- Single-crystal hexagonal disks and rings of ZnO: Low-temperature, large-scale synthesis and growth mechanism
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Solution-phase synthesis of single-crystal ZnO disks and rings was achieved in high yield at low temperature (70-90°C) by using an anionic surfactant as a template. The reaction can be controlled by means of the growth temperature and the molar ratio of reagents to favor formation of disks or rings. A growth mechanism is proposed on the basis of structural information provided by SEM and TEM.
- Li, Feng,Ding, Yong,Gao, Puxian,Xin, Xinquan,Wang, Zhong L.
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- The state of ruthenium in nitrite-nitrate nitric acid solutions as probed by NMR
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The state of ruthenium in nitric acid solutions treated with sodium nitrite has been studied by 14N, 15N, 17O, and 99Ru NMR. In the acidity range 2.7-0.12 mol/L, the dominating ruthenium species are the [RuNO(NO
- Emel'yanov,Fedotov
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- NaIn(CrO4)2·2H2O, the first indium(III) member of the kroehnkite family
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Sodium indium(III) chromate(VI) dihydrate, NaIn(CrO4) 2·2H2O, synthesized from an aqueous solution at room temperature, is the first indium(III) member of the large family of compounds with kroehnkite [Na2CuII(S VIO4)2·2H2O]-type chains. The crystal structure is based on infinite octahedral-tetrahedral [In(CrO 4)2(H2O)2]- chains along [010], linked via charge-balancing Na+ cations. The slightly distorted InO4(H2O)2 octahedra are characterized by a mean In - O distance of 2.125 A. The CrO4 tetrahedra are strongly distorted (mean Cr - O = 1.641 A). The Na atom shows an octahedral coordination, unprecedented among compounds with kroehnkite-type chains. The NaO6 octahedra share opposite edges with the InO4(H2O)2 octahedra to form infinite [001] chains. The hydrogen bonds are of medium strength. NaIn(CrO 4)2·2H2O belongs to the structural type F2 in the classification of Fleck, Kolitsch & Hertweck [Z. Kristallogr. (2002), 217, 435-443], and is isotypic with KAl(CrO4) 2·2H2O and MFe(CrO4)2· 2H2O (M = K, Tl or NH4). All atoms are in special positions except one O atom.
- Kolitsch, Uwe
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- The effects of synthesis pH and hydrothermal treatment on the formation of zinc aluminum hydrotalcites
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Zn/Al hydrotalcites were synthesized by coprecipitation at increasing pH from 6.0 to 14.0, followed by hydrothermal treatment at 150°C for 7 days. The materials were characterized by X-ray diffraction (XRD), STEM, inductively coupled plasma-atomic emission spectroscopy (ICP-AES), thermal analysis, infrared spectroscopy and Raman spectroscopy. The XRD analysis for the samples prepared between pH 9.0 and 12.0 showed a pattern typical of hydrotalcite, with a c-axis distance of ~22.6 A. STEM showed that the pH of preparation affected the stability of the hydrotalcite and that instability, observed at pH 9.0, favored the formation of mixed phases when treated hydrothermally. It was also shown that treatment of a stable starting material increased the crystallinity and resulted in the formation of hexagonal plate-shaped particles. ICP-AES and thermal analysis showed that the Zn/Al ratio and thermal stability increased with pH. Thermal analysis showed three major weight losses corresponding to the loss of interparticle water, interlayer water and dehydroxylation of the hydroxide layers and decarbonization of the interlayer region.
- Kloprogge, J. Theo,Hickey, Leisel,Frost, Ray L.
