scholarly journals Phase formation in the Ag2MoO4–Rb2MoO4–Hf(MoO4)2 system

2021 ◽  
Vol 23 (4) ◽  
pp. 594-599
Author(s):  
Yunna L. Tushinova ◽  
Bair G. Bazarov ◽  
Evgeniy V. Kovtunets ◽  
Jibzema G. Bazarova
Keyword(s):  
Solid Phase ◽  
Thermal Characteristics ◽  
Ternary Systems ◽  
Phase Interaction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Cell Parameters ◽  
Ternary Molybdates ◽  
Ternary Molybdate ◽  
First Time

Systematic studies of the subsolidus structure of ternary molybdate systems allow expanding the representation of ternary molybdates. In this paper we studied the solid phase interaction in the Ag2MoO4–Rb2MoO4–Hf(MoO4)2 system for the first time using X-ray phase analysis.To determine the quasi-binary sections, we use the method of “intersecting cuts”. It helped to reveal the formation of new Rb5Ag1/3Hf5/3(MoO4)6 and Rb3AgHf2(MoO4)6 phases. We also determined their thermal characteristics using differential scanning calorimetry. The ternary molybdate Rb5Ag1/3Hf5/3(MoO4)6 crystallised in the trigonal syngony with the followingunit cell parameters: a = 10.7117(1), c = 38.5464(5) Å (space group R3с, Z = 6). The Ag2MoO4–Rb2MoO4–Hf(MoO4)2 system is characterised by the existence of ten quasi-binary cross sections.The experimental data obtained in this work complement the information on phase equilibria in condensed ternary systems containing molybdates of tetravalent elements and two different monovalent elements. This provides opportunities for the combination of the compositions of ternary molybdates due to cationic substitutions, which will allow controlling their properties.

Preparation and Characterization of Ni2+-Montmorillonite/Polyvinyl Alcohol Water-Soluble Nanocomposite Film

2005 ◽  
Vol 13 (8) ◽  
pp. 839-846 ◽  
Author(s):  
Li-Ping Wang ◽  
Yun-Pu Wang ◽  
Fa-Ai Zhang
Keyword(s):  
Polyvinyl Alcohol ◽  
Photoelectron Spectroscopy ◽  
Thermal Characteristics ◽  
Water Soluble ◽  
Scanning Calorimetry ◽  
Xps Spectra ◽  
X Ray ◽  
Alcohol Water ◽  
Ft Ir ◽  
Silicate Layers

A new type of nano-composite film was prepared from polyvinyl alcohol, Ni2+-montmorillonite (Ni2+-MMT), defoamer, a levelling agent and a plasticizer. Its thermal characteristics were studied by Differential Scanning Calorimetry (DSC). The intermolecular interactions were measured by Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS), and the tensile strength (TS) and elongation at break (%E) were measured. The microstructures were studied by X-ray diffraction (XRD) and atomic force microscopy (AFM). FT-IR and XPS spectra indicated that cross-linking has taken place between PVA and Ni2+-MMT. XRD and AFM indicate that the PVA molecules had inserted themselves into the silicate layers of MMT, exfoliating them and dispersing them randomly into the PVA matrix. Compared to pure PVA film, the TS of the films was increased and %E decreased when the Ni2+-Montmorillonite was added and the dissolution temperature of the film was also reduced.

Synthesis and properties of double gadolinium tellurites

2021 ◽  
Vol 103 (3) ◽  
pp. 67-73
Author(s):  
A.A. Toibek ◽  
◽  
K.T. Rustembekov ◽  
D.A. Kaikenov ◽  
M. Stoev ◽  
...  
Keyword(s):  
Phase Analysis ◽  
Solid Phase ◽  
Heat Capacities ◽  
Ceramic Technology ◽  
Phase Method ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Temperature Range ◽  
Diffraction Patterns

