scholarly journals STRUCTURAL UNITS OF STARCH DETERMINED BY X-RAY CRYSTAL STRUCTURE METHOD

1923 ◽  
Vol 5 (6) ◽  
pp. 757-776 ◽  
Author(s):  
O. L. Sponsler

A few brief statements summarizing the foregoing conclusions may make a picture of the structure of the starch grain somewhat clearer. 1. The presence of lines on the negatives indicates a regular arrangement of the planes of atoms. 2. The lines are in close agreement with lines which would be produced by a lattice of the tetragonal system, the elementary cell of which is a square prism with the dimensions 5.94 x 5.94 x 5.05 Å.u. 3. The unit of the lattice occupies a space equal to the volume of the starch group, C6H10O5. 4. The large number of atoms in the unit makes it highly probable that principal planes and secondary planes of atoms occur for every reflecting position. 5. The effect of the secondary upon the principal planes may readily account for the differences in the density of the lines produced on the negatives. 6. From theoretical considerations, reflections, such as those obtained, would occur if starch grains were built up of concentric layers of units. 7. Two other factors which might affect the density of the lines are thermal agitation and the curvature of the concentric layers. 8. A model of the starch group was constructed to scale based on the accepted sizes of the atoms involved and upon rather meager chemical evidence. The model apparently fulfills the requirements necessary to produce reflections such as were obtained. 9. The model fits the elementary cell loosely enough to suggest a low density and to allow for considerable thermal movement. At the same time, parts of it approach the faces of the cell closely enough to make cohesion seem possible. 10. The model makes clearer the basis for the assumption that reflection from certain positions would be stronger than from others. If the interpretation of the data is correct and if the assumptions made are sound, then the starch grain is built up of units arranged in concentric layers, and the units are groups of atoms, each containing 6 carbon, 10 hydrogen, and 5 oxygen atoms. Such a structure is certainly not an amorphous structure, and on the other hand it is not crystalline in the common sense of the term. Parts of the grain, it is true, act as crystals in that for certain distances the layers of units are in planes, but taken as a whole the layers are curved. As to the validity of the conclusions, those pertaining to the type of lattice and to the size of the unit may be accepted as sound in our present knowledge of x-rays and crystal structure; those, however, pertaining to the nature and the spherical arrangement of the units, while they seem convincing, need the support of further investigation into the various structures deposited by living protoplasm. In conclusion, the assumption that the units form a sort of spherical space lattice, gives a picture of the starch grain which leads us to ponder over the nature of the activity in protoplasm when it is depositing solid substances. Starch, cellulose, and pectic bodies are about the only solid deposits made directly by the living substance of plants, and all three have the same proportional formula, C6H10O5. Investigations, as yet incomplete, indicate that cellulose also consists of a regular arrangement of C6H10O5 groups, each acting as a unit, but the spacing (6.14 x 6.14 x 5.55) is slightly different from that of starch. Pectin has not been studied. Protoplasm may be thought of as being composed of molecules of many different sizes, polypeptides, or even proteins forming the larger, and amino-acids the smaller, if water and electrolytes are ignored. The smaller molecules, such as those of the amino-acid, leucine, are approximately equal in size to the C6H10O5 group of starch. That being the case, what can be the state of affairs at the interface when the starch particles are being deposited? Is it probable that protoplasm is homogeneous to the extent of being able to deposit these particles at 6 Å.u. intervals? From quite another view-point a clear picture of the units of structure and their arrangement in cellulose should give a new point of attack on the many problems connected with osmosis. And from still a different view-point, it might lead perhaps, to a solution of problems connected with swelling. Another line of thought is suggested by the uniformity of the groups in the starch grain. Since the C6H10O5 group occurs as an individual unit, one is inclined to suspect that it is really the molecule. Generally the starch molecule is considered to be very large, to be composed of several dozens of such groups, and to have a molecular weight of 7,000 or much more. No one figure, however, seems satisfactory to the different authorities. There is already at hand considerable evidence which will be assembled in a later paper favoring the single group, C6H10O5, as the molecule. Finally, problems in polarized light may receive more satisfactory explanations through a clearer notion of the molecular structure of the carbohydrates.

