Analyses of Multi- Phase Pharmaceuticals Using SImultaneous Differential Scanning Calorimetry and X-Ray Diffraction

1985 ◽  
Vol 29 ◽  
pp. 323-332
Author(s):  
T. G. Fawcett ◽  
E. J. Martin ◽  
C. E. Crowder ◽  
P. J. Kincaid ◽  
A. J. Strandjord ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Powder Diffraction ◽  
Molecular Water ◽  
Molecular Symmetry ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Pharmaceutical Samples ◽  
X Ray ◽  
Overlapping Peaks ◽  
Multi Phase

The analysis of multi-phase pharmaceuticals, particularly when similar structures are involved (i.e. polymorphs, salts or hydrates), can often be a difficult task. Historically, x-ray powder diffraction (XRD) and differential scanning calorimetry (DSC) have been utilized to study pharmaceutical samples. Relative to other materials, diffraction data for pharmaceuticals are often complex due to the large number of diffraction maxima caused by the size of the molecule and/or the molecular symmetry. Multi-phase mixtures tend to have a large number of overlapping peaks which can hinder the difftactionist's ability to identify phases and interpret the data. When similar structures are analyzed calorimetrically, their thermal events may severely overlap (as will be shown), preventing accurate interpretation of the data. In addition there are several types of thermal events which may not be related to structural transitions. A common one in pharmaceuticals is the loss of solvent or absorbed (versus molecular) water.

Simultaneous measurements of X-ray diffraction (XRD) and differential scanning calorimetry (DSC) data under controlled humidity condition: Instrumentation and application to studies on hydration, dehydration, and rehydration processes of pharmaceutical compounds

2004 ◽  
Vol 19 (1) ◽  
pp. 31-35 ◽  
Author(s):  
A. Kishi ◽  
H. Toraya
Keyword(s):  
Differential Scanning Calorimetry ◽  
Powder Diffraction ◽  
Simultaneous Measurement ◽  
Pharmaceutical Compounds ◽  
Design Concept ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Humidity Condition ◽  
Simultaneous Measurements

An instrument for the simultaneous measurement of X-ray powder diffraction (XRD) data and differential scanning calorimetry (DSC) data under a controlled humidity condition has been developed in order to achieve a design concept of reliable and simple in operation. Examples of the application to studies on hydration, dehydration, and rehydration processes of pharmaceutical compounds under various humidity conditions are presented. The usefulness of the present XRD-DSC system will be demonstrated.

Research on compatibility and surface of high impact bio-based polyamide

2021 ◽  
pp. 095400832110055
Author(s):  
Yang Wang ◽  
Yuhui Zhang ◽  
Yuhan Xu ◽  
Xiucai Liu ◽  
Weihong Guo
Keyword(s):  
Electron Microscopy ◽  
Mechanical Properties ◽  
Scanning Electron Microscopy ◽  
Differential Scanning Calorimetry ◽  
Crystallization Behavior ◽  
High Impact ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Scanning Electron

The super-tough bio-based nylon was prepared by melt extrusion. In order to improve the compatibility between bio-based nylon and elastomer, the elastomer POE was grafted with maleic anhydride. Scanning Electron Microscopy (SEM) and Thermogravimetric Analysis (TGA) were used to study the compatibility and micro-distribution between super-tough bio-based nylon and toughened elastomers. The results of mechanical strength experiments show that the 20% content of POE-g-MAH has the best toughening effect. After toughening, the toughness of the super-tough nylon was significantly improved. The notched impact strength was 88 kJ/m2 increasing by 1700%, which was in line with the industrial super-tough nylon. X-ray Diffraction (XRD) and Differential Scanning Calorimetry (DSC) were used to study the crystallization behavior of bio-based PA56, and the effect of bio-based PA56 with high crystallinity on mechanical properties was analyzed from the microstructure.

scholarly journals Synthesis and mesomorphic properties of calamitic malonates and cyanoacetates tethered to 4-cyanobiphenyls

2012 ◽  
Vol 8 ◽  
pp. 371-378 ◽  
Author(s):  
Katharina C Kress ◽  
Martin Kaller ◽  
Kirill V Axenov ◽  
Stefan Tussetschläger ◽  
Sabine Laschat
Keyword(s):  
Differential Scanning Calorimetry ◽  
Ambient Temperature ◽  
Liquid Crystalline ◽  
X Ray Diffraction ◽  
Cyanoacetic Acid ◽  
Scanning Calorimetry ◽  
Isotropic Liquid ◽  
X Ray ◽  
Nematic Phases ◽  
Mesomorphic Properties

4-Cyano-1,1'-biphenyl derivatives bearing ω-hydroxyalkyl substituents were reacted with methyl 3-chloro-3-oxopropionate or cyanoacetic acid, giving liquid-crystalline linear malonates and cyanoacetates. These compounds formed monotropic nematic phases at 62 °C down to ambient temperature upon cooling from the isotropic liquid. The mesomorphic properties were investigated by differential scanning calorimetry, polarizing optical microscopy and X-ray diffraction (WAXS).

