Reactions in Molten Alkalimetal Polychalcogenides: What Happens in the Melt? A Study of the Reactions in the System K—Nb—S Using Differential Scanning Calorimetry, Infrared Spectroscopy, and X-Ray Powder Diffraction.

ChemInform ◽  
2003 ◽  
Vol 34 (14) ◽  
Author(s):  
Peter Duerichen ◽  
Wolfgang Bensch
CrystEngComm ◽  
2019 ◽  
Vol 21 (29) ◽  
pp. 4319-4328 ◽  
Author(s):  
Mariani A. Ciciliati ◽  
M. Ermelinda S. Eusébio ◽  
Manuela Ramos Silva ◽  
Éder T. G. Cavalheiro ◽  
Ricardo A. E. Castro

A new polymorph of metoprolol base, form II, was identified and characterized by differential scanning calorimetry, X-ray powder diffraction and infrared spectroscopy. A new salt of metoprolol and nicotinic acid was also obtained and characterized.


2002 ◽  
Vol 57 (12) ◽  
pp. 1382-1386 ◽  
Author(s):  
Peter Dürichen ◽  
Wolfgang Bensch

The reactions of potassium polysulfides with elemental Nb were investigated with different analytical techniques. The amount of the polysulfide applied has no influence onto product formation, i. e. the ratio K2Sx: Nb is not important. The length of the polsysulfide chain, i. e. the value of x in K2Sx determines what product is formed. In sulfur-poor melts, K3NbS4 is observed. Increasing x to 5 - 6, K4Nb2S11 is formed with a structure containing S22− anions. Finally, applying a melt with x > 6, K6Nb4S25 is found as the product with a crystal structure containing the S52− polysulfide anion. When K2Sx (x < 5) is heated with sulfur in the first step the pentasulfide K2S5 is formed. Immediately after melting of K2S5 a reaction with elemental Nb occurs. The results of FT-IR and X-ray investigations have demonstrated that after oxidation the anion [Nb2S11]4− is formed relatively fast, and after a short time crystalline K4Nb2S11 can be detected. After 24 h the reaction is complete.


INDIAN DRUGS ◽  
2013 ◽  
Vol 50 (10) ◽  
pp. 53-61
Author(s):  
B. V. Dhokchawle ◽  
◽  
A. B. Bhandari

In the present study, amorphous form of cefuroxime axetil was prepared and characterized by various methods. The result showed that the amorphous form of cefuroxime axetil with hydrophilic carriers was successfully obtained by freeze drying. The amorphous form showed a substantially higher dissolution rate and saturation solubility than cefuroxime axetil and physical mixture. The molecular behaviour of the drug in all samples were characterized by X-ray powder diffraction, Fourier transformed infrared spectroscopy, scanning electron microscopy and differential scanning calorimetry. The dissolution and saturation solubility studies of the samples were performed. The X-ray powder diffraction, Fourier transformed infrared spectroscopy and differential scanning calorimetry provided useful information to support the amorphousness of the samples.


1998 ◽  
Vol 76 (11) ◽  
pp. 1520-1523
Author(s):  
Jennifer F Caplan ◽  
Christopher A Murphy ◽  
Susan Swansburg ◽  
Robert P Lemieux ◽  
T Stanley Cameron ◽  
...  

The synthesis of Ru2(μ-O2CR)4(μ´-O2CR) (1), R = -CH2(CH2)6CH=CH(CH2)5CH3, has been achieved and characterization using elemental analysis and FTIR and UV-Vis spectroscopies undertaken. Strong evidence for a hexagonal discotic mesophase has been found using differential scanning calorimetry, variable-temperature polarizing optical microscopy, and X-ray powder diffraction. A solid to liquid crystal transition was found upon heating at 128°C and the mesophase is found to persist to room temperature upon cooling from 150°C. This is the first report of room temperature mesomorphism in a mixed-valent metallomesogen. Key words: ruthenium carboxylate, liquid crystal, metallomesogen, mixed valence, polymer.


