oven Acid Leachates of Powdered Whole Coal SamplesGEOSTANDARDS & GEOANALYTICAL RESEARCH, Issue 1 2005Sandro Fadda DCP-AES; échantillons de charbon; four à micro-ondes; éléments facilement ionisables; effets de matrice. Major concentrations of Al2O3, Fe2O3, MgO, CaO, Na2O and K2O, minor levels of TiO2, P2O5 and thirty petrologically, geochemically and environmentally significant trace elements have been determined in microwave oven acid leachates of whole powdered coal samples by direct current plasma-atomic emission spectrometry (DCP-AES). A single sample preparation procedure was suitable for all the determinations with no additional dilution step for major elements solution. Dried samples (0.5 g) were treated in low-pressure PFA digestion vessels with HF/HCl/HNO3/HClO4 acids to quantitatively extract the analytes from the bulk material, while leaving the major part of organic matrix as a residue. The major constituents of geological samples, in particular the easily ionised elements (EIEs) such as alkali and alkaline earths, may complicate the instrumental determinations in DCP-AES because of differential enhancements of elemental emission intensities and stray light interferences. Taking account of these factors, the coal matrix is considered to have very low major oxide totals as compared to many other common geo-environmental and related materials (rocks, sediments, soil, ashes etc.). The sample size employed here, while yielding a relatively concentrated solution to cover a wide range of elemental determinations, provided a sample matrix that significantly diminished interferences for DCP measurements. The need for closely matching the unknowns and calibrators was eliminated except for overall acidity and an excess quantity of caesium for EIE buffering. Calibration of the spectrometer was accomplished by simple aqueous single element solutions as high concentration calibrators in addition to a reagent blank as a low concentration calibrator. Two point working curves were established to allow for the maximum concentrations of each element expected in the unknowns. The precision of determinations under routine conditions as well as the reproducibility of the leaching and precision of instrumental measurements have been evaluated. Relative standard deviations (RSD) were of 1,2% for those elements whose concentrations in solid samples were well above the limits of quantification. Method detection limits in the buffered solutions were also evaluated. To evaluate the accuracy of the microwave oven-DCP method a suite of eight certified coal reference materials of differing rank, were analysed with good agreement with the certified and/or available published data. Results are presented for the uncertified major oxides in the AR series reference materials. Les concentrations en éléments majeurs: Al2O3, Fe2O3, MgO, CaO, Na2O et K2O, en éléments mineurs TiO2, P2O5 et en 30 éléments en trace dont le comportement est important en Pétrologie, en Géochimie et en Environnement, ont été analysées par spectrométrie d'émission atomique à plasma à courant direct (DCP-AES), dans des lessivages acides effectués dans un four à micro-ondes sur des échantillons de charbon mis en poudre. Ce mode préparatoire unique est adaptéà toutes les déterminations sans qu'il soit nécessaire d'effectuer une dilution supplémentaire pour l'analyse des éléments majeurs. Les échantillons préalablement desséchés (0.5 g) sont traités dans les pots de PFA de basse pression, avec un mélange d'acides HF/HCl/HNO3/HClO4, afin d'extraire quantitativement les analytes du matériel géologique, tout en laissant la plus grande part de la matrice organique sous forme résiduelle. Les constituants majeurs de ces échantillons géologiques, en particulier les éléments facilement ionisables (EIEs) tels que les alcalins et les alcalino-terreux, peuvent compliquer l'analyse en DCP-AES à cause des rendements variables des intensités d'émission élémentaires et des interférences de raies de lumière. Mais là dessus, la matrice de charbon se révèle être bien plus pauvre en oxydes majeurs que les autres matériaux géologiques, environnementaux ou de type proche (roches, sédiments, sols, cendres). La taille d'échantillon retenue ici, tout en fournissant une solution relativement concentrée qui permet la détermination de beaucoup d'éléments, fournit une matrice qui diminue significativement