The X-Ray Diagram of a Buna-S Vulcanizate

1945 ◽  
Vol 18 (1) ◽  
pp. 20-21
Author(s):  
Ross E. Morris ◽  
Charles B. Jordan

Abstract Sebrell and Dinsmore (India Rubber World 103, 37 (1944); Rubber Chem. Tech. 16, 857 (1943)) found that the x-ray diffraction pattern of Buna-S consists of a broad halo similar to that obtained with liquids. This type of pattern was obtained whether the Buna-S was unstretched or stretched. Unstretched natural rubber gives a similar pattern, but stretched natural rubber gives a characteristic fiber pattern. This fiber pattern demonstrates the existence of three-dimensional crystallites. Buna-S would not be expected to yield a fiber diagram while stretched because the molecules of this synthetic rubber are probably not constructed in a regular fashion. The styrene residues are presumably distributed at random along the length of the molecule, and there may be side-chains which branch off the main chain. However, when considerably stretched, a Buna-S vulcanizate would be expected to exhibit some indication in its x-ray diagram that alignment of the molecules has occurred.

1952 ◽  
Vol 25 (2) ◽  
pp. 258-264 ◽  
Author(s):  
V. I. Kasatochkin ◽  
B. V. Lukin

Abstract The potentialities of x-ray analysis of the molecular structure of rubbers can be widely extended by measuring the intensities of the amorphous halo and continuous background of scattering in the diffraction patterns of unstretched test-specimens. This method can be applied to the study of the effect of repeated stretching of rubbers. Questions pertaining to the fatigue of rubbers have immense importance now in the performance of rubber products. The methods of determining the crystallization of natural rubber and of measuring the intensity of the amorphous halo for synthetic rubber were employed for investigating the changes of the molecular structure of rubber due to repeated stretching. The crystallization of raw smoked-sheet rubber decreased as a result of fatigue; a similar phenomenon was observed for its vulcanizates. The vulcanizates which were stretched less than 300 per cent lost their crystallization property altogether after fatigue, and, at greater elongations, the content of the crystalline phase greatly decreased (see Figure 1).


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

Much of our present knowledge of the architecture of molecules has been obtained from studies of the diffraction of X rays or neutrons by crystals. X rays are scattered by the electrons of atoms and ions, and the interference between the X rays scattered by the different atoms or ions. in a crystal can result in a diffraction pattern. Similarly, neutrons are scattered by the nuclei of atoms. Measurements on a crystal diffraction pattern can lead to information on the arrangement of atoms or ions within the crystal. This is the experimental technique to be described in this book. X-ray diffraction was first used to establish the three-dimensional arrangement of atoms in a crystal by William Lawrence Bragg in 1913 (Bragg, 1913), shortly after Wilhelm Conrad Röntgen had discovered X rays and Max von Laue had shown in 1912 that these X rays could be diffracted by crystals (Röntgen, 1895; Friedrich et al., 1912). Later, in 1927 and 1936 respectively, it was also shown that electrons and neutrons could be diffracted by crystals (Davisson and Germer, 1927; von Halban and Preiswerk, 1936; Mitchell and Powers, 1936). Bragg found from X-ray diffraction studies that, in crystals of sodium chloride, each sodium is surrounded by six equidistant chlorines and each chlorine by six equidistant sodiums. No discrete molecules of NaCl were found and therefore Bragg surmised that the crystal consisted of sodium ions and chloride ions rather than individual (noncharged) atoms (Bragg, 1913); this had been predicted earlier by William Barlow and William Jackson Pope (Barlow and Pope, 1907), but had not, prior to the research of the Braggs, been demonstrated experimentally. A decade and a half later, in 1928, Kathleen Lonsdale used X-ray diffraction methods to show that the benzene ring is a flat regular hexagon in which all carbon–carbon bonds are equal in length, rather than a ring structure that contains alternating single and double bonds (Lonsdale, 1928).Her experimental result, later confirmed by spectroscopic studies (Stoicheff, 1954), was of great significance in chemistry.


