Differential scanning calorimetry and X-ray diffraction studies of a series of synthetic β-D-galactosyl diacylglycerols

1991 ◽  
Vol 69 (12) ◽  
pp. 863-867 ◽  
Author(s):  
D. A. Mannock ◽  
R. N. McElhaney

We have investigated the physical properties of a homologous series of synthetic, saturated 1,2-di-O-acyl-3-O-(β-D-galactopyranosyl)-sn-glycerols using calorimetry and X-ray diffraction. Unannealed aqueous dispersions of these compounds exhibit a lower temperature, moderately energetic, chain-melting (Lβ/Lα phase transition and a higher temperature, weakly energetic, bilayer/nonbilayer phase transition. On annealing below the Lβ/Lα phase transition, the Lβ phase converts to an LC phase, which may undergo a highly energetic LC/Lα or LC/HII phase transition at very high temperatures on reheating. The temperatures of these phase transitions are higher than those seen in the corresponding α- and β-D-glucosyl diacylglycerols. However, the Lβ/Lα and bilayer/nonbilayer phase transition temperatures of the β-D-galactosyl diacylglycerols are lower than those of the corresponding diacyl phosphatidylethanolamines. These observations are discussed in terms of the hydration and hydrogen bonding properties of their respective headgroups.Key words: differential scanning calorimetry, low-angle x-ray diffraction, glycolipids, galactolipids, lipid phase behaviour.

2007 ◽  
Vol 130 ◽  
pp. 257-262
Author(s):  
Maciej Kozak ◽  
Ludwik Domka ◽  
Stefan Jurga

The phase behaviour of lipid bilayer systems prepared with 1,2-distearoyl-sn-glycero-3- phosphocholine (DSPC) with dodecyldimethyl(benzyloxymethyl)ammonium chloride (BzMDDAC) (at concentrations 0.1, 1 and 5%) has been studied by small angle X-ray scattering and differential scanning calorimetry. The SAXS and DSC results of the hydrated 10% DSPC revealed one typical phase transition corresponding to melting of the hydrocarbon chains at 55 °C. In the system of 10% DSPC - 0.1 % BzMDDAC the main transition was somewhat shifted towards lower temperatures, while at 1% concentration of BzMDDAC in the mixture, the lamellar phase disappeared, as evidenced by SAXS and DSC. The increase in BzMDDAC concentration to 5% in the mixture with 10% DSPC resulted in formation of a new lamellar phase.


1990 ◽  
Vol 68 (1) ◽  
pp. 345-351 ◽  
Author(s):  
G. Lipka ◽  
H. Hauser

The phase behaviour of lipid X at high water concentrations (> 60%) is studied using mainly differential scanning calorimetry (DSC) and X-ray diffraction. The critical micellar concentration (CMC) decreases from 8 × 10−5 M at −2 °C to 4 × 10−5 M at 20 °C. The critical micellar temperature (CMT) is 0 °C and decreases slightly with increasing lipid X concentration. Above the CMC and below the CMT, lipid X forms a lamellar gel phase (Lβ). Above 0 °C and at concentrations ranging from the CMC up to about 0.2 M (20%), lipid X forms small micelles. At even higher concentrations there is a transition to a hexagonal phase, probably hexagonal I. Addition of excess NaCl to lipid X dispersions at concentrations < 0.2 M (20%) has several effects on the phase behaviour of lipid X. (i) The lamellar phase is stabilized up to temperatures of ≈20 °C at [NaCl] ≥ 0.7 M. (ii) NaCl induces a tighter packing of the hydrocarbon chains. (iii) At concentrations > 0.7 M NaCl, the bilayer repeat distance decreases to about 43 Å (1 Å = 0.1 nm).Key words: lipid X, phase behaviour, effects of NaCl, differential scanning calorimetry, X-ray diffraction.


