scholarly journals Submerged Eutectic-Assisted, Solvent-Free Mechanochemical Formation of a Propranolol Salt and Its Other Multicomponent Solids

Pharmaceutics ◽  
2021 ◽  
Vol 13 (12) ◽  
pp. 2125
Author(s):  
Klaudia Bialek ◽  
Zaneta Wojnarowska ◽  
Marcin Skotnicki ◽  
Brendan Twamley ◽  
Marian Paluch ◽  
...  
Keyword(s):  
Pharmaceutical Research ◽  
Capric Acid ◽  
Ionic Character ◽  
X Ray Diffraction ◽  
Mechanism Of Formation ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Broadband Dielectric Spectroscopy ◽  
Salt Structure ◽  
Pharmaceutical Processes

Salt preparation via a solid-state reaction offers a solution to challenges posed by current pharmaceutical research, which include combining development of novel forms of active pharmaceutical ingredients with greener, sustainable synthesis. This work investigated in detail the mechanism of salt formation between propranolol (PRO) and capric acid (CAP) and explored the solid eutectic phases comprising this salt, propranolol caprate (PRC). The salt structure was solved by X-ray diffraction, and the properties in the crystalline and supercooled states were fully characterised using thermal analysis, nuclear magnetic resonance, Fourier-transform infrared spectroscopy and broadband dielectric spectroscopy (BDS). PRC forms via a submerged eutectic phase composed of PRO and CAP, below room temperature, by mechanochemistry without an extra input of energy. Two other solid eutectic phases are composed of PRC and either CAP or PRO, at 0.28 and 0.82 mol fraction of PRO, respectively. BDS indicated that the supercooled PRC has ionic character, whereas the supercooled PRC-PRO eutectic had predominantly non-ionic properties despite comprising the salt. In conclusion, knowledge of the mechanism of formation of multicomponent systems can help in designing more sustainable pharmaceutical processes.

The Application of X-Ray Diffraction at Elevated Temperatures to Study the Mechanism of Formation of Sodium Tripolyphosphate

1961 ◽  
Vol 5 ◽  
pp. 276-284
Author(s):  
E. L. Moore ◽  
J. S. Metcalf
Keyword(s):  
High Temperature ◽  
Low Temperature ◽  
Amorphous Phase ◽  
Elevated Temperatures ◽  
Sodium Tripolyphosphate ◽  
X Ray Diffraction ◽  
Mechanism Of Formation ◽  
X Ray ◽  
Temperature Form ◽  
High Temperature Form

AbstractHigh-temperature X-ray diffraction techniques were employed to study the condensation reactions which occur when sodium orthophosphates are heated to 380°C. Crystalline Na4P2O7 and an amorphous phase were formed first from an equimolar mixture of Na2HPO4·NaH2PO4 and Na2HPO4 at temperatures above 150°C. Further heating resulted in the formation of Na5P3O10-I (high-temperature form) at the expense of the crystalline Na4P4O7 and amorphous phase. Crystalline Na5P3O10-II (low-temperature form) appears after Na5P3O10-I.Conditions which affect the yield of crystalline Na4P2O7 and amorphous phase as intermediates and their effect on the yield of Na5P3O10 are also presented.

scholarly journals Assay and physicochemical characterization of the antiparasitic albendazole

2012 ◽  
Vol 48 (2) ◽  
pp. 281-290 ◽  
Author(s):  
Noely Camila Tavares Cavalcanti ◽  
Giovana Damasceno Sousa ◽  
Maria Alice Maciel Tabosa ◽  
José Lamartine Soares Sobrinho ◽  
Leila Bastos Leal ◽  
...  
Keyword(s):  
Physicochemical Characterization ◽  
Analytical Techniques ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
X Ray Diffraction ◽  
Melting Points ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Complementary Techniques

The aim of this study was to characterize three batches of albendazole by pharmacopeial and complementary analytical techniques in order to establish more detailed specifications for the development of pharmaceutical forms. The ABZ01, ABZ02, and ABZ03 batches had melting points of 208 ºC, 208 ºC, and 209 ºC, respectively. X-ray diffraction revealed that all three batches showed crystalline behavior and the absence of polymorphism. Scanning electron microscopy showed that all the samples were crystals of different sizes with a strong tendency to aggregate. The samples were insoluble in water (5.07, 4.27, and 4.52 mg mL-1, respectively) and very slightly soluble in 0.1 M HCl (55.10, 56.90, and 61.70 mg mL-1, respectively) and additionally showed purities within the range specified by the Brazilian Pharmacopoeia 5th edition (F. Bras. V; 98% to 102%). The pharmacopeial assay method was not reproducible and some changes were necessary. The method was validated and showed to be selective, specific, linear, robust, precise, and accurate. From this characterization, we concluded that pharmacopeial techniques alone are not able to detect subtle differences in active pharmaceutical ingredients; therefore, the use of other complementary techniques is required to ensure strict quality control in the pharmaceutical industry.

