scholarly journals SYNTHESIS AND PHYSICOCHEMICAL STUDY OF THE CERIUM AND CEFAZOLIN METAL COMPLEX

2021 ◽  
pp. 881-889
Author(s):  
Тимофей Владимирович Крюков ◽  
Мариана Александровна Феофанова ◽  
Михаил Игоревич Скобин ◽  
Александра Ивановна Иванова
Keyword(s):  
Ir Spectroscopy ◽  
Metal Complex ◽  
Electron Probe ◽  
Thermal Characteristics ◽  
Cerium Chloride ◽  
Scanning Calorimetry ◽  
Electron Probe Analysis ◽  
X Ray ◽  
Inner Sphere ◽  
Solid Form

В данной работе коллективом авторов путём взаимодействия водных растворов хлорида трёхвалентного церия и натриевой соли цефазолина получено и выделено в твердом виде металлокомплексное соединение. Его элементный состав установлен с помощью метода рентгеноспектрального электронно-зондового анализа, описаны термические характеристики данного соединения, температура его разложения, состав и способ координации внутренней сферы данного металлокомплекса был уточнен методами термогравиметрии, и дифференциальной сканирующей калориметрии и методом ИК-спектроскопии. На основании полученных данных установлено, что внутренняя сфера металллокомплекса содержит в своем составе три молекулы цефазолина и три молекулы внутрисферной воды. Состав внутренней сферы отвечает брутто-формуле [CeCzl(HO) ]. На основании данных ИК- спектроскопии сделаны выводы о координации цефазолина к центральному иону через амидную и карбоксильную группы. In this work, a team of authors obtained and isolated in solid form a metal complex compound by the interaction of aqueous solutions of trivalent cerium chloride and sodium salt of cefazolin. Its elemental composition was determined using the X-ray spectral electron probe analysis. The thermal characteristics of this compound, the temperature of its decomposition, the composition and the method of coordination of the inner sphere of this metal complex were clarified by the methods of thermogravimetry, differential scanning calorimetry and IR spectroscopy. Based on the data obtained, the inner sphere of the metal complex contains three molecules of cefazolin and three molecules of inner-sphere water. The composition of the inner sphere corresponds to the formula [CeCzl(HO) ]. Taking into account IR spectroscopy data, the authors concluded that the most likely way of coordination of cefazolin to the central ion is through the amide and carboxyl groups.

A Study of the Interactions Between Oligoamidephosphate (OAPh) and Curatives in a Sulphenamide-Accelerated Sulphur Vulcanizing System

1999 ◽  
Vol 19 (2) ◽  
pp. 95-108 ◽  
Author(s):  
Todorka G. Vladkova ◽  
Alexander Chr. Alaminov ◽  
Milka G. Pankova
Keyword(s):  
Differential Scanning Calorimetry ◽  
Zinc Oxide ◽  
Ir Spectroscopy ◽  
Room Temperature ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Sulphur Vulcanization

Abstract The possible interactions between oligoamidephosphate (OAPli) and the curatives of a sulphenamide-accelerated sulphur vulcanizing system were studied by differential scanning calorimetry, IR-spectroscopy, and X-ray analysis. The interactions in double mixtures were between OAPh and zinc oxide (ZnO) and OAPh and sulphur. The OAPh/ZnO interaction that starts at room temperature seems to be the key for understanding the peculiarities of sulphenamide-accelerated sulphur vulcanization in the presence of OAPh.

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.

scholarly journals Formation of Pharmaceutical Salts and Cocrystals via Vapour-Assisted Tumbling (VAT) – A Solvent Efficient Process with Potential Industrial Applications

2021 ◽  
Author(s):  
Alexander J. Stirk ◽  
Fabio E. S. Souza ◽  
Jenny Gerster ◽  
Fatemeh M. Mir ◽  
Avedis Karadeolian ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Environmental Impact ◽  
Industrial Applications ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
New Techniques ◽  
X Ray ◽  
Industry Standard ◽  
Pharmaceutical Salts ◽  
Solid Form

Crystallisations on both the academic and industrial scale often use large volumes of solvent. In order decrease the environmental impact of such processes, new techniques must be discovered that increase the efficiency of the solvents used. Introduced here is a process that combines repurposed industry standard hardware and aspects of mechanochemistry to produce a technique we call “Vapour Assisted Tumbling” (VAT). Pharmaceutical and well-known cocrystals and salts were formed by tumbling the coformers in an atmosphere of vaporised solvent, in this study, methanol (MeOH). This was done inside a custom built analogue of an industrial rotary cone dryer (RCD). It was found that a desired solid form could be obtained as monitored by powder X-ray diffraction and differential scanning calorimetry. By repurposing industrial RCDs, it is feasible that solid forms can be crystallised with both minimal and reusable/recyclable solvent – drastically lowering the environmental impact of such transformations.

