Beiträge zur Chemie von Molybdän und Wolfram. XI / Contributions to the Chemistry of Molybdenum and Tungsten. XI.

1973 ◽  
Vol 28 (1-2) ◽  
pp. 46-55 ◽  
Author(s):  
F. A. Schröder ◽  
J. Scherle

The direct reaction of MoO3 and WO3 with ethylenglycol and glycerol is reported. The prepared compounds were characterized by chemical analysis, IR-spectra and X-ray diffraction methods (powder and single cystal). Some chemical properties are given. All results indicate that the new compounds are derivatives of the hitherto unknown ortho-molybdic (VI) and tungstic (VI)-acids.

1993 ◽  
Vol 48 (1) ◽  
pp. 85-89 ◽  
Author(s):  
Lin Yang ◽  
Peter G. Jones ◽  
Reinhard Schmutzler

The reaction of 8 -trimethylsiloxyquinoline, 2 with PCl3, PhPCl2, and PhPF2 has furnished the corresponding 8 -quinolyl halophosphite derivatives, 3-5 . The synthesis of two metal complexes, 8 and 9, of 4 with Au(I) and Pt(II) is described. The new compounds were characterized by elemental analysis and by 1H and 31P NMR spectroscopy. A single crystal X-ray diffraction study of 4 has been conducted; a short intramolecular P ··· N contact (230.9 pm) and a long P-Cl bond (218.7 pm) were observed.


Author(s):  
M. Vallet-Regí ◽  
M. Parras ◽  
J.M. González-Calbet ◽  
J.C. Grenier

BaFeO3-y compositions (0.35<y<0.50) have been investigated by means of electron diffraction and microscopy to resolve contradictory results from powder X-ray diffraction data.The samples were obtained by annealing BaFeO2.56 for 48 h. in the temperature range from 980°C to 1050°C . Total iron and barium in the samples were determined using chemical analysis and gravimetric methods, respectively.In the BaFeO3-y system, according to the electron diffraction and microscopy results, the nonstoichiometry is accommodated in different ways as a function of the composition (y):In the domain between BaFeO2.5+δBaFeO2.54, compositional variations are accommodated through the formation of microdomains. Fig. la shows the ED pattern of the BaFeO2.52 material along thezone axis. The corresponding electron micrograph is seen in Fig. 1b. Several domains corresponding to the monoclinic BaFeO2.50 phase, intergrow with domains of the orthorhombic phase. According to that, the ED pattern of Fig. 1a, can be interpreted as formed by the superposition of three types of diffraction maxima : Very strong spots corresponding to a cubic perovskite, a set of maxima due to the superposition of three domains of the monoclinic phase along [100]m and a series of maxima corresponding to three domains corresponding to the orthorhombic phase along the [100]o.


2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihaela Flondor ◽  
Ioan Rosca ◽  
Doina Sibiescu ◽  
Mihaela-Aurelia Vizitiu ◽  
Daniel-Mircea Sutiman ◽  
...  

In this paper the synthesis and the study of some complex compounds of Fe(III) with ligands derived from: 2-(4-chloro-phenylsulfanyl)-1-(2-hydroxy-3,5-diiodo-phenyl)-ethanone (HL1), 1-(3,5-dibromo-2-hydroxy-phenyl)-2-phenylsulfanyl-ethanone(HL2), and 2-(4-chloro-phenylsulfanyl)-1-(3,5-dibromo-2-hydroxy-phenyl)-ethanone (HL3) is presented. The characterization of these complexes is based on method as: the elemental chemical analysis, IR and ESR spectroscopy, M�ssbauer, the thermogravimetric analysis and X-ray diffraction. Study of the IR and chemical analysis has evidenced that the precipitates form are a complexes and the combination ratio of M:L is 1:2. The central atoms of Fe(III) presented paramagnetic properties and a octaedric hybridization. Starting from this precipitation reactions, a method for the gravimetric determination of Fe(III) with this organic ligands has been possible. Based on the experimental data on literature indications, the structural formulae of the complex compounds are assigned.


