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41.
Éder Lisandro de Moraes Flores Juliano Smanioto Barin Érico Marlon de Moraes Flores Valderi Luiz Dressler 《Spectrochimica Acta Part B: Atomic Spectroscopy》2007
This work deals with the determination of fluorine by solid sampling graphite furnace molecular absorption spectrometry. The molecular absorbance of aluminum monofluoride (AlF), which is produced in the vapor phase in the presence of Al3+, is measured at 227.5 nm, a non-resonant platinum line. A conventional graphite furnace program has been used with pyrolysis and vaporization temperatures of 800 and 2300 °C, respectively. Solutions of Ba2+ and Al3+ have been used to avoid fluorine losses during the pyrolysis stage and to produce AlF in the vaporization stage, respectively. Certified coal and alumina samples were analyzed using aqueous standards for calibration. The agreement between the found concentration and the certified value, or the value obtained by another method ranged from 92 to 105%, with a relative standard deviation less than 8.5%. The limit of detection and the characteristic mass was 0.17 μg g− 1 and 205 pg, respectively. 相似文献
42.
The effect of calcinations on the silica surface groups and thereby on the activity of Ziegler-Natta catalysts in ethylene homopolymerisation has been studied. Silica was calcined at different temperatures and treated with MgR2 and HCl. Silica surface groups were identified by using 1H MAS NMR and 13C and 29Si CP MAS NMR techniques. Magnesium, titanium and chlorine were measured by elemental analysis. Ziegler-Natta catalysts were prepared from these supports and subsequently used in ethylene homopolymerisation. Maximum activity was obtained with the catalyst based on 590 °C calcined silica. The results indicate that MgR2 reacts with siloxane-groups (Si-O-Si) in the 300 °C calcined silica, leaving the hydrogen-bonded hydroxyl-groups unreacted. Low activity Si-O-Ti(Cl)2-O-Si species are formed after reacting with TiCl4. The higher activity in the catalyst based on 590 °C calcined silica can be explained by the formation of -Si(R)-O-Si-O-TiCl3 groups, originating from the siloxane bridges which cannot form in 300 °C calcined silica. Other explanations for the higher activity are a higher Mg/Ti ratio or small amounts of crystal water formed in the 590 °C calcined silica. 相似文献
43.
Asmita Kumari 《Journal of solid state chemistry》2007,180(7):2013-2019
New cubic-AGaSnS4 (A=Na, K, Rb, Cs, Tl) and orthorhombic-NaGaSnS4 compounds were synthesized by solid-state reactions and characterized by X-ray diffraction and diffuse reflectance spectroscopy. Single crystals of orthorhombic-Na1.263Ga1.263Sn0.737S4 were obtained in the crystal growth attempts of sodium compound. All six new compounds have orthorhombic AgGaGeS4 and cubic BaGa2S4 structures, as determined from single crystal X-ray structures of Na1.263Ga1.263Sn0.737S4 and cubic-AGaSnS4 (A=Na, K, Rb). Orthorhombic-NaGaSnS4 and known layered-KGaSnS4 undergo structural transformation to thermodynamically stable cubic form. 相似文献
44.
Ju-Chun Huang Chien Hong Cheng Shyang Roeng Sheen Zhi Ling Lee Chien Ming Lei Maw Kuen Wu 《中国化学会会志》1996,43(2):139-143
The synthesis of bulk Y2Ba4Cu7O15-δ superconductor at atmospheric oxygen pressure via solid state sintering is reported. Temperature ranging from 860 to 890 °C as well as time interval over 2 to 15 days were used to investigate the formation of the Y2Ba4Cu7O15-δ phase. A time-temperature profile characterizing the conditions for the preparation of Y2Ba4Cu7O15-δ phase suggests the optimal condition to be sintering at 890 °C for over 10 days. Detailed results of X-ray diffraction, electrical resistivity, iodometric titration and magnetization measurements are described. 相似文献
45.
Zirconyl chloride promoted highly efficient solid phase synthesis of amide derivatives 总被引:1,自引:0,他引:1
Cherkupally Sanjeeva Reddy Adki Nagaraj Pochampally Jalapathi 《中国化学快报》2007,18(10):1213-1217
An efficient solid phase route for the synthesis of amide derivatives by the reaction of carboxylic acids with urea in the presence of catalytic amount of zirconyl chloride under microwave irradiation conditions was described.In this way,a range of interesting amide derivatives was obtained in good to excellent yields.The catalyst was recycled with fresh reactants and it gave almost similar results without significant loss of activity up to the third run. 相似文献
46.
47.