For the first time, double gadolinium tellurites of the composition GdMIITeO4.5 (MII — Sr, Ba) were synthesized by the solid-phase method. The solid-phase synthesis of samples was carried out from decrepitated gadolinium (III) and tellurium (IV) oxides, strontium, and barium carbonates according to the standard ceramic technology. The synthesis was carried out in the temperature range of 800-1100 °C. The samples obtained were confirmed by X-ray phase analysis. X-ray phase analysis was carried out on an Empyrean instrument in the XRDML Pananalitical format. The intensity of the diffraction maxima was estimated on a 100-point scale. X-ray diffraction patterns indexing of the powder of gadolinium tellurites — alkaline earth metals studied were carried out by the homology method. The reliability and correctness of the results of indexing the X-ray diffraction patterns are confirmed by the good agreement between the experimental and calculated values of the interplanar distances (d) and the agreement between the values of the X-ray and pycnometric densities. It was found that compounds GdSrTeO4.5 and GdBaTeO4.5 crystallize in the monoclinic system and have the unit cell parameters, namely GdSrTeO4.5 — a = 12.7610, b = 10.4289, c = 8.6235 Å, V° = 1141.83 Å3, β = 95.77°, Z = 5, ρrent. = 3.22, ρpikn. = (3.10±0.09) g/cm3; GdBaTeO4.5 — a = 15.7272, b = 15.8351, c = 7.1393 Å, V° = 1769.72 Å3, β = 95.53°, Z = 8, ρrent = 3.71, ρpick = (3.61±0.10) g/cm3. Using the Landiya method, the standard heat capacities of the compounds were estimated from the calculated values of the standard entropies, and the temperature dependences of the heat capacities of the gadolinium tellurites synthesized were determined in the temperature range of 298–850 K.

scholarly journals Physical Stability and Viscoelastic Properties of Co-Amorphous Ezetimibe/Simvastatin System

2019 ◽  
Vol 12 (1) ◽  
pp. 40 ◽  
Author(s):  
Justyna Knapik-Kowalczuk ◽  
Krzysztof Chmiel ◽  
Karolina Jurkiewicz ◽  
Natália Correia ◽  
Wiesław Sawicki ◽  
...  
Keyword(s):  
Elevated Temperature ◽  
Viscoelastic Properties ◽  
Room Temperature ◽  
Physical Stability ◽  
Ternary Systems ◽  
Storage Conditions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Temperature Conditions ◽  
First Time

The purpose of this paper is to examine the physical stability as well as viscoelastic properties of the binary amorphous ezetimibe–simvastatin system. According to our knowledge, this is the first time that such an amorphous composition is prepared and investigated. The tendency toward re-crystallization of the amorphous ezetimibe–simvastatin system, at both standard storage and elevated temperature conditions, have been studied by means of X-ray diffraction (XRD). Our investigations have revealed that simvastatin remarkably improves the physical stability of ezetimibe, despite the fact that it works as a plasticizer. Pure amorphous ezetimibe, when stored at room temperature, begins to re-crystallize after 14 days after amorphization. On the other hand, the ezetimibe-simvastatin binary mixture (at the same storage conditions) is physically stable for at least 1 year. However, the devitrification of the binary amorphous composition was observed at elevated temperature conditions (T = 373 K). Therefore, we used a third compound to hinder the re-crystallization. Finally, both the physical stability as well as viscoelastic properties of the ternary systems containing different concentrations of the latter component have been thoroughly investigated.

scholarly journals Synthesis and Crystal Structure of the Bioinorganic Complex [Sb(Hedta)]·2H2O

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Di Li ◽  
Guo-Qing Zhong
Keyword(s):  
Crystal Structure ◽  
Ethylenediaminetetraacetic Acid ◽  
Raw Materials ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Cell Parameters ◽  
Composition And Structure ◽  
Decomposition Processes ◽  
Distorted Trigonal Bipyramid

The antimony(III) complex [Sb(Hedta)]·2H2O was synthesized with ethylenediaminetetraacetic acid (H4edta) and antimonous oxide as main raw materials in aqueous solution. The composition and structure of the complex were characterized by elemental analysis, infrared spectra, single crystal X-ray diffraction, X-ray powder diffraction, thermogravimetry, and differential scanning calorimetry. The crystal structure of the antimony(III) complex belongs to orthorhombic system, space group Pna2(1), with cell parameters ofa=18.4823(18) Å,b=10.9408(12) Å,c=7.3671(5) Å,V=1489.7(2) Å3,Z=4, andDc=1.993 g cm−3. The Sb(III) ion is five-coordinated by two amido N atoms and three carboxyl O atoms from a single Hedta3−ligand, forming a distorted trigonal bipyramid geometry. The thermal decomposition processes of the complex include dehydration, oxidation, and pyrolysis of the ligand, and the last residue is Sb2O3at the temperature of 570°C.