Polymers ◽  
2020 ◽  
Vol 12 (1) ◽  
pp. 75
Author(s):  
Mengfan Wang ◽  
Weiyu Cao

Simultaneous measurements of wide-angle X-ray diffraction (WAXD) and differential scanning calorimetry (DSC) were carried out to investigate the phase transition and melting behaviors of poly(butylene adipate) (PBA). Thermal expansion changes along the a and b axes of the β form unit cell are different from each other during the heating process. At the beginning of the β to αH (high-temperature α phase) phase transition, the β phase melts very fast, while the recrystallization of the αH phase is delayed and slowed. With the further increment of the temperature, the melting rate of the β phase slows down, while the recrystallization of the αH phase accelerates. The diffraction peak intensity ratios of the β(020):β(110) and αH(020):αH(110) diffraction peaks during the first heating process have similar value. However, the above value is different from the value of α(020):α(110) during the following melt-crystallization process. This difference comes from the different orientations of the crystal lattices of the α and αH(β) crystals to the substrate plane, which indicates that the αH phase inherits the orientation of the β phase during phase transition and the orientation of αH form crystals is different from the α form crystals that crystallized from the melt.


2012 ◽  
Vol 68 (3) ◽  
pp. 287-296 ◽  
Author(s):  
Boris A. Zakharov ◽  
Evgeniy A. Losev ◽  
Boris A. Kolesov ◽  
Valeri A. Drebushchak ◽  
Elena V. Boldyreva

The occurrence of a first-order reversible phase transition in glycine–glutaric acid co-crystals at 220–230 K has been confirmed by three different techniques – single-crystal X-ray diffraction, polarized Raman spectroscopy and differential scanning calorimetry. The most interesting feature of this phase transition is that every second glutaric acid molecule changes its conformation, and this fact results in the space-group symmetry change from P21/c to P\bar 1. The topology of the hydrogen-bonded motifs remains almost the same and hydrogen bonds do not switch to other atoms, although the hydrogen bond lengths do change and some of the bonds become inequivalent.


1999 ◽  
Vol 562 ◽  
Author(s):  
J. P. Lokker ◽  
A. J. Bottger ◽  
G. C. A. M. Janssen ◽  
S. Radelaar

ABSTRACTThe precipitate formation occurring in Al-Cu thin foils with copper concentrations of either 1.15 at.% or 0.3 at.%, has been studied. In-situ X-ray diffraction analysis and differential scanning calorimetry are applied to determine the phases formed and the enthalpy changes in the same samples. Both X-ray diffraction and differential scanning calorimetry indicate that the precipitation behaviour of thin films (about 500 nm thickness) differs significantly from that of bulk material. In the films studied the precipitation of Al2Cu occurs at a much lower temperature than expected on the basis of the (bulk) phase diagram. Moreover, no intermediate phases are observed prior to Al2Cu precipitation. Also the amount of Cu in solid solution (0.20 at%Cu) observed by electron-probe micro-analysis after slowly cooling from 500°C to room temperature, exceeds the solubility of bulk Al-Cu.


2018 ◽  
Vol 2018 ◽  
pp. 1-5 ◽  
Author(s):  
Tekalign A. Tikish ◽  
Ashok Kumar ◽  
Jung Yong Kim

We report on the miscibility and phase behaviour of polypyrrole-polyaniline (PPy/PANI) as a function of blend composition. The PPy/PANI blends were prepared by solution processing method, using dimethyl sulfoxide (DMSO) solvent. Characterization of the polymer blends was carried out based on the data analysis from Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and differential scanning calorimetry (DSC). The PPy/PANI system was successfully formed blends in DMSO solvent. The polymer blends showed almost amorphous nature in XRD spectra because of intermolecular interaction between PPy and PANI macromolecules, which was confirmed by FT-IR data. Specifically, the DSC result for the PPY : PANI = 50 : 50 wt.% blend showed only one glass transition temperature (Tg), which indicates that the two polymers are well miscible without undergoing any phase separation.


1999 ◽  
Vol 54 (5) ◽  
pp. 287-290 ◽  
Author(s):  
S. Masberg ◽  
C. Ernst ◽  
G. M. Schneider ◽  
A. Würflinger ◽  
R. Dąbrowski

Abstract The phase behaviour of a new liquid crystal, belonging to the series l-[4-n-alkyl-biphenyl]-2-[4-isothio-cyanato-phenyl]ethane (nTPEB), n = 10, has been investigated with differential scanning calorimetry at ambient and high pressure. The phase behaviour depends on the thermal treatment. Phase transition temperatures have been determined as a function of pressure up to 300 MPa. No pressure-induced or pressure-limited phases are observed in this pressure range. Enthalpy-and volume-changes accompanying the phase transitions have been calculated using the Clausius-Clapeyron equation.


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