THE COMPOSITION, STRUCTURE, AND MECHANISM OF FORMATION OF THE LINING OF THE GIZZARD OF THE CHICKEN

1964 ◽  
Vol 42 (1) ◽  
pp. 59-70 ◽  
Author(s):  
T. E. Webb ◽  
J. Ross Colvin
Keyword(s):  
Electron Microscope ◽  
Sedimentation Coefficient ◽  
Performic Acid ◽  
X Ray Diffraction ◽  
Mechanism Of Formation ◽  
Protein Layer ◽  
Covalent Bonds ◽  
X Ray ◽  
Disulphide Bonds ◽  
Composition Structure

The extracellular protein layer which surrounds the lumen of the gizzard of the chicken has been reinvestigated to determine if it is a keratin. The lining is insoluble in keratin solvents such as urea-bisulphite or Swan's reagent as well as thioglycollate and performic acid. In addition, it contains only 1.45% sulphur so that disulphide bonds cannot play a major role in its consolidation. The lining is insoluble in acids but readily dispersed in alkali without breaking of covalent bonds. The dispersion in alkali is retarded by electrolytes. The lining is hydrolyzed by trypsin and chymotrypsin at pH 8.0 but is resistant to pepsin at pH 2.0. An alkaline dispersion of the lining is heterogeneous in the ultracentrifuge, but not grossly so, with a mean sedimentation coefficient of 5.6 svedbergs. Electron microscope studies of the lining suggest it is an amorphous, precipitated protein, which is consistent with the observation of three hazy rings in X-ray diffraction powder patterns reflecting spacings of 3.5, 4.6, and 9.4 Å. Amino acid analysis shows a ratio of more than three acidic groups to one basic, with no carbohydrate residues and little lipid in the protein layer. These observations are interpreted as indicating the precipitation of an amorphous, non-keratin, acidic, abrasion-resistant protein from the glandular mucosa by the acid in the gizzard.

Copper(II) Complexes of a Tripyridyl Ligand: Anion-Dependent Metallosupramolecular Structures

2013 ◽  
Vol 66 (11) ◽  
pp. 1447 ◽  
Author(s):  
James E. M. Lewis ◽  
James D. Crowley
Keyword(s):  
Mass Spectrometry ◽  
Solid State ◽  
Coordination Polymer ◽  
Elemental Analysis ◽  
Spectroscopic Properties ◽  
Nitrate Salt ◽  
X Ray Diffraction ◽  
X Ray ◽  
Salt Structure ◽  
Solid State Structures

A series of copper(ii) complexes of the ligand 2,6-bis(pyridin-3-ylethynyl)pyridine have been synthesised and characterised by 1H and DOSY NMR, IR and UV-Vis spectroscopies, mass spectrometry, elemental analysis and single crystal X-ray diffraction. In solution these systems display almost identical spectroscopic properties, however the solid state structures are shown to vary widely, depending upon the choice of anion. The tetrafluoroborate salt was revealed to be a discrete Cu2L4 cage-like helicate. The tosylate salt, whilst of the same Cu2L4 stoichiometry, was shown to be a coordination polymer. Finally the nitrate salt structure was observed to be a discrete Cu2L2 metallocycle.