A note on the occurrence of chevkinite, allanite, and zirkelite on St. Kilda, Scotland

1982 ◽  
Vol 46 (341) ◽  
pp. 445-448 ◽  
Author(s):  
R. R. Harding ◽  
R. J. Merriman ◽  
P. H. A. Nancarrow
Keyword(s):  
Rare Earth ◽  
Great Britain ◽  
Electron Probe ◽  
Energy Dispersive ◽  
X Ray Diffraction ◽  
Electron Probe Analysis ◽  
Accessory Minerals ◽  
X Ray ◽  
Probe Analysis ◽  
Recorded Occurrence

AbstractThe occurrence of three accessory minerals with significant rare earth contents in Tertiary acid rocks of St. Kilda is described. Allanite, zirkelite, and chevkinite were identified by electron probe analysis (with energy-dispersive attachment) and the chevkinite confirmed by X-ray diffraction. Brief comparison is made with other Tertiary occurrences of RE minerals. This is the first recorded occurrence of chevkinite in Great Britain.

scholarly journals COMPARISON STUDY OF GRINDING AND SLURRY METHOD ON PHYSICOCHEMICAL CHARACTERISTIC OF ACYCLOVIR – SUCCINIC ACID COCRYSTAL

2017 ◽  
Vol 10 (3) ◽  
pp. 153
Author(s):  
Fauzi Rahman ◽  
Agnes Nuniek Winantari ◽  
Dwi Setyawan ◽  
Siswandono .
Keyword(s):  
Fourier Transform ◽  
Ir Spectroscopy ◽  
Succinic Acid ◽  
Physicochemical Characteristic ◽  
Fourier Transform Infrared ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Slurry Method ◽  
Dissolution Efficiency

ABSTRACTObjective: This study aimed to compare the characteristics of acyclovir (ACV)-succinic acid (SA) cocrystal with grinding and slurry method.Methods: Cocrystals were prepared using grinding and slurry methods. Physicochemical characterizations were performed using powder X-raydiffraction (PXRD), differential scanning calorimetry, Fourier transform infrared (IR) spectroscopy, scanning electron microscope (SEM), anddissolution test.Results: The study revealed that cocrystal of ACV-SA showed a decrease in the melting temperature, i.e., 175.10°C, respectively, in comparison with themelting point of the constituent materials (ACV 253.53°C and SA 187.29°C). PXRD diffractogram showed that cocrystal with grinding method exhibitednew diffraction peaks at angle 2θ=8.92°, 16.24°, and 17.14°, while PXRD diffractogram of cocrystal with slurry method exhibit new diffraction peaksat angle 2θ=16.25°, and 19.63°. Characterization with IR spectroscopy showed the disappearance of transmission peaks at 3441cm disappearance ofC=O stretch at 1584cm and 1612cm. Dissolution efficiency of each treatment group calculated the efficiency of dissolution in 15th minutes, grindingmethod cocrystal with grinding time 15 minutes give the dissolution efficiency were 54.23%. Slurry method cocrystal with solvent concentration12 ml/g gives the high value of the dissolution efficiency is 74.36%. SEM micrographs showed that cocrystals prepared by solvent evaporation methodhave differences crystal form at magnification 5000× magnification compared to pure ACV and physical mixture.Conclusion: The study concluded that cocrystals of ACV-SA were successfully formed using grinding and slurry methods. The formed cocrystalsof ACV-SA exhibited different physicochemical characteristics as compared to the constituent materials. The formed cocrystals prepared by slurrymethod have a high intensity of diffraction peak on X-ray diffraction and highest dissolution efficiency at 15 minutes rather than grinding methodcocrystal.Keywords: Cocrystal, Acyclovir, Succinic acid, Grinding, Slurry, Powder X-ray diffraction, Fourier transform infrared, Dissolution rate. 

scholarly journals ELECTRON PROBE ANALYSIS OF THE CALCIUM DISTRIBUTION IN CELLS OF THE EMBRYONIC CHICK CHORIOALLANTOIC MEMBRANE I. A CRITICAL EVALUATION OF TECHNIQUES