一步室温固相化学反应合成纳米氨基酸杂多电荷转移配合物(HPhe)3PMo12O40·2H2O 总被引:3,自引:0,他引:3
以Keggin结构的钼磷酸(H3PMo12O40·13H2O)与苯丙氨酸(Phe)为原料,利用一步固相化学反应于室温合成了纳米氨基酸杂多电荷转移配合物(HPhe)3PMo12O40·2H2O,采用元素分析,IR,XRD,TEM,UV和循环伏安法等手段对其进行了结构表征及性质研究.结果表明,标题化合物纳米粒子为均匀的球状,粒径约为30~40nm.该化合物中杂多阴离子部分仍保持Keggin结构,但在钼磷酸与苯丙氨酸之间发生了显著的电荷转移. 相似文献
48.
Antonio Doménech María Teresa Doménech‐Carbó Howell G. M. Edwards 《Electroanalysis》2007,19(18):1890-1900
Multivariate chemometric methods are applied for identifying earth pigments from square‐wave voltammetric measurements performed at pigment‐modified paraffin‐impregnated graphite electrodes allowing for a separation between hematite‐based earths, French ochres, Spanish ochres, siennas, umbers and green earths. This methodology is applied to the identification of the pigments in samples from the ceiling frescoes of Antonio Palomino (dated 1707) in the vaulted nave of the Sant Joan del Mercat church in Valencia (Spain). These frescoes suffered considerable damage by fire during the Spanish Civil War in 1936, resulting in severe chemical and chromatic alterations. Electrochemical data, supported by scanning electron microscopy/energy dispersive X‐ray microanalysis and Raman spectroscopy, indicate that thermal stress induced the transformation of goethite‐based yellow ochres into hematite and magnetite. 相似文献
49.
E.?V.?TsipisEmail author V.?V.?Kharton I.?A.?Bashmakov E.?N.?Naumovich J.?R.?Frade 《Journal of Solid State Electrochemistry》2004,8(9):674-680
Developments of intermediate-temperature solid oxide fuel cells (IT SOFCs) require novel anode materials with a high electrochemical activity at 800–1070 K. The polarization of cermet anodes, made of nickel, ceria and yttria-stabilized zirconia (YSZ) and applied onto a YSZ solid electrolyte, can be significantly reduced by catalytically active ceria additions, the relative role of which increases with decreasing temperature. Further improvement is observed when using Ce0.8Gd0.2O2–
(CGO) having a high oxygen ionic conductivity instead of undoped ceria, owing to enlargement of the electrochemical reaction zone. Nanocrystalline CGO powders with grain sizes of 8–35 nm were thus synthesized via the cellulose-precursor technique and introduced into Ni–CGO–YSZ cermets, and tested in contact with a (La0.9Sr0.1)0.98Ga0.8Mg0.2O3–
(LSGM) electrolyte at 873–1073 K. The results showed that the anode performance can be enhanced by additional surface activation, in particular by impregnation with a Ce-containing solution, and also by incorporation of YSZ, which probably acts as a cermet-stabilizing component. The overpotential of the surface-modified Ni–CGO (25 wt%–75 wt%) anode in a 10% H2/90% N2 atmosphere was approximately 110 mV at 1073 K with a current density of 200 mA/cm2.Presented at the OSSEP Workshop Ionic and Mixed Conductors: Methods and Processes, Aveiro, Portugal, 10–12 April 2003 相似文献
50.
Sr3(BS3)2 and Sr3(B3S6)2: Two Novel Non‐oxidic Chalcogenoborates with Boron in a Trigonal‐Planar Coordination The thioborates Sr3(BS3)2 and Sr3(B3S6)2 were prepared from strontium sulfide, amorphous boron and sulfur in solid state reactions at a temperature of 1123 K. In a systematic study on the structural cation influence on this type of ternary compounds, the crystal structures were determined by single crystal X‐ray diffraction. Sr3(BS3)2 crystallizes in the monoclinic spacegroup C2/c (No. 15) with a = 10.187(4) Å, b = 6.610(2) Å, c = 15.411(7) Å, β = 102.24(3)° and Z = 4. The crystal structure of Sr3(B3S6)2 is trigonal, spacegroup R3¯ (Nr. 148), with a = 8.605(1) Å, c = 21.542(4) Å and Z = 3. Sr3(BS3)2 contains isolated [BS3]3— anions with boron in a trigonal‐planar coordination. The strontium cations are found between the layers of orthothioborate anions. Sr3(B3S6)2 consists of cyclic [B3S6]3— anions and strontium cations, respectively. 相似文献