scholarly journals Substituted Azolium Disposition: Examining the Effects of Alkyl Placement on Thermal Properties

Crystals ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 34 ◽  
Author(s):  
Karel Goossens ◽  
Lena Rakers ◽  
Tae Shin ◽  
Roman Honeker ◽  
Christopher Bielawski ◽  
...  

We describe the thermal phase characteristics of a series of 4,5-bis(n-alkyl)azolium salts that were studied using thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), polarized-light optical microscopy (POM), and synchrotron-based small- to wide-angle X-ray scattering (SWAXS) measurements. Key results were obtained for 1,3-dimethyl-4,5-bis(n-undecyl)imidazolium iodide (1-11), 1,3-dimethyl-4,5-bis(n-pentadecyl)- imidazolium iodide (1-15), and 1,2,3-trimethyl-4,5-bis(n-pentadecyl)imidazolium iodide (2), which were found to adopt enantiotropic smectic A mesophases. Liquid-crystalline mesophases were not observed for 1,3-dimethyl-4,5-bis(n-heptyl)imidazolium iodide (1-7), 3-methyl-4,5-bis(n-penta-decyl)thiazolium iodide (3), and 2-amino-4,5-bis(n-pentadecyl)imidazolium chloride (4). Installing substituents in the 4- and 5-positions of the imidazolium salts appears to increase melting points while lowering clearing points when compared to data reported for 1,3-disubstituted analogues.

2009 ◽  
Vol 24 (1) ◽  
pp. 156-163 ◽  
Author(s):  
Rabkwan Chuealee ◽  
Timothy S. Wiedmann ◽  
Teerapol Srichana

Sodium cholesteryl carbonate ester (SCC) was synthesized, and its phase behavior was studied. The chemical structure was assessed by solid-state infrared spectroscopy based on vibration analysis. The wave number at 1705 and 1276 cm−1 corresponds to a carbonyl carbonate and O–C–O stretching of SCC, respectively. Molecular structure of SCC was further investigated with 1H and 13C NMR spectroscopy. The chemical shift, for the carbonyl carbonate resonance appeared at 155.5 ppm. A molecular mass of SCC was at m/z of 452. Differential scanning calorimetry (DSC), video-enhanced microscopy (VEM) together with polarized light microscopy, and small-angle x-ray scattering (SAXS) were used to characterize the phase behavior as a function of temperature of SCC. Liquid crystalline phase was formed with SCC. Based on the thermal properties and x-ray diffraction, it appears that SCC forms a structure analogous to the type II monolayer structure observed with cholesterol esters.


2019 ◽  
Vol 43 (1-2) ◽  
pp. 67-77 ◽  
Author(s):  
Adil A Awad ◽  
Al-Ameen Bariz OmarAli ◽  
Ahmed Jasim M Al-Karawi ◽  
Zyad Hussein J Al-Qaisi ◽  
Samer Ghanim Majeed

{1-[4-( n-Alkoxy)]-2-(4’-decyloxy)benzylidene}hydrazines ( n-alkoxy = O(CH2) nH, n = 1–9, 12, 16 or 18), an asymmetrical series of 1,2-disubstituted hydrazines, were prepared in a simple two-step procedure as a part of our continuing work in evaluating hydrophobic azine compounds as photoluminescent liquid crystalline materials. The compounds were characterized spectroscopically and their liquid crystalline behaviour and luminescent properties were evaluated using polarized light optical microscopy, differential scanning calorimetry and X-ray powder diffraction techniques. The studies revealed that all of these compounds are liquid crystalline materials exhibiting photoluminescent properties in the crystalline and liquid crystal states.


2010 ◽  
Vol 88 (7) ◽  
pp. 639-645 ◽  
Author(s):  
Kyle A. Hope-Ross ◽  
Paul A. Heiney ◽  
John F. Kadla

A series of C2-symmetric compounds with different core sizes and varying lengths and numbers of alkoxy side chains were prepared, and the factors influencing their liquid crystalline mesophase behaviour were investigated. The compounds studied were based on benzophenone, dibenzylidene-acetone, and 1,9-diphenyl-nona-1,3,6,8-tetraen-5-one cores with either 1 or 2 linear alkoxy side chains. The side chains were varied in length from C6H13 to C12H25. The liquid crystalline mesophase behaviour of the compounds was investigated using differential scanning calorimetry, polarizing optical microscopy, and small-angle X-ray scattering (SAXS). It was found that a number of the molecules were able to self-assemble into smectic and nematic liquid crystalline phases.


1998 ◽  
Vol 10 (1) ◽  
pp. 147-153 ◽  
Author(s):  
M Tanaka ◽  
M Konda ◽  
M Miyamoto ◽  
Y Kimura ◽  
A Yamaguchi

Anomalous solid structures formed by a thermotropic liquid crystalline polyimide (PI-LC) were investigated by thermal analysis, polarized light microscopy and x-ray analysis. It was revealed that PI-LC should undergo a phase transition from the crystalline to the isotropic phase through the smectic or nematic phase in the temperature range 277–300 °C. The PI-LC filament extruded at 280 °C, at which temperature the polymer was in liquid crystalline phase, was formed to have a structure similar to the smectic C phase, while that extruded and melt-drawn at 310 °C, at which temperature the polymer was in the isotropic phase, had a structure similar to the smectic A phase.


