scholarly journals Algorithm for Reconstruction of 3D Images of Nanorice Particles from Diffraction Patterns of Two Particles in Independent Random Orientations with an X-ray Laser

2017 ◽  
Vol 7 (7) ◽  
pp. 646 ◽  
Author(s):  
Sung Kim ◽  
Sandi Wibowo ◽  
Dilano Saldin
Keyword(s):  
X Ray ◽  
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.


Author(s):  
D J H Cockayne ◽  
D R McKenzie

The study of amorphous and polycrystalline materials by obtaining radial density functions G(r) from X-ray or neutron diffraction patterns is a well-developed technique. We have developed a method for carrying out the same technique using electron diffraction in a standard TEM. It has the advantage that studies can be made of thin films, and on regions of specimen too small for X-ray and neutron studies. As well, it can be used to obtain nearest neighbour distances and coordination numbers from the same region of specimen from which HREM, EDS and EELS data is obtained.The reduction of the scattered intensity I(s) (s = 2sinθ/λ ) to the radial density function, G(r), assumes single and elastic scattering. For good resolution in r, data must be collected to high s. Previous work in this field includes pioneering experiments by Grigson and by Graczyk and Moss. In our work, the electron diffraction pattern from an amorphous or polycrystalline thin film is scanned across the entrance aperture to a PEELS fitted to a conventional TEM, using a ramp applied to the post specimen scan coils. The elastically scattered intensity I(s) is obtained by selecting the elastically scattered electrons with the PEELS, and collecting directly into the MCA. Figure 1 shows examples of I(s) collected from two thin ZrN films, one polycrystalline and one amorphous, prepared by evaporation while under nitrogen ion bombardment.


Author(s):  
Karimat El-Sayed

Lead telluride is an important semiconductor of many applications. Many Investigators showed that there are anamolous descripancies in most of the electrophysical properties of PbTe polycrystalline thin films on annealing. X-Ray and electron diffraction studies are being undertaken in the present work in order to explain the cause of this anamolous behaviour.Figures 1-3 show the electron diffraction of the unheated, heated in air at 100°C and heated in air at 250°C respectively of a 300°A polycrystalline PbTe thin film. It can be seen that Fig. 1 is a typical [100] projection of a face centered cubic with unmixed (hkl) indices. Fig. 2 shows the appearance of faint superlattice reflections having mixed (hkl) indices. Fig. 3 shows the disappearance of thf superlattice reflections and the appearance of polycrystalline PbO phase superimposed on the [l00] PbTe diffraction patterns. The mechanism of this three stage process can be explained on structural basis as follows :


Author(s):  
B. B. Chang ◽  
D. F. Parsons

The significance of dynamical scattering effects remains the major question in the structural analysis by electron diffraction of protein crystals preserved in the hydrated state. In the few cases (single layers of purple membrane and 400-600 Å thick catalase crystals examined at 100 kV acceleration voltage) where electron-diffraction patterns were used quantitatively, dynamical scattering effects were considered unimportant on the basis of a comparison with x-ray intensities. The kinematical treatment is usually justified by the thinness of the crystal. A theoretical investigation by Ho et al. using Cowley-Moodie multislice formulation of dynamical scattering theory and cytochrome b5as the test object2 suggests that kinematical analysis of electron diffraction data with 100-keV electrons would not likely be valid for specimen thickness of 300 Å or more. We have chosen to work with electron diffraction patterns obtained from actual wet protein crystals (rat hemoglobin crystals of thickness range 1000 to 2500 Å) at 200 and 1000 kV and to analyze these for dynamical effects.


Author(s):  
T.W. Jeng ◽  
W. Chiu

With the advances in preparing biological materials in a thin and highly ordered form, and in maintaining them hydrated under vacuum, electron crystallography has become an important tool for biological structure investigation at high resolution (1,2). However, the electron radiation damage would limit the capability of recording reflections with low intensities in an electron diffraction pattern. It has been demonstrated that the use of a low temperature stage can reduce the radiation damage effect and that one can expose the specimen with a higher dose in order to increase the signal contrast (3). A further improvement can be made by selecting a proper photographic emulsion. The primary factors in evaluating the suitability of photographic emulsion for recording low dose diffraction patterns are speed, fog level, electron response at low electron exposure, linearity, and usable range of exposure. We have compared these factors with three photographic emulsions including Kodak electron microscopic plate (EMP), Industrex AA x-ray film (AA x-ray) and Kodak nuclear track film (NTB3).


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.


1987 ◽  
Vol 52 (1) ◽  
pp. 93-102 ◽  
Author(s):  
Jaroslav Vinš ◽  
Jan Šubrt ◽  
Vladimír Zapletal ◽  
František Hanousek

A method has been worked out for the reproducible preparation of Green Rust substances involving SO42-, Cl-, Br-, and I- anions. The chemical composition of the substances prepared has been followed in dependence on the synthesis conditions. The powder X-ray and electron diffraction patterns and infrared and Moessbauer spectra have been measured and discussed.


Materials ◽  
2021 ◽  
Vol 14 (9) ◽  
pp. 2207
Author(s):  
Żaneta Garczyk ◽  
Zbigniew Jaegermann ◽  
Piotr Duda ◽  
Andrzej S. Swinarew ◽  
Sebastian Stach

The main aim of this study was to analyze microtomographic data to determine the geometric dimensions of a ceramic porous material’s internal structure. Samples of a porous corundum biomaterial were the research material. The samples were prepared by chemical foaming and were measured using an X-ray scanner. In the next stage, 3D images of the samples were generated and analyzed using Thermo Scientific Avizo software. The analysis enabled the isolation of individual pores. Then, the parameters characterizing the pore geometry and the porosity of the samples were calculated. The last part of the research consisted of verifying the developed method by comparing the obtained results with the parameters obtained from the microscopic examinations of the biomaterial. The comparison of the results confirmed the correctness of the developed method. The developed methodology can be used to analyze biomaterial samples to assess the geometric dimensions of biomaterial pores.


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