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951.
Sbai K. Abouimrane A. El Kababi K. Vilminot S. 《Journal of Thermal Analysis and Calorimetry》2002,68(1):109-122
We have studied the thermal behaviour under atmospheric pressure of isotypic tetrahydrate cyclotriphosphates MII(NH4)4(P3O9)2x4H2O (M
II=Cu, Ni and Co), between 25 and 1400°C, by X-ray diffraction, thermal analyses (TG and DTA) and infrared spectrometry. This
study shows that the series of the compounds MII(NH4)4(P3O9)2x4H2O (M
II=Cu, Ni and Co) after elimination of water, in two different stages, and ammonia leads, at 400°C to cyclotetraphosphate M2
IIP4O12 crystallized and to a thermal residue with a formula H4P4O12 which undergoes under a thermal degradation by evolving water and pentoxide phosphorus. The kinetic characteristics of the
dehydration and elimination of ammonia have been determinated. The vibrational spectra of Cu(NH4)4(P3O9)2x4H2O were examined and interpreted, in the domain of the valency frequencies, on the basis of the crystalline structure of its
isotypic compound Co(NH4)4(P3O9)2x4H2O whose cycle has the site symmetry C1, of our results of the calculation of the IR frequencies and the successive isotopic substitutions of the equivalent atoms
(3P, 3Oi and 6Oe belonging to the P3Oi3Oe6 ring) of the P3O9
3− cycle with high symmetry D3h.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
952.
The brown crystals of [NEt4]2[Se3Br8(Se2Br2)] ( 1 ) were obtained when selenium and bromine reacted in the solution of acetonitrile in the presence of tetraethylammonium bromide. The crystal structure of 1 has been determined by the X‐ray methods and refined to R = 0.0308 for 10433 reflections. The crystals are monoclinic, space group P21 with Z = 2 and a = 12.0393(3) Å, b = 11.8746(3) Å, c = 13.1946(3) Å, β = 96.561(1)° (123 K). In the solid state structure the anion of 1 is built up of Se3Br8 unit which consists of a triangular arrangement of three planar SeBr4 units sharing a common edge through two μ3‐bridging Br atoms, and one Se2Br2 molecule which is linked to one of μ3‐bridging Br atoms. The three SeII atoms form a triangle which is almost perpendicular to the planes given by three SeBr4 moieties. The contact between the μ3Br and the SeI atom of the Se2Br2 molecule is 3.1711(8) Å and can be interpreted as a bond of the donor‐acceptor type with the μ3Br as donor and the Se2Br2 molecule as acceptor. The terminal SeII‐Br and μ3Br‐SeII bond lengths are in the ranges 2.3537(7)–2.4737(7) Å and 2.7628(7)–3.1701(7) Å, respectively. The bond lengths in coordinated Se2Br2 molecule are: SeI‐SeI = 2.2636(9) Å, SeI‐Br = 2.3387(11) and 2.3936(8) Å. 相似文献
953.
Biswanath Das D. Nandan Kumar Keetha Laxminarayana B. Ravikanth 《Helvetica chimica acta》2007,90(7):1330-1334
The synthesis of 14‐aryl‐ or 14‐alkyl‐14H‐dibenzo[a,j]xanthenes 3 involving the treatment of naphthalen‐2‐ol ( 1 ) with arenecarboxaldehydes or alkanals 2 in the presence of HClO4?SiO2 as a heterogeneous catalyst was achieved (Table 1), and this reaction was extended to the preparation of N‐[(2‐hydroxynaphthalen‐1‐yl)methyl]amides 5 by a three‐component reaction with urea ( 4a ) or an amide 4b – d as a third reactant (Table 2). 相似文献
954.
J.W.H. van KrevelJ.W.T. van Rutten H. MandalH.T. Hintzen R. Metselaar 《Journal of solid state chemistry》2002,165(1):19-24
New interesting luminescent α-sialon (M(m/val+)val+ Si12-(m+n) Al(m+n)OnN(16−n)) (M=Ca, Y) materials doped with Ce, Tb, or Eu have been prepared and their luminescence properties studied. These show that Tb and Ce are in the 3+ and Eu in the 2+ state. Low-energy 4f↔5d transitions are observed as compared to the luminescence of these ions doped in oxidic host-lattices. This is partially explained by the nitrogen-rich coordination of the rare-earth ion and partially by the narrow size of the lattice site. The latter gives rise to a strong crystal-field splitting of the 5d band and a rather large Stokes shift for Ce3+ and Eu2+ (6500-7500 and 7000-8000 cm−1, respectively). For (Y,Tb)-α-sialon the Tb3+ 4f→5d excitation band (∼260 nm) is in the low-energy host-lattice absorption band (?290 nm), giving rise to a strong absorption for 254-nm excitation, but a low quantum efficiency. The latter is due to photoionization processes or selective excitation of Tb3+ at the defect-rich surface, resulting in radiationless transitions. Ce- and Eu-doped Ca-α-sialon show bright long-wavelength luminescence (maxima at 515-540 and 560-580 nm for Ce and Eu, respectively) with a high quantum efficiency and high absorption for 365- and 254-nm excitation. The Eu2+ emission intensity and absorption increases for increasing m, which is explained by the Eu2+ richer α-sialon composition. The position of the Eu2α emission does not shift with changing composition of the host-lattice (m, n values), indicating that the local coordination of the Eu2+ ion is hardly dependent on the matrix composition. 相似文献
955.