Author(s):  
Jenny Pickworth Glusker ◽  
Kenneth N. Trueblood

This book aims to explain how and why the detailed three-dimensional architecture of molecules can be determined by an analysis of the diffraction patterns obtained when X rays or neutrons are scattered by the atoms in single crystals. Part 1 deals with the nature of the crystalline state, diffraction generally, and diffraction by crystals in particular, and, briefly, the experimental procedures that are used. Part II examines the problem of converting the experimentally obtained data into a model of the atomic arrangement that scattered these beams. Part III is concerned with the techniques for refining the approximate structure to the degree warranted by the experimental data. It also describes the many types of information that can be learned by modern crystal structure analysis. There is a glossary of terms used and several appendixes to which most of the mathematical details have been relegated.


Author(s):  
David C. Joy

In a crystalline solid the regular arrangement of the lattice structure influences the interaction of the incident beam with the specimen, leading to changes in both the transmitted and backscattered signals when the angle of incidence of the beam to the specimen is changed. For the simplest case the electron flux inside the specimen can be visualized as the sum of two, standing wave distributions of electrons (Fig. 1). Bloch wave 1 is concentrated mainly between the atom rows and so only interacts weakly with them. It is therefore transmitted well and backscattered weakly. Bloch wave 2 is concentrated on the line of atom centers and is therefore transmitted poorly and backscattered strongly. The ratio of the excitation of wave 1 to wave 2 varies with the angle between the incident beam and the crystal structure.


Author(s):  
Matthew Wilding ◽  
Colin Scott ◽  
Thomas S. Peat ◽  
Janet Newman

The NAD-dependent malonate-semialdehyde dehydrogenase KES23460 fromPseudomonassp. strain AAC makes up half of a bicistronic operon responsible for β-alanine catabolism to produce acetyl-CoA. The KES23460 protein has been heterologously expressed, purified and used to generate crystals suitable for X-ray diffraction studies. The crystals belonged to space groupP212121and diffracted X-rays to beyond 3 Å resolution using the microfocus beamline of the Australian Synchrotron. The structure was solved using molecular replacement, with a monomer from PDB entry 4zz7 as the search model.


1. The nature of X-rays X-rays were discovered in 1895 by Rontgen in Wurtzburg. For the next 17 years the nature of these rays was one of the dominant questions in physics: were they particles or were they waves? W.H. Bragg, of Adelaide, found indisputable evidence that they were particles; C.G. Barkla, of Liverpool and Edinburgh, found even more indisputable evidence that they were waves. The decisive experiment was carried out by Friedrich and Knipping (1) in 1912 in Munich, under the guidance of von Laue; they passed a fine beam of X-rays through a crystal of copper sulphate, hoping that it would behave as a diffraction grating. It did! The background was emotionally described bv von Laue in 1948 (2). * W.H. Bragg had a son, W.L. Bragg, who was a research student under J.J. Thomson at Cambridge. He was, as he himself said later, rather upset that his father seemed to have been proved wrong, and he tried to think up an alternative explanation of particles travelling through tunnels in the crystal. But he soon realized that the wave explanation had to be accepted.


Minerals ◽  
2018 ◽  
Vol 8 (8) ◽  
pp. 311 ◽  
Author(s):  
Carlotta Giacobbe ◽  
Jonathan Wright ◽  
Dario Di Giuseppe ◽  
Alessandro Zoboli ◽  
Mauro Zapparoli ◽  
...  

Nowadays, due to the adverse health effects associated with exposure to asbestos, its removal and thermal inertization has become one of the most promising ways for reducing waste risk management. Despite all the advances in structure analysis of fibers and characterization, some problems still remain that are very hard to solve. One challenge is the structure analysis of natural micro- and nano-crystalline samples, which do not form crystals large enough for single-crystal X-ray diffraction (SC-XRD), and their analysis is often hampered by reflection overlap and the coexistence of multiple fibres linked together. In this paper, we have used nano-focused synchrotron X-rays to refine the crystal structure of a micrometric tremolite fibres from Val d’Ala, Turin (Italy) after various heat treatment. The structure of the original fibre and after heating to 800 °C show minor differences, while the fibre that was heated at 1000 °C is recrystallized into pyroxene phases and cristobalite.