les interférences lors de la mesure par DCP-AES. Le besoin d'avoir les solutions d'échantillons et les solutions de calibration avec des matrices très proches est donc éliminé, mis à part pour l'acidité totale et la quantité excessive de Césium pour tamponner les EIE. La calibration du spectromètre est faite avec des solutions mono- élémentaires aqueuses, pour déterminer les points de concentrations élevées et avec le blanc de réactifs pour le point de concentration basse. Les courbes de calibrations sont déterminées avec 2 points, pour autoriser l'analyse de concentrations maximales pour chaque élément dans les échantillons inconnus. La précision des déterminations en conditions de routine ainsi que la reproductibilité de l'opération de lessivage et la précision instrumentale des analyses ont étéévaluées. Les déviations standards relatives (RSD) sont de 1,2% pour tout élément dont les concentrations dans le solide sont au dessus des limites de quantification. Les limites de détection de la méthode dans les solutions tamponnées ont aussi étéévaluées. Enfin, pour évaluer la justesse de cette méthode "micro-ondes - DCP" huit charbons certifiés matériaux de référence de différents types ont été analysés, et sont en bon accord avec les données certifiées ou seulement disponibles publiées. Les données sur un certain nombre d'oxydes d'éléments majeurs actuellement non certifiés sont présentées pour les matériaux de référence AR. [source] Hydrothermal Synthesis of Rare Earth (Tb, Y) Hydroxide and Oxide Nanotubes,ADVANCED FUNCTIONAL MATERIALS, Issue 12 2003Y.-P. Fang Abstract In this paper, Tb(OH)3 and Y(OH)3 single-crystalline nanotubes with outer diameters of 30,260,nm, inner diameters of 15,120,nm, and lengths of up to several micrometers were synthesized on a large scale by hydrothermal treatment of the corresponding oxides in the presence of alkali. In addition, Tb4O7 and Y2O3 nanotubes can be obtained by calcination of Tb(OH)3 and Y(OH)3 nanotubes at 450,°C. X-ray diffraction (XRD), field-emission scanning electron microscopy, transmission electron microscopy (TEM), electron diffraction (ED), energy-dispersive X-ray spectroscopy (EDS), thermogravimetry, and differential scanning calorimetry (DSC) have been employed to characterize these nanotube materials. The growth mechanism of rare earth hydroxide nanotubes can be explained well by the highly anisotropic crystal structure of rare earth hydroxides. These new types of rare earth compound nanotubes with open ends have uses in a variety of promising applications such as luminescent devices, magnets, catalysts, and other functional materials. Advantages of this method for easily realizing large-scale production include that it is a simple and unique one-pot synthetic process without the need for a catalysts or template, is low cost, has high yield, and the raw materials are readily available. The present study has enlarged the family of nanotubes available, and offers a possible new, general route to one-dimensional single-crystalline nanotubes of other materials. [source] Solvent-free alkali and alkaline earth metal complexes of di-imine ligands,HETEROATOM CHEMISTRY, Issue 6 2006Igor L. Fedushkin Compound [(dph-BIAN)Mg(THF)]2(2) was prepared by reacting magnesium metal with 1,2- bis[(2-biphenyl)imino]acenaphthene (dph-BIAN) in THF, followed by crystallization from toluene. Reac- tion of CaI2 with (dpp-BIAN)Li2 in toluene afforded [(dpp-BIAN)Li]2Ca (3) (dpp-BIAN = 1,2-bis[(2,6-diisopropylphenyl)imino]acenaphthene). Both complexes 2 and 3 were characterized by single crystal X-ray diffraction. The 1H NMR spectroscopic data obtained for complex 3 in toluene solution indicated an agostic interaction between the methyl groups of the ligand and lithium atoms. © 2005 Wiley Periodicals, Inc. Heteroatom Chem 16:663,670, 2005; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/hc.20277 [source] Modelling the structural behaviour of a dam affected by alkali,silica reactionINTERNATIONAL JOURNAL FOR NUMERICAL METHODS IN BIOMEDICAL ENGINEERING, Issue 1 2006Eduardo M. R. Fairbairn Abstract In this work we present an alkali,silica reaction (ASR) thermo-chemo-mechanical expansion model, whose main feature is to represent the stress-induced anisotropy by means of a classical smeared cracking model. This model considers the influence of temperature and humidity in the development of ASR. Since