1982 ◽  
Vol 47 (4) ◽  
pp. 1069-1077 ◽  
Author(s):  
Karel Mádlo ◽  
František Hanousek ◽  
Antonín Petřina ◽  
Jaroslav Tláskal

Ferrous sulphate was oxidized by potassium chlorate in the pH region 2-7 and at temperatures ranging from 298.1 to 323.1 K and various hydrolytic products of Fe(III) were separated and indentified. The separated solid ferric products were analyzed using a combination of the chemical analysis, IR spectroscopy, X-ray diffraction, and electron microscopy. The following substances were found as major components of the products: Fe2O3.n H2O ("ferric gel"), Fe2O3.n H2O with bound SO2-4 ions ("sulphogel"), α-FeO(OH), γ-FeO(OH) and Fe3O4. Their amount depends particularly on the pH temperature of the reaction medium.


Materials ◽  
2021 ◽  
Vol 14 (9) ◽  
pp. 2160
Author(s):  
Alexander Bogdanov ◽  
Ekaterina Kaneva ◽  
Roman Shendrik

Elpidite belongs to a special group of microporous zirconosilicates, which are of great interest due to their capability to uptake various molecules and ions, e.g., some radioactive species, in their structural voids. The results of a combined electron probe microanalysis and single-crystal X-ray diffraction study of the crystals of elpidite from Burpala (Russia) and Khan-Bogdo (Mongolia) deposits are reported. Some differences in the chemical compositions are observed and substitution at several structural positions within the structure of the compounds are noted. Based on the obtained results, a detailed crystal–chemical characterization of the elpidites under study was carried out. Three different structure models of elpidite were simulated: Na2ZrSi6O15·3H2O (related to the structure of Russian elpidite), partly Ca-replaced Na1.5Ca0.25ZrSi6O15·2.75H2O (close to elpidite from Mongolia), and a hypothetical CaZrSi6O15·2H2O. The vibration spectra of the models were obtained and compared with the experimental one, taken from the literature. The strong influence of water molecule vibrations on the shape of IR spectra of studied structural models of elpidite is discussed in the paper.


Crystals ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 129
Author(s):  
Liana Vella-Zarb ◽  
Ulrich Baisch

There is much interest and focus on solid forms of famciclovir. However, in spite of the abundance of reported differences in oral bioavailability, compressibility, and other physical–chemical properties of the various crystal forms of this drug, very little precise structural analysis is available in the literature to date. The form used in the commercial formulation is the anhydrous form I. Patents and patent applications report three different anhydrous crystalline forms on the basis of unindexed powder diffraction patterns. Single-crystal and variable-temperature X-ray diffraction experiments using the commercially available anhydrous form of famciclovir were carried out and led not only to the crystal structure determination of the anhydrous form I, but also to discovery of a new crystal form of anhydrous famciclovir from powder data.


2012 ◽  
Vol 217-219 ◽  
pp. 733-736
Author(s):  
Xiu Mei Han ◽  
Shu Ai Hao ◽  
Ying Ling Wang ◽  
Gui Fang Sun ◽  
Xi Wei Qi

Zn2SiO4:Eu3+, Dy3+ phosphors have been prepared through the sol-gel process. X-ray diffraction (XRD), thermogravimetric and ddifferential thermal analysis (TG-DTA), FT-IR spectra and photoluminescence spectra were used to characterize the resulting phosphors. The results of XRD indicated that the phosphors crystallized completely at 1000oC. In Zn2SiO4:Eu3+,Dy3+ phosphors, the Eu3+ and Dy3+ show their characteristic red(613nm, 5D0-7F2), blue (481nm, 4F9/2–6H15/2) and yellow (577nm, 4F9/2–6H13/2) emissions.