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- A "green chemistry" approach to the synthesis of rare-earth aluminates: Perovskite-type LaAlO3 nanoparticles in molten nitrates
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Perovskite-type LaAlO3 nanoparticles have been prepared by a facile, rapid, and environmentally friendly molten salts method using alkali metal nitrates as low-temperature fluxes. Starting from hydrated lanthanum and aluminum nitrates and alkali metal hydroxides, the proposed methodology consists briefly of two steps: a mechanically induced metathesis reaction followed by short firing at temperatures above nitrates melting points. The purpose of the first is twofold: on the one hand to generate in situ the alkali metal nitrate flux and on the other hand, to obtain a La and Al-containing precursor material suitable for the synthesis of bulk LaAlO3 nanoparticles in molten nitrates. Different alkali metal nitrates and eutectic mixtures were used to analyze the influence of melt basicity in the reaction outcome. Single phase LaAlO3 was obtained directly, without any purification step when using three molten media: LiNO3, NaNO3, and their mixture; using KNO3 as flux either alone or as part of eutectic compositions, prevents complete conversion, and the title material is obtained mixed with additional crystalline phases such as lanthanum hydroxinitrates and carbonates. As-prepared LaAlO3 powders are composed of loosely agglomerated nanoparticles with very fine crystallite size (32-45 nm). The present method reduces considerably previously reported synthesis time/temperatures for this material.
- Mendoza-Mendoza, Esmeralda,Montemayor, Sagrario M.,Escalante-Garcia, Jose I.,Fuentes, Antonio F.
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- The synthesis of apatites with an organophosphate and in nonaqueous media
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The syntheses of barium, cadmium, calcium, lead, and strontium apatites were performed in anhydrous polar organic solvents such as DMSO, anisole, pyridine, glacial acetic acid, ethanol, methanol, and DMF. Reactions took place under anhydrous conditions at
- Sternlieb, Mitchell P.,Brown, Heather M.,Schaeffer Jr., Charles D.,Yoder, Claude H.
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- Electrochemical response of nitrite and nitric oxide on graphene oxide nanoparticles doped with Prussian blue (PB) and Fe2O3 nanoparticles
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Electrocatalytic behaviour of graphene oxide (GO), iron(iii) oxide (Fe2O3) and Prussian blue (PB) nanoparticles and their nanocomposite towards nitrite (NO2-) and nitric oxide (NO) oxidation in neutral and acidic media respectively was investigated on a platinum (Pt) modified electrode. Successful synthesis of these nano materials was confirmed using microscopic and spectroscopic techniques. Successful modification of the electrode was confirmed using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The results showed that the Pt-GO-Fe2O3 and Pt-GO-PB nanocomposite modified electrodes gave a faster electron transfer process in both a 5 mM Ferri/Ferro ([Fe(CN)6]3-/4-) redox probe and 0.1 M phosphate buffer solution (PBS). The Pt-GO-Fe2O3 and Pt-GO-PB electrodes also gave an enhanced NO2- and NO oxidation current compared with bare Pt and the other electrodes studied. Electrocatalytic oxidation of the analyte occurred through a simple diffusion process but were characterized with some level of adsorption. Tafel slopes b of 468.4, 305.2 mV dec-1 (NO2-, NO); and 311.5, 277.2 mV dec-1 (NO2-, NO) were obtained for the analyte at the Pt-GO-Fe2O3 and Pt-GO-PB electrode respectively. The Pt-GO-Fe2O3 limit of detection and sensitivity in NO2- and NO are 6.60 μM (0.0084 μA μM-1) and 13.04 μM (0.0160 μA μM-1) respectively, while those of the Pt-GO-PB electrode are 16.58 μM (0.0093 μA μM-1) and 16.50 μM (0.0091 μA μM-1). The LoD compared favourably with literature reported values. Pt-GO-Fe2O3 gave a better performance to NO2- and NO electrooxidation, good resistance to electrode fouling, a higher catalytic rate constant and lower limit of detection. The adsorption equilibrium constant β and the standard free energy change ΔG0 due to adsorption are 10.29 × 103 M-1 (-22.89 kJ mol-1) and 3.26 × 103 M-1 (-20.04 kJ mol-1) for nitrite and nitric oxide respectively at the Pt-GO-Fe2O3 electrode. An interference study has also been reported. The fabricated sensors are easy to prepare, cost effective and can be applied for real sample analysis of nitrite and nitric oxide in food, water, biological and environmental samples.