Joseph M. Levy Athos C. Rosselli David S. Boyer Kathryn Cross 《Journal of separation science》1990,13(6):418-421
The usefulness and ease of utilizing supercritical fluid extraction (SFE) directly coupled to capillary gas chromatography (GC) as quantitative or qualitative analytical problem-solving tools will be demonstrated. As an alternative to conventional liquid solvent extractions, SFE presents itself as a means to achieve high extraction efficiencies of different compounds in complex solid matrices in very rapid tims frames. Moreover, SFE has an additional advantage of being able to achieve distinct extraction selectivities as a function of the solubilizing power of the supercritical fluid extracting phase. For on-line SFE/GC, the extraction effluent is directly transferred to the analytical chromatograph. On-line SFE/GC involves the decompression of pressurized extraction effluent directly into a heated, unmodified capillary split injection port of the GC. In this respect, SFE introduction into GC can be used as an alternative means of GC injection, comparable to such modes of injection as pyrolysis and thermal desorption. This paper will show applications of SFE/GC where mass spectrometric detection together with flame ionization detection was used for component identification from environmental, tobacco, and petroleum matrices. 相似文献
956.
Spectrophotometric Determination of Rhenium(IV) with Thiocyanate,TX-100 and N,N′-Diphenylbenzamidine
A spectrophotometric method to determine rhenium(IV) at trace level is based on the extraction of Re(IV)-SCN? complex in sulphuric acid media with N,N′-diphenylbenzamidine(DPBA) in presence of a non-ionic surfactant triton X-100 (TX-100) in chloroform. The complex shows maximum absorbance at 435 nm with amolar absorptivity value of 4.24 × 104 L mol?1 cm?1 at an acidity range 3.5-6.5 M H2SO4. The method followed Beer's Law for the system Re(IV)-SCN?(TX-100)-DPBA upto 4.0 μg Re(IV) mL?1. The detection limit of the method is 5 ppb. None of the tested foreign ions, except molybdenum(VI), interfere with the determination of rhenium. The interference due to molybdenum could effectively be removed by prior precipitation with oxine. The effect of various analytical parameters on the extraction of the metal are discussed. 相似文献
957.
J. David Pinkston Thomas E. Delaney Donald J. Bowling Thomas L. Chester 《Journal of separation science》1991,14(6):401-406
Components of hamster feces ranging from low molecular weight fatty acids through the expected range of triglycerides have been eluted in a single SFC run with simultaneous pressure and temperature programming. Temperature programming from 140°C to 240°C was required to provide optimum conditions for separation of the fatty acids and to move the elution region of the sterol esters away from that of the triglycerides. Data from chemical ionization and electron impact mass spectrometry of compounds separated by SFC were used to confirm identities suggested by retention measurements and to provide tentative identities of unknown compounds. SFC with flame ionization detection was used to compare Soxhlet extraction, off-line supercritical fluid extraction (SFE), and on-line SFE of the feces. Although samples obtained by Soxhlet extraction and SFE produced very similar chromatograms, SFE required far less time and consumed much smaller quantities of organic solvent. 相似文献
958.
Reduced Clusters with Remarkable Topological and Electronic Properties of the Type of [V18O42(X)]n? (X = SO4, VO4) with Td-Symmetry and Related Clusters [V(18—p)As2pO42(X)]m? (X = SO3, SO4, H2O; p = 3, 4) The novel cluster-compounds Na6[V18O42H9(VO4)] · 21 H2O, (NH4)8[V18O42(SO4)] · 25 H2O, K6[V15As6O42(H2O)] · 8 H2O, (NH4)6[V14As8O42(SO3)], (NH4)6[V14As8O42(SO4)] and [N(CH3)3]4[4V14As8042(H20)] were prepared and characterized by IR- and UV/Vis/NIR-spectroscopy, magnetic measurements and complete crystal structure analysis. For structural data see Inhaltsübersicht. Topological relations to the rhombicuboctahedron spanned by 24 0-atoms of the genuine hypothetical a-Keggin ion, at which the square planes are capped by V?O or As2O groups, are discussed. Of particular interest are the ?extended”? Keggin ions [V18O42(X)]n- (X = SO4 VO4), (formaly derived from the hypothetical genuine a-Keggin ion by addition of six V?O groups) which have quite different electron populations in spite of the same structure of their cluster shells. 相似文献
959.
Andrea GotiMartin F. Semmelhack 《Journal of organometallic chemistry》1994,470(1-2):C4-C7
Arene displacement from the title complex occurs under unprecedented mild conditions in neutral media to afford (η6-arene)tricarbonylchromium complexes. The process is most effective with heteroaromatic compounds: the first synthesis of a tricarbonyl(η6-quinoline)chromium complex and the diastereoselective preparation of a (η6-indole) complex derived from L-tryptophan are reported as representative examples. 相似文献
960.
A. L. Rusanov M. L. Keshtov N. M. Belomoina A. K. Mikitaev G. B. Sarkisyan S. V. Keshtova 《Russian Chemical Bulletin》1997,46(4):777-779
Bis (p-fluorophenylethynyl) derivatives were obtained by the reaction of bisbromoaromatic compounds withp-fluorophenylacetylene in the presence of a Pd catalyst. Subsequent oxidation of these products using an I2-DMSO system led to new bis(p-fluorophenylglyoxaly)ketones, α-diketones, and heterocyclic compounds.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 810–812, April, 1997. 相似文献