Shape-Controlled Synthesis and Formation Mechanism of Cobalt Nanopowders by a PVP-Assisted Method

2010 ◽  
Vol 654-656 ◽  
pp. 1186-1189 ◽  
Author(s):  
Bing Cong Zhang ◽  
Hong Ying Yu ◽  
Dong Bai Sun
Keyword(s):  
Hydrazine Hydrate ◽  
Chemical Reduction ◽  
Reducing Agent ◽  
Soft Template ◽  
Basic Solution ◽  
X Ray Diffraction ◽  
Mechanism Of Formation ◽  
X Ray ◽  
Nucleation Sites ◽  
Shape Controlled

Three different kinds of morphologies including spherical, chainlike and wirelike cobalt nanopowders, have been synthesized by chemical reduction of coblat chloride solution with hydrazine hydrate in basic solution. The products were characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). It was revealed that the morphologies of the nanopowders depend on the concentration of Co2+ and the way of adding reducing agent (hydrazine hydrate). These two features affected the nucleation sites and the number of nucleuses. When the concentration of Co2+ was low, nucleuses formed in the soft template, while the reducing of the reducing agent added drop wise, a little number of nucleuses was formed. Based on that, a mechanism of formation, as a basis of gram-scale syntheses, was proposed.

Morphological and Chemical Analyses of Manganese Dioxide Accretions on Mexican Ceramics

2004 ◽  
Vol 852 ◽  
Author(s):  
Caitlin R. O'Grady
Keyword(s):  
Manganese Dioxide ◽  
Microscopic Analysis ◽  
Chemical Analyses ◽  
X Ray Diffraction ◽  
Mechanism Of Formation ◽  
X Ray ◽  
Metropolitan Museum Of Art ◽  
The Arts ◽  
Spot Tests ◽  
Scanning Electron

ABSTRACTMicroscopic analysis of West Mexican ceramics (dating between in the collection of the Department of the Arts of Africa, Oceania and the Americas at the Metropolitan Museum of Art has established five different morphological types of manganese dioxide (MnO2) accretions. The accretions result mostly from a combination of bacterial and weathering activity in post-depositional contexts. Optical microscopy, scanning electron microscopy with energy dispersive x-ray analysis (SEM-EDS) and x-ray fluorescence (XRF) were successful; whereas microchemical spot tests, x-ray diffraction (XRD) and Raman spectroscopy proved inconclusive in the identification and differentiation of the five morphologies. Accretion morphology and substrate characteristics, together, suggest scenarios for the mechanism of formation and offer a qualitative tool for authentication. Accretions were documented using photomicrography, categorized based on empirical observations; sampled and analyzed using SEM-EDS and ND-XRF.

Whisker growth from an electroplated zinc coating

2010 ◽  
Vol 25 (11) ◽  
pp. 2175-2182 ◽  
Author(s):  
Alongheng Baated ◽  
Keun-Soo Kim ◽  
Katsuaki Suganuma
Keyword(s):  
Intermetallic Compounds ◽  
Whisker Growth ◽  
Steel Substrate ◽  
Zinc Coating ◽  
Floor Tile ◽  
X Ray Diffraction ◽  
Mechanism Of Formation ◽  
Oxide Formation ◽  
Reliable Operation ◽  
X Ray

The formation of Zn whiskers threatens the reliable operation of electronic equipment with an electrical shorting hazard. As with tin whiskers (much more intensively researched than Zn whiskers), the mechanism of formation is still not clear. This work investigated the Zn whisker growth mechanism for an electroplated Zn coating above a carbon steel substrate from a raised floor tile. Iron–zinc (Fe–Zn) intermetallic and Zn oxides were identified by x-ray diffraction analysis (XRD) and electron probe microanalysis (EPMA). Fe–Zn intermetallic compounds formed on the surface of the Zn layer in addition to the interface between the Zn coating and the steel substrate. Zn oxides formed primarily on the surface of the Zn coating. Fe–Zn intermetallic compounds and Zn oxide formation can be the source of a residual stress that promotes Zn diffusion to the surface of electroplated Zn coating, resulting in the formation of Zn whiskers.

scholarly journals Influence of cation order on the dielectric properties of (1 – x)Pb(Sc0:5Nb0:5)O3-xPb(Yb0:5Nb0:5)O3 ceramics

2020 ◽  
Vol 0 (0) ◽  
Author(s):  
Barbara Garbarz-Glos ◽  
Wojciech Bąk ◽  
Maija Antonova ◽  
Anna Kalvane ◽  
Czesław Kajtoch ◽  
...  
Keyword(s):  
Relaxor Ferroelectric ◽  
Solid State Reactions ◽  
Dielectric Studies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Broadband Dielectric Spectroscopy ◽  
Cation Order ◽  
Ceramic Samples ◽  
All Ceramic ◽  
Diffuse Phase