Purification, characterization, gene cloning and preliminary X-ray data of the exo-inulinase from Aspergillus awamori

2002 ◽  
Vol 362 (1) ◽  
pp. 131-135 ◽  
Author(s):  
Michael ARAND ◽  
Alexander M. GOLUBEV ◽  
J. R. Brandao NETO ◽  
Igor POLIKARPOV ◽  
R. WATTIEZ ◽  
...  
Keyword(s):  
Amino Acid ◽  
Amino Acid Sequence ◽  
Solid Phase ◽  
Aspergillus Awamori ◽  
Glycoside Hydrolase Family ◽  
Orthorhombic Space Group ◽  
Ph Optimum ◽  
X Ray ◽  
Cell Parameters ◽  
Hydrolysis Of

Extracellular exo-inulinase has been isolated from a solid-phase culture of the filamentous fungus Aspergillus awamori var. 2250. The apparent molecular mass of the monomer enzyme was 69±1kDa, with a pI of 4.4 and a pH optimum of 4.5. The enzyme hydrolysed the β-(2 → 1)-fructan (inulin) and β-(2 → 6)-fructan (levan) via exo-cleavage, releasing fructose. The values for the Michaelis constants Km and Vmax in the hydrolysis of inulin were 0.003±0.0001mM and 175±5μmol·min−1·mg−1. The same parameters in the hydrolysis of levan were 2.08±0.04mg/ml and 1.2±0.02μmol/min per mg, respectively. The gene and cDNA encoding the A. awamori exo-inulinase were cloned and sequenced. The amino acid sequence indicated that the protein belongs to glycoside hydrolase family 32. A surprisingly high similarity was found to fructosyltransferase from Aspergillus foetidus (90.7% on the level of the amino acid sequence), despite the fact that the latter enzyme is unable to hydrolyse inulin and levan. Crystals of the native exo-inulinase were obtained and found to belong to the orthorhombic space group P212121 with cell parameters a = 64.726 Å (1Å = 0.1 nm), b = 82.041 Å and c = 136.075 Å. Crystals diffracted beyond 1.54 Å, and useful X-ray data were collected to a resolution of 1.73 Å.

Study of the structure and thermal characteristics of nanocomposites based on polyvinyl alcohol and intercalated montmorillonite

2019 ◽  
pp. 089270571987919
Author(s):  
Volodymyr Krasinskyi ◽  
Ivan Gajdos ◽  
Oleh Suberlyak ◽  
Viktoria Antoniuk ◽  
Tomasz Jachowicz
Keyword(s):  
Thermal Stability ◽  
Differential Scanning Calorimetry ◽  
Acrylic Acid ◽  
Polyvinyl Alcohol ◽  
Thermal Characteristics ◽  
Degree Of Crystallinity ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
The Degree Of Crystallinity

The structure and thermal characteristics of nanocomposites based on polyvinyl alcohol (PVA) and montmorillonite (MMT) intercalated with polyvinylpyrrolidone were investigated by X-ray diffraction analysis and differential scanning calorimetry. The modification of PVA with intercalated MMT reduces the degree of crystallinity of the resulting nanocomposites but significantly increases their thermal stability. Under ultrasound, the intercalated MMT was completely distributed in a PVA solution and formed a monocrystalline structure. Films based on PVA with modified MMT were cross-linked at 110°C in the presence of 5 wt% acrylic acid and 0.5 wt% Ferrous(II) sulfate as an initiator. The formed films have a homogeneous cross-linked structure.

Manufacture of Ternary Solid Dispersions Composed of Nifedipine, Eudragit® E and Adsorbent

2011 ◽  
Vol 317-319 ◽  
pp. 185-188 ◽  
Author(s):  
Pornsak Sriamornsak ◽  
Srisuda Kontong ◽  
Yotsanan Weerapol ◽  
Jurairat Nunthanid ◽  
Srisagul Sungthongjeen ◽  
...  
Keyword(s):  
Dissolution Rate ◽  
Solid Dispersions ◽  
Ternary Systems ◽  
Dissolution Enhancement ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Ternary Solid Dispersions ◽  
Diffraction Patterns ◽  
Physical Mixtures

The aim of this study was to manufacture the ternary solid dispersions composed of nifedipine, Eudragit® E and adsorbent. Dissolution enhancement of nifedipine was also investigated. The inert solid carriers were added in the mixtures of nifedipine and Eudragit® E at varying ratios. The physicochemical properties of ternary systems, compared to physical mixtures, were analyzed using powder x-ray diffraction (PXRD) and differential scanning calorimetry (DSC). The dissolution of nifedipine from ternary systems was compared to the drug alone. The influence of drug:polymer: adsorbent ratio and type of adsorbent on the dissolution rate of the drug was also evaluated. The PXRD and DSC results of the systems with high amount of polymer showed that the drug was present in an amorphous form. On the other hand, the diffraction patterns and DSC thermograms of the physical mixtures revealed that to some extent the drug was present in a crystalline form. The results from this study demonstrated that an improvement in dissolution rate of nifedipine with Eudragit® E and adsorbents was obtained.