- Adekunle, Abolanle S.,Lebogang, Seonyane,Gwala, Portia L.,Tsele, Tebogo P.,Olasunkanmi, Lukman O.,Esther, Fayemi O.,Boikanyo, Diseko,Mphuthi, Ntsoaki,Oyekunle, John A. O.,Ogunfowokan, Aderemi O.,Ebenso, Eno E.
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- Morphology control and large piezoresponse of hydrothermally synthesized lead-free piezoelectric (Bi0.5Na0.5)TiO3 nanofibres
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Lead-free piezoelectric bismuth sodium titanate (BNT) nanostructures were synthesised using a low-temperature hydrothermal technique. It is found that the phase and morphology of the products are strongly dependent on the composition and concentration of the precursors, as well as the processing conditions. Through optimising the synthesis parameters, well-crystallized BNT nanofibers with 150-200 nm diameters and ~5 μm length were obtained. The BNT fibres show a pure perovskite phase with (011) orientation along the length direction. A piezoelectric constant of d33 = ~15 pm V-1 in the diameter direction was observed for these BNT nanofibers.
- Ghasemian, Mohammad Bagher,Lin, Qianru,Adabifiroozjaei, Esmaeil,Wang, Feifei,Chu, Dewei,Wang, Danyang
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p. 15020 - 15026
(2017/03/17)
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- A highly selective and simultaneous determination of ascorbic acid, uric acid and nitrite based on a novel poly-N-acetyl-l-methionine (poly-NALM) thin film
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This paper demonstrates the facile fabrication of an N-acetyl-l-methionine (NALM) polymer film on a glassy carbon electrode (GCE) by an electropolymerization technique. Atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and electrochemical techniques such as cyclic voltammetry (CV) and differential pulse voltammetry (DPV) were used to characterize the modified electrode. This poly-NALM/GCE not only exhibits strong electrocatalytic activity towards the oxidation of ascorbic acid (AA), uric acid (UA) and nitrite with a shift in oxidation potential towards the less positive side, but also enhances peak current responses at physiological pH (7.2) conditions. Further, the overlapped anodic voltammetric peaks of the three analytes on a bare GC electrode were well-resolved into their independent oxidation peaks at the poly-NALM/GC modified electrode with a peak separation of 160 and 590 mV for AA-UA and UA-nitrite, respectively. Under the optimal experimental conditions, the anodic peak currents of AA, UA and nitrite increased linearly within the concentration ranges 10-1000 μM, 1-600 μM and 1-500 μM with correlation coefficients of 0.990, 0.996 and 0.994, respectively. The detection limits are 0.97, 0.34 and 0.75 μM for AA, UA and nitrite ion, respectively (S/N = 3). The modified electrode was successfully utilized to determine AA, UA and nitrite ion simultaneously in real samples such as human urine and tap water samples.
- Kannan, Ayyadurai,Sivanesan, Arumugam,Kalaivani, Govindasamy,Manivel, Arumugam,Sevvel, Ranganathan
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p. 96898 - 96907
(2016/10/25)
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- BDO a harmless treatment method for organic waste
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The invention discloses a method for innocent treatment of a BDO organic wastewater. The method comprises the following steps: firstly, carrying out dealcoholizing treatment on the BDO organic wastewater to obtain a normal butanol product, rectifying tower overhead distillate and a water enriching layer; carrying out further rectifying extraction on the rectifying tower overhead distillate to obtain an oily mixture at the tower bottom; combusting the oily mixture in a conduction oil heating furnace so as to heat conduction oil; and dissolving the combustion waste residues with and mixing with nitric acid, so as to prepare sodium nitrate. According to the method disclosed by the invention, the BDO organic wastewater is processed to obtain an alcohol product and sodium nitrate, and meanwhile, tar with a high heat value is fully utilized, thus innocent treatment of pollutants is achieved; the whole method has the advantages that the steps are simple, conditions are easy to control, the product yield is high, all obtained products are good in purity, equipment investment is low, the production cost is low, and energy consumption is low. The method has economic and social significance on the aspects of improvement of the production additional value, reduction of environmental pollution and the like.