Molecules ◽  
2020 ◽  
Vol 25 (8) ◽  
pp. 1910
Author(s):  
U. B. Rao Khandavilli ◽  
Leila Keshavarz ◽  
Eliška Skořepová ◽  
René R. E. Steendam ◽  
Patrick J. Frawley

The presence of impurities can drastically affect the efficacy and safety of pharmaceutical entities. p-Aminophenol (PAP) is one of the main impurities of paracetamol (PA) that can potentially show toxic effects such as maternal toxicity and nephrotoxicity. The removal of PAP from PA is challenging and difficult to achieve through regular crystallization approaches. In this regard, we report four new salts of PAP with salicylic acid (SA), oxalic acid (OX), l-tartaric acid (TA), and (1S)-(+)-10-camphorsulfonic acid (CSA). All the PAP salts were analyzed using single-crystal X-ray diffraction, powder X-ray diffraction, infrared spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. The presence of minute amounts of PAP in paracetamol solids gives a dark color to the product that was difficult to remove through crystallization. In our study, we found that the addition of small quantities of the aforementioned acids helps to remove PAP from PA during the filtration and washings. This shows that salt formation could be used to efficiently remove challenging impurities.


CrystEngComm ◽  
2020 ◽  
Vol 22 (7) ◽  
pp. 1230-1238 ◽  
Author(s):  
Philippe Negrier ◽  
Bacem Ben Hassine ◽  
Maria Barrio ◽  
Michela Romanini ◽  
Denise Mondieig ◽  
...  

The polymorphism of 1,3-dimethyladamantane (13DMA), 1,3-adamantanediol (13DOHA) and 1,3-dibromoadamantane (13DBrA) has been studied by X-ray powder diffraction, density measurements and differential scanning calorimetry at normal and high-pressure.


Author(s):  
Kuralla Hari ◽  
Saripilli Rajeswari ◽  
Kolapalli Venkata Ramanamurthy

Objective: To formulate orally disintegrating taste masked tablets of drotaverine hydrochloride (HCl) by sublimation technique.Methods: Initially superdisintegrant was selected and its concentration was optimized by pre-compression and post-compression parametric evaluation. Camphor and menthol were used as sublimating agents alone and in combination to mask the taste of drotaverine hydrochloride. Prepared tablets were evaluated for physicochemical evaluation, in vitro dissolution studies and fourier transformation-infrared spectroscopy, differential scanning calorimetry and X-ray diffractometry studies.Results: The optimised formulation DCM2 prepared with a mixture of camphor and menthol was characterised by fourier transformation-infrared spectroscopy, differential scanning calorimetry and X-ray diffractometry studies and found no incompatibility and no major shifts were noticed.Conclusion: The results demonstrated that the prepared drotaverine HCl orally disintegrating tablets showed better taste masking. The present sublimation technique can be effectively used for taste masking and also for orally disintegrating tablets.


Author(s):  
Peter Zietlow ◽  
Tobias Beirau ◽  
Boriana Mihailova ◽  
Lee A. Groat ◽  
Thomas Chudy ◽  
...  

AbstractRadiation damage in minerals is caused by the α-decay of incorporated radionuclides, such as U and Th and their decay products. The effect of thermal annealing (400–1000 K) on radiation-damaged pyrochlores has been investigated by Raman scattering, X-ray powder diffraction (XRD), and combined differential scanning calorimetry/thermogravimetry (DSC/TG). The analysis of three natural radiation-damaged pyrochlore samples from Miass/Russia [6.4 wt% Th, 23.1·10


Author(s):  
R. Hübner ◽  
A. Belger ◽  
D. C. Meyer ◽  
P. Paufler ◽  
I. G. Polyakova

AbstractCrystallisation and annealing behaviour of two caesium borosilicate glass samples with approximate boroleucite composition were characterised by means of differential scanning calorimetry measurements as well as X-ray powder diffraction investigations with subsequent profile fitting of the observed patterns according to the Rietveld and/or Pawley method. While one sample crystallised primarily in an orthorhombic phase (


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