scholarly journals Kinetics of the Solution-Mediated Polymorphic Transformation of the Novel l-Carnitine Orotate Polymorph, Form-II

Pharmaceutics ◽  
2018 ◽  
Vol 10 (4) ◽  
pp. 171 ◽  
Author(s):  
Ji-Hun An ◽  
Wonno Youn ◽  
Alice Kiyonga ◽  
Changjin Lim ◽  
Minho Park ◽  
...  
Keyword(s):  
Mass Transfer ◽  
Solid State ◽  
Polymorphic Transformation ◽  
Transformation Process ◽  
Resonance Spectroscopy ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Treatment And Prevention ◽  
Transfer Equations ◽  
Reactive Crystallization

Research studies related to the polymorphs of l-Carnitine orotate (CO), a medication used for the treatment and prevention of liver diseases, are insignificant or almost nonexistent. Accordingly, in the present study, l-Carnitine orotate (CO) was prepared for investigating CO polymorphs. Here, a reactive crystallization was induced by reacting 1g of l-Carn (1 equivalent) and 0.97 g of OA (1 equivalent) in methanol (MeOH); as a result, CO form-I and CO form-II polymorphs were obtained after 1 h and 16 h of stirring, respectively. The characterization of CO polymorphs was carried out utilizing Powder X-ray diffraction (PXRD), Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA) and solid-state Nuclear Magnetic Resonance Spectroscopy (solid-state CP/MAS 13C-NMR). The solution-mediated polymorphic transformation (SMPT) of CO polymorphs was investigated in MeOH at controlled temperature and fixed rotational speed. The results revealed that CO form-I is a metastable polymorph while CO form-II is a stable polymorph. From the same results, it was confirmed that CO form-I was converted to CO form-II during the polymorphic phase transformation process. Moreover, it was assessed that the increase in temperature and supersaturation level significantly promotes the rate of nucleation, as well as the rate of mass transfer of CO form-II. In addition, nucleation and mass transfer equations were employed for the quantitative determination of SMPT experimental results. Lastly, it was suggested that CO form-II was more thermodynamically stable than CO form-I and that both polymorphs belong to the monotropic system.

scholarly journals Synthesis and Characterization of N-Substituted Polyether-Block-Amide Copolymers

Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 773
Author(s):  
Jyun-Yan Ye ◽  
Kuo-Fu Peng ◽  
Yu-Ning Zhang ◽  
Szu-Yuan Huang ◽  
Mong Liang
Keyword(s):  
Titanium Isopropoxide ◽  
Decomposition Temperature ◽  
Phenyl Isocyanate ◽  
Cross Linking ◽  
Resonance Spectroscopy ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Degradation Temperature ◽  
Melt Polycondensation ◽  
Structural Regularity

A series of N-substituted polyether-block-amide (PEBA-X%) copolymers were prepared by melt polycondensation of nylon-6 prepolymer and polytetramethylene ether glycol at an elevated temperature using titanium isopropoxide as a catalyst. The structure, thermal properties, and crystallinity of PEBA-X% were investigated using nuclear magnetic resonance spectroscopy, Fourier-transform infrared spectroscopy, differential scanning calorimetry, wide angle X-ray diffraction, and thermogravimetric analysis. In general, the crystallinity, melting point, and thermal degradation temperature of PEBA-X% decreased as the incorporation of N-methyl functionalized groups increased, owing to the disruption caused to the structural regularity of the copolymer. However, in N-acetyl functionalized analogues, the crystallinity first dropped and then increased because of a new γ form arrangement that developed in the microstructure. After the cross-linking reaction of the N-methyl-substituted derivative, which has electron-donating characteristics, with poly(4,4′-methylenebis(phenyl isocyanate), the decomposition temperature of the resulting polymer significantly increased, whereas no such improvements could be observed in the case of the electro-withdrawing N-acetyl-substituted derivative, because of the incompleteness of its cross-linking reaction.