cracking occurs generally at the beginning of the swelling process, it is suggested that the assessment of the reaction characteristics in free expansion tests could be attained considering a cracked specimen. Hence, an inverse analysis is used to determine ASR parameters. The model was applied to the 3D simulation of alkali,silica expansion in a real gravity dam. We computed the displacements at the crest of the block comparing it with measures taken in situ for the last 25 years. The good correlation between experimental and numerical data displays the accuracy of the model, indicating its potentialities for engineering applications. Copyright © 2005 John Wiley & Sons, Ltd. [source] Oxidation of diclofenac sodium by diperiodatoargantate(III) in aqueous alkaline medium and its determination in urine and blood by kinetic methodsINTERNATIONAL JOURNAL OF CHEMICAL KINETICS, Issue 6 2010P. N. Naik The kinetics and oxidation of diclofenac sodium (DFS) by diperiodatoargentate(III) (DPA) in alkaline medium at 298 K and at a constant ionic strength of 0.60 mol dm,3 were studied spectrophotometrically. The oxidation products were [2-(2,6-dicloro-phynylamino)-phenyl]-methenol and Ag(I), identified by LC-ESI-MS and IR spectral studies. The reaction between DFS and DPA in alkaline medium exhibits 1:1 stoichiometry. The reaction is first order in [DPA] and has a less than unit order dependence each in [DFS] and [alkali]. Increasing concentrations of IO,4 retard the reaction. The active species of DPA proposed to be monoperiodatoargentate(III), and a mechanism is suggested. The rate constants involved in the different steps of the mechanism were determined and are discussed. The activation parameters with respect to a rate-limiting step of the mechanism were determined. The thermodynamic quantities were also determined. Using the oxidation of DFS by DPA, DFS was analyzed by kinetic methods in urine and blood sample. The proposed method enables DFS analysis in the range from 5.0 × 10,5 to 5.0 × 10,3 mol dm,3. © 2010 Wiley Periodicals, Inc. Int J Chem Kinet 42: 336,346, 2010 [source] Theoretical investigation of ion pair SN2 reactions of alkali isothiocyanates with alkyl halides.INTERNATIONAL JOURNAL OF QUANTUM CHEMISTRY, Issue 1 2005Part 1. Abstract The gas-phase ionic SN2 reactions NCS - + CH3F and ion pair SN2 reaction LiNCS + CH3F with inversion mechanism were investigated at the level of MP2(full)/6-311+G**//HF/6-311+G**. Both of them involve the reactants complex, inversion transition state, and products complex. There are two possible reaction pathways in the ionic SN2 reaction but four reaction pathways in the ion pair SN2 reaction. Our results indicate that the introduction of lithium significantly lower the reaction barrier and make the ion pair displacement reaction more facile. For both ionic and ion pair reaction, methyl thiocyanate is predicted to be the major product, but the latter is more selective. More-stable methyl isothiocyanate can be prepared by thermal rearrangement of methyl thiocyanate. The theoretical predictions are consistent with the known experimental results. © 2004 Wiley Periodicals, Inc. Int J Quantum Chem, 2005 [source] Chemical bonding in ternary magnesium hydridesINTERNATIONAL JOURNAL OF QUANTUM CHEMISTRY, Issue 3 2003Emilio Orgaz Abstract The electronic structure of various alkali and alkaline,earth magnesium-based hydrides was investigated in detail. These types of crystalline compounds show MgH4 or MgH6 units ordered within a light-metal framework. We investigated the nature of the chemical bonding in these units by means of quantum chemical calculations of several related clusters. The properties of the charge density of the clusters, within the framework of the theory of atoms in molecules, was analyzed. A further set of computations of the band structure of the solid hydrides was conducted using a state-of the-art density functional-based method and the mechanism of stabilization of the MgH units is discussed. It was found that the properties obtained at the molecular level correlate well with those of the solid crystals, indicating the molecular nature of the extended systems in which the units MgHx, x = 4, 6, are stabilized by means of MgH closed-shell interactions. © 2003 Wiley Periodicals, Inc. Int J Quantum Chem 94: 150,164, 2003 [source] | |||||||||||||||||||||||||||||||||||||||||||||||||