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Paragraph 0023; 0024; 0025
(2017/02/24)
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- Multistep soft chemistry method for valence reduction in transition metal oxides with triangular (CdI2-type) layers
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Transition metal (M) oxides with MO2 triangular layers demonstrate a variety of physical properties depending on the metal oxidation states. In the known compounds, metal oxidation states are limited to either 3+ or mixed-valent 3+/4+. A multistep soft chemistry synthetic route for novel phases with M2+/3+O2 triangular layers is reported.
- Blakely, Colin K.,Bruno, Shaun R.,Poltavets, Viktor V.
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supporting information
p. 2797 - 2800
(2014/03/21)
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- ANTIMICROBIAL SOLUTION COMPRISING A METALLIC SALT AND A SURFACTANT
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The present invention concerns solutions having an antimicrobial activity. The solutions described herein comprise particles containing slightly soluble metallic salt and surfactant. In the solutions described herein, the molar ratio between the slightly soluble metallic salt and the surfactant is lower than or equal to about 1. Also described are substrates comprising the solutions, methods for producing substrate comprising the solutions, methods for producing the solutions and uses of the solutions for substrate finishing and substrate sanitization.
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Page/Page column 27-28
(2008/06/13)
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- Weakly coordinating anions: Crystallographic and NQR studies of halogen-metal bonding in silver, thallium, sodium, and potassium halomethanesulfonates
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35Cl, 79,81Br, and 127l NQR (nuclear quadrupole resonance) spectroscopy in conjunction with X-ray crystallography is potentially one of the best ways of characterizing secondary bonding of metal cations such as Ag+ to halogen donor atoms on the surfaces of very weakly coordinating anions. We have determined the X-ray crystal structure of Ag(O3SCH2Cl) (a = 13.241(3) A; b = 7.544(2) A; c = 4.925(2) A; orthorhombic; space group Pnma; Z = 4) and compared it with the known structure of Ag(O3SCH2Br) (Charbonnier, F.; Faure, R.; Loiseleur, H. Acta Crystallogr., Sect. B 1978, 34, 3598-3601). The halogen atom in each is apical (three-coordinate), being weakly coordinated to two silver ions. 127I NQR studies on Ag(O3SCH2I) show the expected NQR consequences of three-coordination of iodine: substantially reduced NQR frequencies v1 and v2 and a fairly small NQR asymmetry parameter ν. The reduction of the halogen NQR frequency of the coordinating halogen atom in Ag(O3SCH2X) becomes more substantial in the series X = Cl + strengthens in this series, as expected from hard-soft acid-base principles. The numbers of electrons donated by the organic iodine atom to Ag+ have been estimated; these indicate that the bonding to the cation is weak but not insignificant. We have not found any evidence for the bonding of these organohalogen atoms to another soft-acid metal ion, thallium. A scheme for recycling of thallium halide wastes is included.