PHASE TRANSFORMATIONS DURING HEATING OF AMORPHOUS/NANOCRYSTALLINE Ni–Ti POWDERS

2010 ◽  
Vol 24 (09) ◽  
pp. 1137-1140 ◽  
Author(s):  
M. M. VERDIAN ◽  
M. SALEHI ◽  
K. RAEISSI
Keyword(s):  
Differential Scanning Calorimetry ◽  
Solid State ◽  
Phase Transformations ◽  
Low Energy ◽  
Heating Process ◽  
Study Phase ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Niti Phase

Amorphous/nanocrystalline 50 Ni –50 Ti powders were synthesized from elemental Ti and Ni powders by solid state synthesis utilizing low energy mechanical alloying with times up to 100 h. The produced powders were investigated by X-ray diffraction and differential scanning calorimetry to study phase transformations that occurred during heating in the calorimeter. It was found that at the first stage of the heating process, a disordered NiTi phase was formed at temperature of about 400°C. Further investigations indicated that this phase transformed into the Ni 3 Ti and Ti 2 Ni intermetallic compounds after heating at a temperature of about 800°C.

Tautomeric polymorphism of the neuroactive inhibitor kynurenic acid

2019 ◽  
Vol 75 (6) ◽  
pp. 793-805
Author(s):  
Dorota Pogoda ◽  
Jan Janczak ◽  
Sylwia Pawlak ◽  
Michael Zaworotko ◽  
Veneta Videnova-Adrabinska
Keyword(s):  
Solid State ◽  
Kynurenic Acid ◽  
Variable Temperature ◽  
Neurological Diseases ◽  
Crystal Form ◽  
Phase Behaviour ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray

Kynurenic acid (KYN; systematic name: 4-hydroxyquinoline-2-carboxylic acid, C10H7NO3) displays a therapeutic effect in the treatment of some neurological diseases and is used as a broad-spectrum neuroprotective agent. However, it is understudied with respect to its solid-state chemistry and only one crystal form (α-KYN·H2O) has been reported up to now. Therefore, an attempt to synthesize alternative solid-state forms of KYN was undertaken and six new species were obtained: five solvates and one salt. One of them is a new polymorph, β-KYN·H2O, of the already known KYN monohydrate. All crystal species were further studied by single-crystal and powder X-ray diffraction, thermal and spectroscopic methods. In addition to the above methods, differential scanning calorimetry (DSC), in-situ variable-temperature powder X-ray diffraction and Raman microscopy were applied to characterize the phase behaviour of the new forms. All the compounds display a zwitterionic form of KYN and two different enol–keto tautomers are observed depending on the crystallization solvent used.

Physicochemistry of the Tomb of Nefertari, Egypt.

1988 ◽  
Vol 123 ◽  
Author(s):  
J. E. Smeaton ◽  
George Burns
Keyword(s):  
Differential Scanning Calorimetry ◽  
Sodium Chloride ◽  
Solid State ◽  
Kinetic Study ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Physicochemical Processes ◽  
Gypsum Dehydration

AbstractThe Tomb of Nefertari, no. 66, Valley of the Queens, is an internationally known monument of historic and artistic importance; it is considere d one of the most beautiful of the Royal Egyptian tombs. The fragility of its plaster along with its ubiquitous sodium chloride crystals and microcrystals have complicated its conservation and restoration. In order to determine the optimum pathway for its conservation, the physicochemical processes which occur now in this Tomb must be well understood. To improve this understanding, samples of plaster taken from the Tomb have been analyzed using Differential Scanning Calorimetry and X-ray Diffraction and have been shown to be fully dehydrated; previous findings suggest that this is not the case in all contemporary Royal tombs. Although we are not aware of any kinetic study of gypsum dehydration in the solid state, the presence of anhydrite in the Tomb of Nefertari suggests that the CaSO4 ·2H2O → CaSO4 + 2H2O reaction is catalyzed. It is reasoned that finely-dispersed sodium chloride crystals act as effective catalysts in this reaction.