Inosose-Flüssigkristalle / Inosose Liquid Crystals

1990 ◽  
Vol 45 (7) ◽  
pp. 1084-1090 ◽  
Author(s):  
Klaus Praefcke ◽  
Bernd Kohne ◽  
Andreas Eckert ◽  
Joachim Hempel
Keyword(s):  
Differential Scanning Calorimetry ◽  
Liquid Crystal ◽  
High Temperature ◽  
Liquid Crystalline ◽  
Structural Features ◽  
Lyotropic Liquid Crystal ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Alkyl Chains

Six S,S-dialkyl acetals 2a-f of inosose (1), tripodal in structure, have been synthesized, characterized and investigated by optical microscopy and differential scanning calorimetry (d.s.c.). The four S,S-acetals 2c-f with sufficiently long alkyl chains are thermotropic liquid crystalline; 2 e and 2 f are even dithermomesomorphic. Each of these four inosose derivatives 2c-f exhibits monotropically a most likely cubic mesophase (MI); in addition 2e and 2f show enantiotropically a hexagonal mesophase (Hx) with a non-covalent, supramolecular H-bridge architecture. Whereas the nature of the optically isotropic mesophase MI needs further clarification the stable high temperature mesophase Hx of 2 e and 2 f has been established by a miscibility test using a sugar S,S-dialkyl acetal also tripodal in structure and with a Hx phase proved by X-ray diffraction, but in contrast to 2 with an acyclic hydrophilic part. Similarities of structural features between the Hx-phases of 2e and 2f as well as of other thermotropic and lyotropic liquid crystal systems are discussed briefly.

scholarly journals Stacking Control by Molecular Symmetry of Sterically Protected Phthalocyanines

Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5552
Author(s):  
Ryota Kudo ◽  
Masahiro Sonobe ◽  
Yoshiaki Chino ◽  
Yu Kitazawa ◽  
Mutsumi Kimura
Keyword(s):  
Lamellar Structure ◽  
Synthesis And Characterization ◽  
Molecular Symmetry ◽  
X Ray Diffraction ◽  
Melting Points ◽  
Scanning Calorimetry ◽  
Structural Isomers ◽  
X Ray ◽  
Temperature Controlled

The synthesis and characterization of two phthalocyanine (Pc) structural isomers, 1 and 2, in which four 2,6-di(hexyloxy)phenyl units were attached directly to the 1,8,15,22- or 1,4,15,18-positions of the Pc rings, are described. Both Pcs 1 and 2 exhibited low melting points, i.e., 120 and 130 °C respectively, due to the reduction in intermolecular π-π interaction among the Pc rings caused by the steric hindrance of 2,6-dihexyloxybenzene units. The thermal behaviors were investigated with temperature-controlled polarizing optical microscopy, differential scanning calorimetry, powder X-ray diffraction, and absorption spectral analyses. Pc 1, having C4h molecular symmetry, organized into a lamellar structure containing lateral assemblies of Pc rings. In contrast, the other Pc 2 revealed the formation of metastable crystalline phases, including disordered stacks of Pcs due to rapid cooling from a melted liquid.

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.

scholarly journals Thermal behaviour study of solid state compounds of manganese (II), zinc (II) and lead (II) with cinnamic acid

1998 ◽  
Vol 23 (0) ◽  
pp. 09-16
Author(s):  
Marco Aurélio da Silva CARVALHO FILHO ◽  
Massao IONASHIRO
Keyword(s):  
Thermal Stability ◽  
Aqueous Solution ◽  
Differential Scanning Calorimetry ◽  
Cinnamic Acid ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Manganese Zinc ◽  
Behaviour Study ◽  
Derivative Thermogravimetry

Compounds of cinnamic acid with manganese, zinc and lead have been prepared in aqueous solution. Thermogravimetry, derivative thermogravimetry (TG, DTG), differential scanning calorimetry (DSC), X-ray diffraction and complexometry have been used in the characterization as well as in the study of the thermal stability and interpretation concerning the thermal decomposition.

scholarly journals Nanocrystal, phase transformation and microstructure of Ni50Ti50 shape memory alloy

2018 ◽  
Vol 24 (02) ◽  
pp. 22-25
Author(s):  
Dovchinvanchig M ◽  
Chunwang Zhao
Keyword(s):  
Differential Scanning Calorimetry ◽  
Phase Transformation ◽  
Shape Memory Alloy ◽  
Shape Memory ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
One Step ◽  
Niti Matrix ◽  
Electronic Microscope

The nanocrystal, phase transformation and microstructure behavior of Ni50Ti50 shape memory alloy was investigated by scanning electronic microscope, X-ray diffraction and differential scanning calorimetry. The results showed that the microstructure of Ni-Ti binary alloy consists of the NiTi2 phase and the NiTi matrix phase. One-step phase transformation was observed alloy.

Influence of Gd Addition on the Structure and Capability of Ni-Mn-In Metamagnetic Shape Memory Alloys

2012 ◽  
Vol 535-537 ◽  
pp. 950-953
Author(s):  
Li Na Bai ◽  
Gui Xing Zheng ◽  
Zhi Jian Duan ◽  
Jian Jun Zhang
Keyword(s):  
Differential Scanning Calorimetry ◽  
Magnetic Properties ◽  
Magnetic Property ◽  
Transition Temperature ◽  
Martensitic Transformation ◽  
Room Temperature ◽  
Vibrating Sample Magnetometry ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray

The influences of Gd concentration on martensitic transformation and magnetic properties of NiMnIn alloys were investigated by differential scanning calorimetry (DSC) , vibrating sample magnetometry (VSM), X-ray diffraction (XRD) and etc. It is Observed through the experiment: the addition of Gd enhances martensite transition temperature;X-ray diffraction analysis of experimental alloys is revealed that to the mixture is martensite and austenite at room temperature; content of Gd is not proportional to the improvement of magnetic property.

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