2012 ◽  
Vol 727-728 ◽  
pp. 1585-1590
Author(s):  
Neuza Evangelista ◽  
Jorge Alberto Soares Tenório ◽  
José Roberto Oliveira ◽  
Paulo R. Borges ◽  
Taiany Coura M. Ferreira

Ceramic fibers are characterized by their light weight, high degree of purity, low heat storage, low thermal conductivity, thermal shock resistance and superior corrosion resistance in high-temperature environments. In addition, they can be produced extensively in substitution to all materials used in the coating of almost all heating equipment as well as contributing to the reduction of energy consumption. Such characteristics make them ideal in the coating of distributors, mufflers, heating ovens, among others, as highly demanded by the mining and metallurgical industries, among others. After use in the process of industrial production, generated waste will lose their insulation capacity and thus require safe disposal. The present work focuses specifically on ceramic and glass wools aiming at an evaluation of their recycling prospect of incorporation into cement mortars and concrete. This residues were pulverized and displayed ~30µm average particle size. The scan electronic microscopy (SEM) presented elongated, thin and straight particles, which is very different than flocular structure of cement. The X-rays diffraction revealed amorphous structure for glass wool and crystalline structure for ceramics wool. The chemical analysis showed high concentrations of Al2O3 and silica in both residues, with higher percentage of calcium oxide in glass wool.


The solid phase of the compound 2'-methoxy-2 : 4 : 4 : 7 : 4'- pentamethylflavan differs in many respects from normally crystalline materials, yet is not amorphous. It tends to form spherical masses which exhibit no regular crystal boundaries, even when seen under the microscope. The solid melts over a range of up to 3° C and the actual temperatures at which melting begins and ends vary according to the thermal treatment previously received by the specimen. The temperature at which the melt starts to solidify on cooling is always several degrees below the melting range; this is not due to normal supercooling. Solidification from the melt presents several other interesting features, including some rhythmic effects. Variations in the external conditions during solidification can give rise to three superficially different forms of the solid phase. The solid-liquid and liquid-solid transitions have been followed by measurements of density, rigidity and dielectric constant, all of which give further indications of the diffuse nature of the melting process and the existence of hysteresis between melting and solidifica­tion. These effects recall the behaviour of some crystalline high polymers and examination of solid methoxypentamethylflavan by polarized light, X-rays and electron microscopy has revealed further analogies with such materials. It is tentatively concluded that the solid is composed of submicroscopic crystalline regions which are organized into larger spherulitic aggregates, but no definite explanations of the failure of the compound to form macroscopic crystals or of the similarities between it and polymers seem possible at present.


2011 ◽  
Vol 67 (6) ◽  
pp. 535-551 ◽  
Author(s):  
David A. Bardwell ◽  
Claire S. Adjiman ◽  
Yelena A. Arnautova ◽  
Ekaterina Bartashevich ◽  
Stephan X. M. Boerrigter ◽  
...  

Following on from the success of the previous crystal structure prediction blind tests (CSP1999, CSP2001, CSP2004 and CSP2007), a fifth such collaborative project (CSP2010) was organized at the Cambridge Crystallographic Data Centre. A range of methodologies was used by the participating groups in order to evaluate the ability of the current computational methods to predict the crystal structures of the six organic molecules chosen as targets for this blind test. The first four targets, two rigid molecules, one semi-flexible molecule and a 1:1 salt, matched the criteria for the targets from CSP2007, while the last two targets belonged to two new challenging categories – a larger, much more flexible molecule and a hydrate with more than one polymorph. Each group submitted three predictions for each target it attempted. There was at least one successful prediction for each target, and two groups were able to successfully predict the structure of the large flexible molecule as their first place submission. The results show that while not as many groups successfully predicted the structures of the three smallest molecules as in CSP2007, there is now evidence that methodologies such as dispersion-corrected density functional theory (DFT-D) are able to reliably do so. The results also highlight the many challenges posed by more complex systems and show that there are still issues to be overcome.


1968 ◽  
Vol 49 (12) ◽  
pp. 5438-5444 ◽  
Author(s):  
M. P. Marzocchi ◽  
P. Manzelli ◽  
V. Schettino ◽  
S. Califano

1957 ◽  
Vol 1 ◽  
pp. 483-494
Author(s):  
Selby E. Summers

AbstractThe X-ray microscope is an electrostatic optical instrument employing X-rays for shadow projection to magnify and reveal detailed internal structure of specimens opaque to light or electrons. Its many advantages — high resolving power, greater penetration, large depth of field, and stereographic presentation — make the X-ray Microscope a versatile instrument for industrial research and development. Because the instrument was recently introduced, little information is available on specimen preparation techniques, or types of specimens suitable for study. A few of the many possible applications will be discussed, as well as a brief review of the technical details of the instrument.


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