- Wulfsberg, Gary,Parks, Katherine D.,Rutherford, Richard,Jackson, Debra Jones,Jones, Frank E.,Derrick, Dana,IIsley, William,Strauss, Steven H.,Miller, Susie M.,Anderson, Oren P.,Babushkina,Gushchin,Kravchenko,Morgunov
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p. 2032 - 2040
(2008/10/08)
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- Uptake and reaction of ClONO2 on NaCl and synthetic sea salt
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The uptake and reaction of chlorine nitrate (ClONO2) on NaCl and synthetic sea salt (SSS) powders was studied at 298 K using a Knudsen cell interfaced to a quadrupole mass spectrometer. A time-dependent uptake coefficient was observed, with a large initial uptake coefficient measured for most samples of γinit > 0.1, followed by a smaller and slowly declining uptake coefficient at longer reaction times. This behavior is shown to be consistent with uptake into, and reaction in, water on the salt surface. The steady-state uptake coefficient on NaCl was invariant over a range of ClONO2 concentrations from 1012 to 1013 molecules cm-3 but was dependent on the number of salt particle layers in a manner consistent with approximately two layers of particles being available for reaction. The results of experiments using monolayers and sub-monolayers of salts, where the available reactive surface is known, give an uptake coefficient at longer times after the rapid initial uptake for ClONO2 on NaCl of γt = (6.5 ± 3.0) × 10-3 (2σ). The larger uptake coefficient obtained initially compared to longer reaction times helps to reconcile different values reported earlier by other research groups for this reaction. The uptake coefficient on SSS, which holds more water, is much larger than that for NaCl, with γinit = (0.42-0.42+0.46) and γt = (0.16-0.16+0.20 (2σ). At the higher uptake coefficients measured for SSS, this reaction could be a significant source of Cl2 in the marine boundary layer if chlorine nitrate is available at a constant concentration of ~5 ppt.
- Gebel, Michael E.,Finlayson-Pitts, Barbara J.
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p. 5178 - 5187
(2007/10/03)
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- Thermal studies of N-phenylethane-1,2-diamine complexes of nickel(II) in the solid state
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[NiL3]X2, (where L = N-phenylethane-1,2-diamine and X = I- and ClO4-), [NiL2X2] (X is Cl-, Br-, NCS-, 0.5SO42- or 0.5SeOsu
- Das,Chaudhuri
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p. 895 - 902
(2008/10/08)
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- In situ monitoring of the NaCl + HNO3 surface reaction: The observation of mobile surface strings
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The reaction of single-crystal NaCl(100) with dry HNO3 was monitored using atomic force microscopy in contact mode. Initial exposure to dry HNO3 results in the growth of a two-dimensional metastable layer of NaNO3 to nearly complete surface coverage. Exposure of this metastable NaNO3 layer to small amounts of H2O produces deliquescence of the surface with concomitant rearrangement of the NaNO3 adlayer to form unusual mobile strings presumed to contain NaNO3. These strings are transient and eventually crystallize to form rhombohedral NaNO3 crystals sitting on top of the NaCl surface.
- Zangmeister, Christopher D.,Pemberton, Jeanne E.
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p. 8950 - 8953
(2007/10/03)
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- Diffuse reflectance infrared studies of the reaction of synthetic sea salt mixtures with NO2: A key role for hydrates in the kinetics and mechanism
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The heterogeneous reactions of oxides of nitrogen with NaCl as a model for sea salt particles have been the focus of many studies, due to their potential to act as precursors to atomic halogens in the troposphere. While a great deal has been learned about the kinetics and mechanisms of NaCl reactions, it is not clear how well this extrapolates to the complex mixture of inorganics found in sea salt. We report here diffuse reflectance infrared Fourier transform spectrometry (DRIFTS) studies in which nitrate formation on the salt surface is followed with time during the reaction of gaseous NO2 with synthetic sea salt at 298 K in the presence of either He or air as the carrier gas. The infrared bands due to surface nitrate formed during the reaction of NO2 are shown to be similar to those from the reaction of MgCl2·OH2O, a major hydrate in the mixture which was used as a surrogate for all of the crystalline hydrates. Significant amounts of surface-adsorbed water are generated in the reaction of synthetic sea salt with NO2 in air, which appears at least in part to be due to liberation of bound water of hydration in the crystalline hydrates. The reaction order with respect to NO2 is (1.8 ± 0.2) (2σ) when the reaction of the synthetic sea salt is carried out in He but only (1.2 ± 0.2) (2σ) when air is used as the carrier gas. For comparison, the reaction order for the NO2-NaCl reaction was reexamined and found to be (1.8 ± 0.3) (2σ) in He and (1.6 ± 0.3) (2σ) in air, in agreement with previous work19 using this technique. It is assumed for slopes ≥ 1.6 that N2O4 is the reacting species for the purpose of expressing the kinetics in the usual form of reaction probabilities. For the N2O4-NaCl reactions in He and air, and for the N2O4-synthetic sea salt reaction in He, the reaction probabilities are similar (~10-4). The reaction of synthetic sea salt with NO2 in the presence of air is treated in terms of a first-order reaction with NO2 being the reactive species, which gives a reaction probability for the NO2-synthetic sea salt reaction of ~10-8. The atmospheric implications are discussed.
