X-ray Diffraction Patterns of Liquid Crystalline Solutions of Poly-γ-benzyl-L-glutamate

Nature ◽  
1965 ◽  
Vol 206 (4984) ◽  
pp. 616-617 ◽  
Author(s):  
D. A. D. PARRY ◽  
A. ELLIOTT
2014 ◽  
Vol 18 (01n02) ◽  
pp. 139-148 ◽  
Author(s):  
Buket S. Erdoğan ◽  
Devrim Atilla ◽  
Ayşe G. Gürek ◽  
Vefa Ahsen

Methylene-bridged tetra- and octa-alkylthia substituted metal free- and Ni ( II ) phthalocyanines were synthesized from the corresponding phthalonitrile derivatives in the presence of the anhydrous metal salt ( NiCl 2) or a strong organic base. The new compounds were fully characterized by elemental analyses, UV-vis, IR, NMR and mass spectra. The mesogenic properties of these materials were studied by differential scanning calorimetry, optical microscopy and X-ray diffraction investigations. X-ray diffraction patterns of the mesophase confirmed that the tetra- and the octa-substituted compounds formed hexagonal columnar mesophases (Colh). The mesogenic properties of these compounds were compared to that of their octa alkythia substituted phthalocyanine derivatives in the literature.


1976 ◽  
Vol 54 (10) ◽  
pp. 1074-1078 ◽  
Author(s):  
B. D. McKersie ◽  
J. E. Thompson ◽  
J. K. Brandon

Smooth microsomal membranes were isolated from bean cotyledons at various intervals after planting. Wide-angle x-ray diffraction patterns were recorded at room temperature from oriented specimens of the membranes. Patterns for membranes from 2-day-old cotyledons featured a broad lipid reflection centered about a Bragg spacing of 4.6 Å. This diffraction band derives from the apolar hydrocarbon chains of the membrane phospholipid, and its diffuse nature indicates that these hydrocarbons are in a disordered liquid–crystalline state. By day 4 in the germination sequence a faint sharp band superimposed on the broad lipid reflection was discernable at a Bragg spacing of 4.15 Å. This sharp reflection represents lipid in an ordered, crystalline state and derives from a close hexagonal packing of the hydrocarbon chains. During the later stages of germination the 4.15-Å reflection intensified to the point of becoming very pronounced in patterns for membranes from 9-day-old cotyledons. These patterns also displayed a sharp but weaker reflection at 3.75 Å, which derives from an orthorhombic packing of the hydrocarbon chains in crystalline lipid. By 9 days of age the cotyledons were extensively senescent and beginning to abscise.The data indicate that senescence of membranes involves a phase change whereby the proportion of crystalline to liquid– crystalline lipid progressively increases. This changed physical state of the lipid represents a substantial decrease in membrane fluidity and may well contribute to loss of membrane function in senescing membranes.


1996 ◽  
Vol 351 (1344) ◽  
pp. 1205-1222 ◽  

The egg case of the dogfish, Scyliorhinus canicula is a composite material largely constructed from collagen fibrils. It is formed as a drawn extrusion from transverse rows of spinnerets within the lining of the nidamental gland. In the L 2 layer, which forms over 90% of the thickness of the marginal rib, each spinneret extrudes a flattened ribbon which runs the length of the rib and measures approximately 150 x 8.5 μm in cross section. The structure of these ribbons and the orientation of collagen molecules and fibrils within them has been investigated in a correlative study using: low angle x-ray diffraction; bright field microscopy of peeled preparations; transmission (TEM) and scanning (SEM) electron microscopy; confocal and quantitative polarizing microscopy. The way in which the molecular orientations are defined within the spinneret has been followed by SEM of fixed material from actively secreting nidamental glands. The extruded ribbon showed a predominantly biaxial fibril orientation in low angle x-ray diffraction patterns recorded with the beam passing horizontally through the marginal rib. This x-ray pattern is derived from a remarkably regular parabolic arrangement of fibrils superficially resembling that seen in biological twisted nematic liquid crystals. However, evidence is presented here that the arrangement in the marginal rib is novel, apparently arising from authentically curved fibres showing a splayed- or bent- rather than twisted-nematic construction. Evidence is also presented that the spinnerets are able to control molecular orientations in a nematic liquid crystal to produce this and the other arrangements seen in the egg case.