1996 ◽  
Vol 425 ◽  
Author(s):  
C. S. Hsu ◽  
C. J. Lee

AbstractThe synthesis of two series of side-chain liquid crystalline polyoxetanes and polyoxiranes containing 4-alkanyloxybiphenyl-4′ -yl (2S,3S)-2-chloro-3-methylvalerate side groups is presented. Differential scanning calorimetry, polarizing optical microscopy, and X-ray diffractometry reveal smectic mesomorphism for all obtained polymers. Most of the prepared polyoxetanes present smectic A and chiral smectic C phases. The polyoxetane containing tweleve methylene units in the spacer is the only one showing two enantiotropic smectic A and B phases. All of the obtained polyoxiranes display two enantiotropic smectic A and B phases. Although the polyoxetane and polyoxirane backbones are more flexible than the polymethacrylate backbone, side-chain crystallization do not occur in any of the synthesized polymers.


Polymers ◽  
2021 ◽  
Vol 13 (15) ◽  
pp. 2442
Author(s):  
Nicolás María ◽  
Jon Maiz ◽  
Daniel E. Martínez-Tong ◽  
Angel Alegria ◽  
Fatimah Algarni ◽  
...  

The crystallization and morphology of two linear diblock copolymers based on polymethylene (PM) and poly(vinylidene fluoride) (PVDF) with compositions PM23-b-PVDF77 and PM38-b-PVDF62 (where the subscripts indicate the relative compositions in wt%) were compared with blends of neat components with identical compositions. The samples were studied by SAXS (Small Angle X-ray Scattering), WAXS (Wide Angle X-ray Scattering), PLOM (Polarized Light Optical Microscopy), TEM (Transmission Electron Microscopy), DSC (Differential Scanning Calorimetry), BDS (broadband dielectric spectroscopy), and FTIR (Fourier Transform Infrared Spectroscopy). The results showed that the blends are immiscible, while the diblock copolymers are miscible in the melt state (or very weakly segregated). The PVDF component crystallization was studied in detail. It was found that the polymorphic structure of PVDF was a strong function of its environment. The number of polymorphs and their amount depended on whether it was on its own as a homopolymer, as a block component in the diblock copolymers or as an immiscible phase in the blends. The cooling rate in non-isothermal crystallization or the crystallization temperature in isothermal tests also induced different polymorphic compositions in the PVDF crystals. As a result, we were able to produce samples with exclusive ferroelectric phases at specific preparation conditions, while others with mixtures of paraelectric and ferroelectric phases.


Soft Matter ◽  
2021 ◽  
Author(s):  
Vida Jamali ◽  
Francesca Mirri ◽  
Evan G. Biggers ◽  
Robert A. Pinnick ◽  
Lucy Liberman ◽  
...  

Quantitative characterization of the phase behavior of carbon nanotube liquid crystalline solutions at high concentrations using polarized light microscopy and small angle X-ray scattering


2018 ◽  
Vol 8 (4) ◽  
pp. 609-615 ◽  
Author(s):  
Maryam Rezvani ◽  
Javad Hesari ◽  
Seyed Hadi Peighambardoust ◽  
Maria Manconi ◽  
Hamed Hamishehkar

Purpose: To potentially enhance the bioavailability and extend the bioactivity effectiveness of Isoleucine-Proline-Proline (IPP, an antihypertensive bioactive peptide of dairy origin), a novel Lyotropic Liquid Crystalline Pharmacosomal Nanoparticle (LLCPNP) was synthesized, and its physicochemical and technological characteristics were studied. Methods: LLCPNPs precursors were developed using IPP and soy phosphatidylcholine via complex formation. Polarized light microscopy, small angle X-ray scattering, differential scanning calorimetry, dynamic light scattering and Fourier transform infrared spectroscopy were employed to characterize the physicochemical properties of the nanoparticles. The in-vitro release and its related mechanisms were also studied. Results: Fourier transform infrared spectroscopy confirmed the complexation between the components of LLCPNPs. Phase behavior evaluation by polarized light microscope showed the characteristic birefringent texture. These findings along with those of small angle X-ray scattering and differential scanning calorimetry proved the formation of lamellar LLCPNPs. These particles represented nanometric size (<100 nm), high incorporation efficiency (93.72%) and proper physicochemical stability during long-term storage. In-vitro studies demonstrated a sustained release behavior fitted to non-Fickian diffusion and Higuchi kinetic models. Conclusion: The present study results emphasized that LLCPNPs could be proposed as an unrivaled carrier to promote the bioavailability, stability and shelf-life of nutraceutical and biopharmaceutical formulations containing bioactive peptides.


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