- Langer, Sarka,Pemberton, R. Sean,Finlayson-Pitts, Barbara J.
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p. 1277 - 1286
(2007/10/03)
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- The reaction of ionic nitrites with liquid dinitrogen tetraoxide
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The reaction of nitrites of Na+, Bun4N+ and Ni2+ with liquid dinitrogen tetraoxide and the factors affecting the rate and extent of the reaction have been studied. Oxidation occurs to the corresponding nitrate in a manner consistent only with the heterolytic dissociation of N2O4 into NO+ and NO3. The synthesis of anhydrous Ni(NO2)2 is described in detail.
- Addison, C. Clifford,Arrowsmith, Stephen,Dove, Michael F. A.,Johnson, Brian F. G.,Logan, Norman,Wood, Simon A.
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p. 781 - 784
(2008/10/09)
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- Solution Equilibria and Redox Reactivities of a Dioxo-bridged Manganese Complex
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The dinuclear complex (3+) (bipy = 2,2'-bipyridyl) 1 was stabilised in bipy-Hbipy(+) buffer where it coexists with the diaqua derivative (3+) 2 (equilibrium constant KH).Reduction of 1 by NO2(-) has been found to be kinetically insignificant, but that of 2 is rapid, quantitative and follows the sequence Mn(III)Mn(IV) (Mn(III))2 Mn(II)Mn(III) 2Mn(II).In the presence of an excess of NO2(-), first-order kinetics was observed at 830 nm, but a biphasic profile at 525 nm.At 30.0 deg C and I = 1.0 mol dm-3, k1KH1 and K2KH2 are 34.9 +/- 0.8 and 3.3 +/- 0.2 dm3 mol-1 s-1 respectively.Added bipy retards, while Mn(2+) accelerates, the reaction.The solution equilibria are much more complex for 1 in HNO3 and H3PO4, but the known solution chemistry of 1 in such different media may be correlated by a unified reaction scheme.
- Chaudhuri, Swapan,Mukhopadhyay, Subrata,Banerjee, Rupendranath
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p. 621 - 624
(2007/10/02)
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- Heterogeneous Reaction of HNO3(g) + NaCl(s) -> HCl(g) + NaNO3(s) and N2O5(g) + NaCl(s) -> ClNO2(g) + NaNO3(s)
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The hetrogeneous reactions of HNO3(g) + NaCl(s) -> HCl(g) + NaNO3(s) (eq 1) and N2O5(g) + NaCl(s) -> ClNO2(g) + NaNO3(s) (eq 2) were investigated over the temperature range 223-296 K in a flow-tube reactor coupled to a quadrupole mass spectrometer.Either a chemical ionization mass spectrometer (CIMS) or an electron-impact ionization mass spectrometer (EIMS) was used to provide suitable detection sensitivity and selectivity.In order to mimic atmospheric conditions, partial pressures of HNO3 and N2O5 in the range 6 x 10-8 ca. 2 x 10-6 Torr were used.Granule sizes and surface roughness of the solid NaCl substrates were determined by us ing a scanning electron microscope.For dry NaCl substrates, decay rates of HNO3 were used to obtain γ(1) = 0.013 +/- 0.004 (1?) at 296 K and >0.008 at 223 K, respectively.The error quoted is the statistical error.After all corrections were made, the overall error, including systematic error, was estimated to be about a factor of 2.HCl was found to be the sole gas-phase product of reaction 1.The mechanism changed from heterogeneous reaction to predominantly physical adsorption when the reactor was cooled from 296 to 223 K.For reaction 2 using dry salts, γ(2) was found to be less then 1.0 x 10-4 at both 223 and 296 K.The gas-phase reaction product was identified as ClNO2 in previous studies using an infrared spectrometer.An emhancement in reaction probability was observed if water was not completely removed from salt surfaces, probably due to the reaction of N2O5(g) + H2O(s) -> 2HNO3(g).Our results are compared with previous literature values obtained using diferent experimental techniques and conditions.The implications of the present results for the enhancement of the hydrogen chloride column density in the lower stratosphere after EI Chichon volcanic eruption and for the chemistry of HCl and HNO3 in the marine troposphere are discussed.