Author(s):  
T. Gulik-Krzywicki ◽  
M.J. Costello

Freeze-etching electron microscopy is currently one of the best methods for studying molecular organization of biological materials. Its application, however, is still limited by our imprecise knowledge about the perturbations of the original organization which may occur during quenching and fracturing of the samples and during the replication of fractured surfaces. Although it is well known that the preservation of the molecular organization of biological materials is critically dependent on the rate of freezing of the samples, little information is presently available concerning the nature and the extent of freezing-rate dependent perturbations of the original organizations. In order to obtain this information, we have developed a method based on the comparison of x-ray diffraction patterns of samples before and after freezing, prior to fracturing and replication.Our experimental set-up is shown in Fig. 1. The sample to be quenched is placed on its holder which is then mounted on a small metal holder (O) fixed on a glass capillary (p), whose position is controlled by a micromanipulator.


Author(s):  
J. P. Robinson ◽  
P. G. Lenhert

Crystallographic studies of rabbit Fc using X-ray diffraction patterns were recently reported. The unit cell constants were reported to be a = 69. 2 A°, b = 73. 1 A°, c = 60. 6 A°, B = 104° 30', space group P21, monoclinic, volume of asymmetric unit V = 148, 000 A°3. The molecular weight of the fragment was determined to be 55, 000 ± 2000 which is in agreement with earlier determinations by other methods.Fc crystals were formed in water or dilute phosphate buffer at neutral pH. The resulting crystal was a flat plate as previously described. Preparations of small crystals were negatively stained by mixing the suspension with equal volumes of 2% silicotungstate at neutral pH. A drop of the mixture was placed on a carbon coated grid and allowed to stand for a few minutes. The excess liquid was removed and the grid was immediately put in the microscope.


2020 ◽  
Vol 86 (6) ◽  
pp. 29-35
Author(s):  
V. P. Sirotinkin ◽  
O. V. Baranov ◽  
A. Yu. Fedotov ◽  
S. M. Barinov

The results of studying the phase composition of advanced calcium phosphates Ca10(PO4)6(OH)2, β-Ca3(PO4)2, α-Ca3(PO4)2, CaHPO4 · 2H2O, Ca8(HPO4)2(PO4)4 · 5H2O using an x-ray diffractometer with a curved position-sensitive detector are presented. Optimal experimental conditions (angular positions of the x-ray tube and detector, size of the slits, exposure time) were determined with allowance for possible formation of the impurity phases during synthesis. The construction features of diffractometers with a position-sensitive detector affecting the profile characteristics of x-ray diffraction peaks are considered. The composition for calibration of the diffractometer (a mixture of sodium acetate and yttrium oxide) was determined. Theoretical x-ray diffraction patterns for corresponding calcium phosphates are constructed on the basis of the literature data. These x-ray diffraction patterns were used to determine the phase composition of the advanced calcium phosphates. The features of advanced calcium phosphates, which should be taken into account during the phase analysis, are indicated. The powder of high-temperature form of tricalcium phosphate strongly adsorbs water from the environment. A strong texture is observed on the x-ray diffraction spectra of dicalcium phosphate dihydrate. A rather specific x-ray diffraction pattern of octacalcium phosphate pentahydrate revealed the only one strong peak at small angles. In all cases, significant deviations are observed for the recorded angular positions and relative intensity of the diffraction peaks. The results of the study of experimentally obtained mixtures of calcium phosphate are presented. It is shown that the graphic comparison of experimental x-ray diffraction spectra and pre-recorded spectra of the reference calcium phosphates and possible impurity phases is the most effective method. In this case, there is no need for calibration. When using this method, the total time for analysis of one sample is no more than 10 min.


1985 ◽  
Vol 50 (10) ◽  
pp. 2139-2145
Author(s):  
Alexander Muck ◽  
Eva Šantavá ◽  
Bohumil Hájek

The infrared spectra and powder X-ray diffraction patterns of polycrystalline YPO4-YCrO4 samples are studied from the point of view of their crystal symmetry. Mixed crystals of the D4h19 symmetry are formed over the region of 0-30 mol.% YPO4 in YCrO4. The Td → D2d → D2 or C2v(GS eff) correlation is appropriate for both PO43- and CrO43- anions.


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