1972 ◽  
Vol 20 (6) ◽  
pp. 401-413 ◽  
Author(s):  
JAMES R. COLEMAN ◽  
A. RAYMOND TEREPKA
Keyword(s):  
Electron Probe ◽  
Critical Evaluation ◽  
Chorioallantoic Membrane ◽  
Embryonic Chick ◽  
Total Calcium ◽  
Electron Probe Analysis ◽  
X Ray ◽  
Chick Chorioallantoic Membrane ◽  
Minor Losses

The chorioallantoic membrane of the developing chick embryo is an epithelium that actively transports calcium. The methodology utilized to prepare this soft tissue for calcium localization with the electron probe x-ray microanalyzer is presented in detail. The preparative procedures are evaluated according to general histochemical principles and in relationship specifically to electron probe investigations. It is shown that the method employed in these studies preserves the normal fine structure of the tissue, prevents selective loss of calcium, permits only minor losses of total calcium and appears to maintain the distribution of calcium that existed in vivo. Examples are presented of artifacts that can be induced during tissue sectioning and mounting procedures. Problems of defining electron probe resolution in biologic specimens are discussed, and the critical importance of evaluating x-ray images in association with simultaneously generated sample current images is emphasized.

Electron Probe Microanalysis of Zinc-Bearing Hexagonal Ferrites

1965 ◽  
Vol 9 ◽  
pp. 304-313
Author(s):  
J. R. Shappirio
Keyword(s):  
Electron Probe ◽  
Hexagonal Ferrites ◽  
Structural Units ◽  
Electron Probe Analysis ◽  
X Ray ◽  
Layer Structures ◽  
Cell Data ◽  
Unit Cell Data ◽  
The Ideal

AbstractThe electron probe is shown to be an effective tool for the analysis of the series of ferrimagnetic oxides referred to as the hexagonal ferrites. This series of compounds) containing barium, Fe3+, and a divalent metal cation, is formed by an ordered stacking of basic structural units in varying ratios. The ideal, complex stoichiornewy of these polytype-like mixed-layer structures can be computed from X-ray unit cell data; the various structures and their predicted stoichiometry are reviewed. Results of electron probe analysis of zinc-bearing single-crystal hexagonal ferrites are compared with theoretical values, the various correction procedures applied to the probe data are presented, and the limitations of the method in the analysis of hexagonal ferrites are discussed. The information obtained from this study has laid the groundwork for the determination of chemistry in substituted members of the hexagonal ferrite group, and will contribute significantly to the interpretation of the magnetic properties exhibited by these compounds.

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.

Cosmochlore—a new examination

1981 ◽  
Vol 44 (335) ◽  
pp. 265-267 ◽  
Author(s):  
A. G. Couper ◽  
M. H. Hey ◽  
R. Hutchison
Keyword(s):  
Electron Probe ◽  
Optical Data ◽  
Electron Probe Analysis ◽  
X Ray ◽  
Probe Analysis

AbstractExamination of cotype cosmochlore from the Toluca meteorite confirms Laspeyres's observations (1897) in every respect, except that what he determined as iron was largely titanium. His data are completed by an electron-probe analysis and by full optical and X-ray data. Accepting the identity of cosmochlore and ureyite, the optical data of Frondel and Klein (1965) for the latter are partly in error or misprinted.

scholarly journals Untersuchungen am System Vanadium—Gallium

1966 ◽  
Vol 21 (5) ◽  
pp. 531-540 ◽  
Author(s):  
R. G. Maier ◽  
Y. Uzel ◽  
H. Kandler
Keyword(s):  
Crystal Structure ◽  
Phase Diagram ◽  
Electron Probe ◽  
Liquidus Curve ◽  
X Ray Diffraction ◽  
Equilibrium Conditions ◽  
Electron Probe Analysis ◽  
X Ray ◽  
Oxygen System ◽  
Annealing Experiments

The phase diagram of the vanadium-gallium system was investigated by means of thermoanalysis, microscopy, x-ray diffraction, and electron probe analysis.The liquidus curve was measured in the range from 40—80% Gallium. The existence of the known phases V3Ga (Cr3Si-typ), V6Ga5 (Ti6Sn5-typ), V6Ga7 (Cu5Zn8-typ), V2Ga5 (Mn2Hg5-typ), V4GaO and V5Ga3Ox (Mn5Si3-typ) was reestablished. The existence of V3GaOx and V5 (Ga, Si)3Ox is stated and their crystal structure investigated.It is shown that the oxygen content of he samples greatly influences the equilibrium conditions of the system. By means of annealing experiments and dilatometric measurements the phase diagram of the vanadium-gallium-oxygen system was investigated in the range of small oxygen contents.

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