AbstractCeramic lead niobates and their solid solutions (1 – x)Pb(Sc0:5Nb0:5)O3 – xPb(Yb0:5Nb0:5)O3 were synthesized by solid state reactions from oxides. The structure of investigated samples was characterized by X-ray diffraction (XRD). Dielectric studies of the ceramics were performed by means of broadband dielectric spectroscopy at the temperature ranging from 600 K to 140 K. For all ceramic samples a diffuse phase transition as well as relaxor ferroelectric behavior were observed.

scholarly journals Evaluation of Thermal-Induced Polymorphic Transformation on Desloratadine and Desloratadine-Benzoic Acid Salt

2020 ◽  
Vol 26 (4) ◽  
pp. 399-405
Author(s):  
Ahmad Ainurofiq ◽  
Rachmat Mauludin ◽  
Diky Mudhakir ◽  
Sundani Nurono Soewandhi
Keyword(s):  
Melting Point ◽  
Benzoic Acid ◽  
Polymorphic Transformation ◽  
Heating Process ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Pharmaceutical Ingredients ◽  
Physicochemical Changes ◽  
Transformation Methods

Background: Active pharmaceutical ingredients face a challenge in manufacturing due to adverse physicomechanical properties. Desloratadine (DES) form I exhibits poor mechanical behavior through the formation of capping during the tableting process. Salt formation from DES and benzoic acid (BA) has been observed to resolve poor mechanical properties. However, the ability to withstand heat from the manufacturing process should be implemented in DES and DES-BA salt. The aim of this study was to determine the differences between thermal treatment results on DES and DES-BA salt and whether it causes them to undergo polymorphic transformation. Methods: Salt was crystallized between DES and BA using the solvent evaporation method. DES and DES-BA salt were heated at 110°C, 159°C (melting point of DES), 181°C (melting point of DES-BA), and 190°C. Following this, characterization was performed using differential scanning calorimetry (DSC), powder X-ray diffraction (PXRD), Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and solubility testing. Results: Polymorphic transformation caused by heat occurred in DES, but not in DES-BA salt. The transformation of DES was induced by the effect of heating, which changed polymorph I to a mixture of polymorph I and III at 110°C, to polymorph II at 159°C, and to a mixture of polymorph I, II, and III at 190°C. Under 190oC, DES-BA is still stable and did not undergo a polymorphic transformation. However, at 190oC, decomposition started to occur, which implied decreased solubility, which did not occur in DES. Conclusion: The heating process did not cause DES-BA salt to undergo a polymorphic transformation. However, it caused decomposition at 190oC. DES underwent a polymorphic transformation when exposed to the same condition without decomposition. This provided information to always pay attention to temperature during manufacturing processes that include DES or DES-BA salt to avoid physicochemical changes.

Phase Diagram and Cation Dynamics of Mixed MA1-xFAxPbBr3 Hybrid Perovskites

2021 ◽  
Author(s):  
Mantas Simenas ◽  
Sergejus Balčiūnas ◽  
Sarunas Svirskas ◽  
Martynas Kinka ◽  
Maciej Ptak ◽  
...  
Keyword(s):  
Phase Diagram ◽  
Room Temperature ◽  
Structural Phase ◽  
Cubic Phase ◽  
Structural Phase Transitions ◽  
X Ray Diffraction ◽  
X Ray ◽  
Dielectric Relaxations ◽  
Broadband Dielectric Spectroscopy ◽  
Molecular Cation

<p>We use a multi-technique approach to determine the phase diagram and molecular cation dynamics of mixed methylammonium-formamidinium MA1-xFAxPbBr3 (0 ≤ x ≤ 1) hybrid perovskites. The calorimetric, ultrasonic and X-ray diffraction experiments show a substantial suppression of the structural phase transitions and stabilization of the cubic phase upon mixing. We use the broadband dielectric and Raman spectroscopies to study the MA and FA cations dynamics in these compounds. The broadband dielectric spectroscopy indicates absence of the MA cation ordering and a gradual increase of the rotation barrier upon mixing. The room-temperature dielectric permittivity substantially decreases as the fraction of the FA cations is increased. No significant changes of the permittivity are detected at temperatures where the dielectric relaxations are absent. We also observe weak signatures of a dipolar glass phase for the highest mixing level (x = 0.5). The Raman spectroscopy supports the dielectric results and reveals additional subtle information about the FA cation dynamics.</p><br>

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