Preparation of γ–Fe2O3 nanoparticles from a nonaqueous precursor

2001 ◽  
Vol 16 (12) ◽  
pp. 3471-3475 ◽  
Author(s):  
P. Deb ◽  
A. Basumallick
Keyword(s):  
Heat Treatment ◽  
Thermal Characteristics ◽  
Homogeneous Solution ◽  
Nanosized Particles ◽  
Narrow Size Distribution ◽  
Fe2o3 Nanoparticles ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
X Ray Scattering

Nanosized particles of γ–Fe2O3 were prepared by heat treatment of the precipitates, obtained from a homogeneous solution of stearic acid and hydrated iron(III) nitrate. The compositional and thermal characteristics of the precipitates were studied with the aid of infrared spectroscopy and differential scanning calorimetry. The x-ray diffraction and small-angle x-ray scattering investigation shows that γ–Fe2O3 nanoparticles with narrow size distribution can be prepared successfully by this route.

scholarly journals Synthesis and X-ray analysis of complex ferrite YbBiNaFe2O6,5

2017 ◽  
pp. 14-17
Author(s):  
Muhkametkali Mataev ◽  
Moldir Abdraimova ◽  
A. Atabay
Keyword(s):  
Crystal Lattice ◽  
Solid Phase ◽  
Oxide Phase ◽  
Fluorite Structure ◽  
Solid Phase Reaction ◽  
Phase Reaction ◽  
X Ray Diffraction ◽  
X Ray ◽  
Cell Parameters ◽  
Mixed Ferrite

The complex oxide phase of the composition YbBiNaFe2O6,5 was synthesized by the high-temperature solid-phase reaction. X-ray diffraction analysis was used to study the structure for the first time; the type of syngony, unit cell parameters, X-ray diffraction and pycnometric densities were determined. X-ray diffraction was carried out by homology method from the initial fluorite structure δBi2O3. The method of least squares refined the parameters of the crystal lattice. The parameters of the orthorhombic lattice of complex mixed ferrite at the value of the number of formula units Z=4 are: a=5.2319, в=5.2186, с=7.5702 Å. The correctness of the results of the X-ray diffraction of complex mixed ferrite was confirmed by the good agreement between the experimental and calculated values of the inverse squares of the interplanar distances (104/d2). Satisfactory consistency of the values of the X-ray and pycnometric densities, ρrad = 8.335, ρpik = 8.328 g/cm3, proves the correctness of the results of the experiment. A comparative analysis of the interrelation between the parameters of the crystal lattice and the parameters of the crystal lattices of the initial oxide δBi2O3. The analysis shows the values of the parameters “a” and “c” are in satisfactory agreement with the parameters of the crystal lattice δBi2O3, the parameter “c” is distorted from the value of the parameter “a” on √2.

scholarly journals Структура и термодинамические свойства SmGaGe-=SUB=-2-=/SUB=-O-=SUB=-7-=/SUB=-

2020 ◽  
Vol 62 (2) ◽  
pp. 332
Author(s):  
Л.Т. Денисова ◽  
М.С. Молокеев ◽  
Л.А. Иртюго ◽  
В.В. Белецкий ◽  
Н.В. Белоусова ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Heat Capacity ◽  
Solid Phase Synthesis ◽  
Solid Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Phase Synthesis ◽  
High Temperature Heat Capacity ◽  
X Ray ◽  
Temperature Heat

SmGaGe2O7 has been prepared by solid-phase synthesis in air at temperatures from 1273 to 1473 K using the Sm2O3, Ga2O3, and GeO2 oxides as starting materials. The structure of the studied germanate was determined by X-ray diffraction (space group P2_1 / c; a = 7.18610(9) Angstrem, b = 6.57935(8) Angstrem, c = 12.7932(2) Angstrem). Its high-temperature heat capacity has been measured by differential scanning calorimetry. The obtained experimental dependence C_p = f (T) has been used to evaluate the thermodynamic properties of the compound.

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