scholarly journals Preparation and thermal decomposition of solid state cinnamates of alkali earth metals, except beryllium and radium

1998 ◽  
Vol 23 (0) ◽  
pp. 91-98 ◽  
Author(s):  
Ana Glauce ZAINA CHIARETTO ◽  
Marco Aurélio da Silva CARVALHO FILHO ◽  
Nedja Suely FERNANDES ◽  
Massao IONASHIRO
Keyword(s):  
Thermal Stability ◽  
Differential Scanning Calorimetry ◽  
Thermal Decomposition ◽  
Solid State ◽  
General Formula ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Preparation And Thermal Decomposition ◽  
Derivative Thermogravimetry

Solid state compounds of general formula ML2.nH2O [where M is Mg, Ca, Sr or Ba; L is cinnamate (C6H5 -CH=CH-COO-) and n = 2, 4, 0.8, 3 respectively], have been synthetized. Thermogravimetry (TG), derivative thermogravimetry (DTG), differential scanning calorimetry (DSC) and X-ray diffraction powder patterns have been used to characterize and to study the thermal stability and thermal decomposition of these compounds.

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.

Sustainable Pharmaceutical Preparation Methods and Solid-state analysis Supporting Green Pharmacy

2020 ◽  
Vol 16 ◽  
Author(s):  
Ilma Nugrahani
Keyword(s):  
Solid State ◽  
Pharmaceutical Preparation ◽  
Three Dimensional ◽  
Chemical Properties ◽  
Environmental Damage ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Preparation Methods ◽  
Physical And Chemical ◽  
State Analysis

: Every "entity" or compound has physical and chemical properties as references for the synthesis and determination of the entity's structure. Thermodynamically, solid-state is the most stable matter in the universe and to be the ideal form in structure elucidation of pharmaceutical. The dry treatments become popular, such as mechanochemistry, microwave heating, and the using of deep eutectic agent. These techniques are viewed as the futuristic methods for reducing environmental damage, in line with "green pharmacy" concept. On the other hand, solid-state analysis methods from the simplest to the most sophisticated one have been used in the long decades, but most are for qualitative purposes. Recently many reports have proven that solid-state analysis instruments are reliable and prospective for implementing in the quantitative measurement. Infrared spectroscopy, powder x-ray diffraction, and differential scanning calorimetry have been employed in various kinetics and content determination studies. A revolutionary method developed for structural elucidation is single-crystal diffraction, which is capable of rapidly and accurately determining a three-dimensional chemical structure. Hereby it shown that the accurate, precise, economical, ease, rapid-speed, and reliability of solid-state analysis method are eco-benefits by reducing the reagent, catalyst, and organic solvent.

scholarly journals Synthesis, characterization and thermal behaviour of solid-state compounds of 4-methoxybenzoate with lanthanum (III) and trivalent lighter lanthanides

2006 ◽  
Vol 31 (1) ◽  
pp. 21-30 ◽  
Author(s):  
E. C. Rodrigues ◽  
A. B. Siqueira ◽  
E. Y. Ionashiro ◽  
G. Bannach ◽  
M. Ionashiro
Keyword(s):  
Thermal Analysis ◽  
Differential Scanning Calorimetry ◽  
Thermal Decomposition ◽  
Differential Thermal Analysis ◽  
Solid State ◽  
Thermal Behaviour ◽  
Polymorphic Transformation ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Lighter Lanthanides

Solid-state M-4-MeO-Bz compounds, where M stands for trivalent La, Ce, Pr, Nd and Sm and 4-MeO-Bz is 4-methoxybenzoate, have been synthesized. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffractometry, infrared spectroscopy and complexometry were used to characterize and to study the thermal behaviour of these compounds. The results led to information about the composition, dehydration, polymorphic transformation, ligand's denticity, thermal behaviour and thermal decomposition of the isolated compounds.

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