- Leu, Ming-Taun,Timonen, Raimo S.,Keyser, Leon F.,Yung, Yuk L.
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p. 13203 - 13212
(2007/10/02)
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- Synthetic and structural studies of a series of soluble cerium (IV) alkoxide and alkoxide nitrate complexes
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The reactions of (NH4)2Ce(NO3)6 (CAN) with 2-8 equiv of NaOCMe3 in THF and in tert-butyl alcohol have been studied. A series of ceric alkoxide complexes of general formula Ce(OCMe3)a,(NO3)b(solvent) cNad (a = 1-6; b = 0-3; c = 2, 4; d = 0, 2; a + b = 4 + d) have been identified as well as Ce2(OCMe3)9Na and Ce3(OCMe3)10O. Interconversion of these complexes by treatment with NaOCMe3 or NH4NO3 has also been studied. CAN reacts with 3 equiv of NaOCMe3 in THF to form Ce(OCMe3)(NO3)3(THF)2 (1). In tert-butyl alcohol this reaction forms the HOCMe3 solvate Ce(OCMe3)(NO3)3(HOCMe3)2 (1′). 1 reacts with 1 equiv of NaOCMe3 and CAN reacts with 4 equiv of NaOCMe3 to form Ce(OCMe3)2(NO3)2(THF)2 (2). In tert-butyl alcohol solvent, 1′ reacts with NaOCMe3 to form Ce(OCMe3)2(NO3)2(HOCMe 3)2 (2′). 2′ crystallizes from a concentrated toluene solution at -34°C in space group P1 (No. 2; Ci1) with a = 10.7548 (56) A?, b = 11.0853 (49) A?, c = 12.4403 (56) A?, α = 72.760 (34)°, β = 88.190 (39)°, γ = 69.050 (35)°, V = 1318.0 (11) A?3, and Z = 2 for Dcalcd = 1.41 g cm-3. Least-squares refinement of the model based on 4935 observed reflections converged to RF = 7.7%. If each NO3 ligand is taken to occupy just one coordination site, the structure of 2′ is that of a distorted octahedron in which identical ligands are trans to each other. Ce(OCMe3)3(NO3)(THF)2 (3) can be prepared from 2 or 2′ and NaOCMe3 or from CAN and 5 equiv of NaOCMe3. Ce(OCMe3)4(THF)2 (4) is prepared from 3 and NaOCMe3 or from CAN and 6 equiv of NaOCMe3. The reaction of 4 with 2 equiv of NaOCMe3 or reaction of CAN with 8 equiv of NaOCMe3 forms Ce(OCMe3)6Na2(THF)4 (5). 5 crystallizes from dimethoxyethane (DME) at -34°C as Ce(OCMe3)6Na2(DME)2 (5′) in space group Pna21 with a = 20.5337 (36) A?, b = 10.9557 (23) A?, c = 19.4128 (38) A?, V = 4367.1 (15) A?3, and Z = 4 for Dcalcd = 1.22 g cm-3. Least-squares refinement of the model based on 9092 observed reflections converged to RF = 4.9%. 5′ contains a distorted-octahedral arrangement of OCMe3 groups around cerium. Each sodium ion is coordinated by one DME ligand and a facial set of three OCMe3 groups of the Ce(OCMe3)62- octahedron. The reaction of 4 with 1/2 equiv of NaOCMe3 forms Ce2(OCMe3)9Na (6). Both 4 and 6 in toluene slowly form Ce3(OCMe3)10O (7). Complex 5 reacts with 5 equiv of NH4NO3 to form 1 in quantitative yield.