1987 ◽  
Vol 113 ◽  
Author(s):  
Scott Schlorholtz ◽  
Ken Bergeson ◽  
Turgut Demirel

ABSTRACTThe physical and chemical properties of fly ash produced at Ottumwa Generating Station have been monitored since April, 1985. The fly ash is produced from burning a low sulfur, sub-bituminous coal obtained from the Powder River Basin near Gillette, Wyoming. One-hundred and sixty samples of fly ash were obtained during the two year period. All of the samples were subjected to physical testing as specified by ASTM C 311. About one-hundred of the samples were also subjected to a series of tests designed to monitor the self-cementing properties of the fly ash. Many of the fly ash samples were subjected to x-ray diffraction and fluorescence analysis to define the mineralogical and chemical composition of the bulk fly ash as a function of sampling date. Hydration products in selected hardened fly ash pastes, were studied by x-ray diffraction and scanning electron microscopy. The studies indicated that power plant operating conditions influenced the compressive strength of the fly ash paste specimens. Mineralogical and morphological studies of the fly ash pastes indicated that stratlingite formation occurred in the highstrength specimens, while ettringite was the major hydration product evident in the low-strength specimens.


2013 ◽  
Vol 832 ◽  
pp. 589-595 ◽  
Author(s):  
N.A. Edama ◽  
A. Sulaiman ◽  
K.H. Ku Hamid ◽  
M.N. Muhd Rodhi ◽  
Mohibah Musa ◽  
...  

This study analyzed the effects of sulphuric acid (H2SO4) treatment on pysico-chemical properties and morphological changes of clay obtained from Sg. Sayong, Perak. The clay was ground and sieved to <150μm and treated with different concentrations of H2SO4. The treatment was completed by refluxing the clay with different concentration of H2SO4 (1M, 5M and 10M ) at 100 °C for 4 hours and followed by calcination at 500 °C for 1 hour. The physic-chemical properties and morphological changes of the untreated and treated clay were compared using Surface Area Analyser, X-Ray Diffraction (XRD), Field Emission Scanning Electron Micrograph (FESEM), X-Ray Diffraction (XRD) and Fourier Transformed Infrared Spectroscopy (FTIR). The results showed that acid treatment of 5M increased the surface area from 25 m2/g to 75 m2/g and the pore volume increased from 0.1518 cc/g to 0.3546 cc/g. The nanopore size of the clay decreased from 24.8 nm to 19.4 nm after treated with acid. This can be explained due to the elimination of the exchangeable cations and generation of microporosity. The results of XRF showed SiO2 increased from 58.34% to 74.52% and Al2O3 reduced from 34.6% to 18.31%. The mineral oxides such as Fe2O3, MgO, CaO, K2O and TiO2 also reduced. This concluded that H2SO4 treatment has led to significant removal of octahedral Al3+, Fe3+ cations and other impurities. In conclusion, this study showed the physico-chemical properties and morphology of Sayong clay were improved once treated with H2SO4 and therefore suggests better supporting material for enzyme immobilization.


2003 ◽  
Vol 802 ◽  
Author(s):  
R. G. Haire ◽  
S. Heathman ◽  
T. Le Bihan ◽  
A. Lindbaum ◽  
M. Iridi

ABSTRACTOne effect of pressure on elements and compounds is to decease their interatomic distances, which can bring about dramatic perturbations in their electronic nature and bonding, which can be reflected in changes in physical and/or chemical properties. One important issue in the actinide series of elements is the effect of pressure on the 5f-electrons. We have probed changes in electronic behavior with pressure by monitoring structure by X-ray diffraction, and have studied several actinide metals and compounds from thorium through einsteinium. These studies have employed angle dispersive diffraction using synchrotron radiation, and energy dispersive techniques via conventional X-ray sources. The 5f-electrons of actinide metals and their alloys are often affected significantly by pressure, while with compounds, the structural changes are often not linked to the involvement of 5 f-electron. We shall present some of our more recent findings from studies of selected actinide metals, alloys and compounds under pressure. A discussion of the results in terms of the changes in electronic configurations and bonding with regard to the element's position in the series is also addressed.


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