Dichroism has been observed in the infra-red spectrum of a single crystal of ribonuclease. The dichroism suggests that the crystal contains folded polypeptide chains whose direction is mainly along or near that of the c axis, in agreement with conclusions arrived at by Carlisle & Scouloudi from consideration of the X-ray diffraction pattern. A band ascribed to the N—H vibration of the amide groups in the side chains has been found to be dichroic, and this appears to show that the plane of the NH 2 group in the side chain amides is oriented parallel to the b axis of the crystal.


1932 ◽  
Vol 5 (1) ◽  
pp. 7-29
Author(s):  
Wallace H. Carothers ◽  
Ira Williams ◽  
Arnold M. Collins ◽  
James E. Kirby

Abstract Chloro-2-butadiene-1,3 (chloroprene) is described and its structure established through reactions leading to its conversion into butane-α, β,γ,δ-tetracarboxylic acid, and into β-chloroanthraquinone. Within ten days under ordinary conditions in a closed vessel containing a little air, chloroprene spontaneously changes into a transparent, resilient, strong, non-plastic, elastic mass resembling vulcanized rubber. This product is called μ-polychloroprene. By interrupting the polymerization before it has proceeded to completion one obtains a soft, plastic product (α-polymer) that resembles unvulcanized rubber. Under the action of heat the α-polymer rapidly changes to the μ-polymer. Other polymers of chloroprene described are volatile (β-) polymer, granular (ω-) polymer, and balata-like polymer. The structures of the polymers are discussed as well as the effect of conditions on the formation of each type. Unlike any previously described synthetic rubbers, μ-polychloroprene resembles natural rubber in the fact that when it is stretched its x-ray diffraction pattern shows a point diagram. The transformation of chloroprene into μ-polychloroprene occurs very rapidly in aqueous emulsion. The resulting product constitutes a synthetic (vulcanized) latex. It has a much smaller particle size than natural latex and it penetrates porous materials more readily. Chloroprene can also be polymerized in the pores of porous or bibulous materials. The materials thus become intimately impregnated with synthetic rubber. Compared with natural rubber the new synthetic rubber is more dense, more resistant to absorption or penetration by water, less strongly swelled by petroleum hydrocarbons and less permeable to many gases. It is much more resistant to attack by oxygen, ozone, hydrogen chloride, hydrogen fluoride and many other chemicals.


Author(s):  
James A. Lake

The understanding of ribosome structure has advanced considerably in the last several years. Biochemists have characterized the constituent proteins and rRNA's of ribosomes. Complete sequences have been determined for some ribosomal proteins and specific antibodies have been prepared against all E. coli small subunit proteins. In addition, a number of naturally occuring systems of three dimensional ribosome crystals which are suitable for structural studies have been observed in eukaryotes. Although the crystals are, in general, too small for X-ray diffraction, their size is ideal for electron microscopy.


Author(s):  
J. M. Galbraith ◽  
L. E. Murr ◽  
A. L. Stevens

Uniaxial compression tests and hydrostatic tests at pressures up to 27 kbars have been performed to determine operating slip systems in single crystal and polycrystal1ine beryllium. A recent study has been made of wave propagation in single crystal beryllium by shock loading to selectively activate various slip systems, and this has been followed by a study of wave propagation and spallation in textured, polycrystal1ine beryllium. An alteration in the X-ray diffraction pattern has been noted after shock loading, but this alteration has not yet been correlated with any structural change occurring during shock loading of polycrystal1ine beryllium.This study is being conducted in an effort to characterize the effects of shock loading on textured, polycrystal1ine beryllium. Samples were fabricated from a billet of Kawecki-Berylco hot pressed HP-10 beryllium.


Author(s):  
Daniel C. Pease

A previous study demonstrated that tissue could be successfully infiltrated with 50% glutaraldehyde, and then subsequently polymerized with urea to create an embedment which retained cytomembrane lipids in sectioned material. As a result, the 180-190 Å periodicity characteristic of fresh, mammalian myelin was preserved in sections, as was a brilliant birefringence, and the capacity to bind OsO4 vapor in the hydrophobic bilayers. An associated (unpublished) study, carried out in co-operation with Drs. C.K. Akers and D.F. Parsons, demonstrated that the high concentration of glutaraldehyde (and urea) did not significantly alter the X-ray diffraction pattern of aldehyde-fixed, myelin. Thus, by itself, 50% glutaraldehyde has little effect upon cytomembrane systems and can be used with confidence for the first stages of dehydration.


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