- Evans, William J.,Deming, Timothy J.,Olofson, Jeffrey M.,Ziller, Joseph W.
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p. 4027 - 4034
(2008/10/08)
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- Thermal Decomposition of Sodium trans-Hyponitrite
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Samples of amorphous sodium trans-hyponitrite (Na2N2O2), heated with a continuous rise in temperature in the absence of oxygen, decompose suddenly between 360 and 390 deg C.The decomposition products are Na2O and N2O, along with secondary reaction product
- Abata, J. D.,Dziobak, M. P.,Nachbor, M.,Mendenhall, G. D.
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p. 3368 - 3372
(2007/10/02)
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- Reaction of thorium nitrate with sodium thioarsenate as a function of pH
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The stoichiometries of the compounds formed by the interaction of thorium nitrate and sodium orthothioarsenate/pyrothioarsenate have been established as 3ThS2*As2S5 and ThS2*As2S5 employing pH and conductometric titrations.Formation of these compounds is supported by analytical determinations.
- Prasad, Shiva
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p. 536 - 537
(2007/10/02)
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- ON THE ELECTRICAL PROPERTIES OF POLYCRYSTALLINE DELAFOSSITE-TYPE AgNiO2.
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AgNiO//2 is prepared by reaction of molten silver nitrate with NaNiO//2. Powder X-ray diffraction shows that the compound has the delafossite structure of space group R OVER BAR 3m. Magnetic data give evidence for the localization of the 3d-electrons of most Ni atoms. Electrical conductivity and thermoelectric measurements performed between 4. 2 and 300 K on polycrystalline samples show that AgNiO//2 behaves like a semimetal. N-type and p-type charge carriers are created by a slight overlapping of the d band of silver atoms with the sigma antibonding band resulting from the overlapping of the Ni 3d- and O 2p-orbitals.
- Wichainchai,Dordor,Doumerc,Marquestaut,Pouchard,Hagenmuller
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p. 126 - 131
(2008/10/08)
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- KINETICS OF INTERACTION OF GLASERITE WITH CALCIUM NITRATE SOLUTION.
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The authors report a study of the kinetics of interaction of glaserite of mono- and polydisperse composition with calcium nitrate solution at 25-80 degree . It is shown that the process includes formation of an intermediate product, syngenite, which passes into gypsum at 80 degree . It is also shown that difficultly soluble reaction products crystallize both in the bulk solution and on the surface of the glaserite particles, where they form a gradually thickening crust whose porosity varies with time and which hinders free diffusion of the reactants. The thickness of this crust as a function of temperature was calculated theoretically and measured experimentally.
- Sokolov,Stepanova,Murav'ev
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p. 1373 - 1376
(2008/10/08)
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- Oxidation of Nitrite Ion by Bis(2-ethyl-2-hydroxybutyrato)oxochromate(V)
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Bis(2-ethyl-2-hydroxybutyrato)oxochromate(V) oxidises NO2(-) to NO3(-) in acetic acid-acetate buffers (pH 3.7 to 4.6) with an oxygen atom transfer in the rate-determining step.The specific rate is unaffected by the addition of unbound carboxylato ligand, suggesting the attack by NO(+)(OAc)(-) on the oxygen end of chromium(V) complex.These results are at variance with those of earlier works .The initial product of the reaction has been identified as a chelated or non-chelated monocarboxylatochromium(III) compound.
- Rajavelu, A.,Srinivasan, Vangalur S.
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p. 963 - 964
(2007/10/02)
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