Helium Path Diffractometry and its Application to Determination of Retained Austenite and Macrostress in Steel

1962 ◽  
Vol 6 ◽  
pp. 85-90
Author(s):  
Robert A. McCune

AbstractThe helium X-ray path has long been used, in spectrography to increase the intensity of the long-wavelength X-rays. The same principle has been applied to diflractometry. Up to threefold intensity increase is observed with chromium Ka radiation with very little increase In background. The peak to background ratio, therefore, is Improved by almost the same factor as the increase in intensity. Application of the technique is illustrated by analysis of gauge block steel for retained austcnite and macrostress.

IUCrJ ◽  
2019 ◽  
Vol 6 (3) ◽  
pp. 373-386 ◽  
Author(s):  
Shibom Basu ◽  
Vincent Olieric ◽  
Filip Leonarski ◽  
Naohiro Matsugaki ◽  
Yoshiaki Kawano ◽  
...  

Native single-wavelength anomalous dispersion (SAD) is an attractive experimental phasing technique as it exploits weak anomalous signals from intrinsic light scatterers (Z < 20). The anomalous signal of sulfur in particular, is enhanced at long wavelengths, however the absorption of diffracted X-rays owing to the crystal, the sample support and air affects the recorded intensities. Thereby, the optimal measurable anomalous signals primarily depend on the counterplay of the absorption and the anomalous scattering factor at a given X-ray wavelength. Here, the benefit of using a wavelength of 2.7 over 1.9 Å is demonstrated for native-SAD phasing on a 266 kDa multiprotein-ligand tubulin complex (T2R-TTL) and is applied in the structure determination of an 86 kDa helicase Sen1 protein at beamline BL-1A of the KEK Photon Factory, Japan. Furthermore, X-ray absorption at long wavelengths was controlled by shaping a lysozyme crystal into spheres of defined thicknesses using a deep-UV laser, and a systematic comparison between wavelengths of 2.7 and 3.3 Å is reported for native SAD. The potential of laser-shaping technology and other challenges for an optimized native-SAD experiment at wavelengths >3 Å are discussed.


1968 ◽  
Vol 12 ◽  
pp. 518-533 ◽  
Author(s):  
Y. Gohshi

AbstractA simple two-crystal spectrometer was constructed, making use of a commercial one-crystal spectrometer. A detector attached to a 2θ-arm has been replaced by a second crystal. After adjustment, the second crystal is fixed to the 2θ-arm. The detector is placed at an appropriate position apart from the 2θ-arm. The spectrometer is operated as if it were a one-crystal spectrometer. The dispersion of the spectrometer in this mode of operation is the sum of those of the first and second crystals. Ge(220) crystals gave the best resolution which was about 3-3 eV fwhm for Cu Kα1. The strongest Intensity was observed using etched LIF crystals. The intensity was about 1/4 of that of a one-crystal spectrometer and the resolution was about 9.5 eV fwhm for Cu Kα1. The spectrometer was applied to the determination of hafnium in zirconium and sircaloy. The Zr Kα 2nd order line, which coincides with the Hf Lα1 line, was completely eliminated by successive reflections by Ge(111) crystals owing to the extinction rule and the high resolving power. The detection limit was about 7 ppm of hafnium. Another example is the separation of the As Kα2 line from the Pb Lα1 line. Arsenic in low alloy steel was determined without the correction for the well known Interference of lead. The very common interference of Cr Kβ on Mn Kα was also eliminated completely by this spectrometer. Though the spectrometer is not very suitable for a wide wavelength range spectroscopic measurement, owing to its narrow window region (about ±1°), the chemical effects on Kg spectra of sulfur in various compounds were investigated. Fine structures were found In the sulfur Kβ spectra of several thiocyanates and elemental sulfur. To observe long wavelength region spectra, the X-ray path of the spectrometer was modified to a hybrid path (vacuum and helium).


Author(s):  
J N Chapman ◽  
W A P Nicholson

Energy dispersive x-ray microanalysis (EDX) is widely used for the quantitative determination of local composition in thin film specimens. Extraction of quantitative data is usually accomplished by relating the ratio of the number of atoms of two species A and B in the volume excited by the electron beam (nA/nB) to the corresponding ratio of detected characteristic photons (NA/NB) through the use of a k-factor. This leads to an expression of the form nA/nB = kAB NA/NB where kAB is a measure of the relative efficiency with which x-rays are generated and detected from the two species.Errors in thin film x-ray quantification can arise from uncertainties in both NA/NB and kAB. In addition to the inevitable statistical errors, particularly severe problems arise in accurately determining the former if (i) mass loss occurs during spectrum acquisition so that the composition changes as irradiation proceeds, (ii) the characteristic peak from one of the minority components of interest is overlapped by the much larger peak from a majority component, (iii) the measured ratio varies significantly with specimen thickness as a result of electron channeling, or (iv) varying absorption corrections are required due to photons generated at different points having to traverse different path lengths through specimens of irregular and unknown topography on their way to the detector.


Crystals ◽  
2018 ◽  
Vol 8 (7) ◽  
pp. 273 ◽  
Author(s):  
José Brandão-Neto ◽  
Leonardo Bernasconi

Macromolecular crystallography at cryogenic temperatures has so far provided the majority of the experimental evidence that underpins the determination of the atomic structures of proteins and other biomolecular assemblies by means of single crystal X-ray diffraction experiments. One of the core limitations of the current methods is that crystal samples degrade as they are subject to X-rays, and two broad groups of effects are observed: global and specific damage. While the currently successful approach is to operate outside the range where global damage is observed, specific damage is not well understood and may lead to poor interpretation of the chemistry and biology of the system under study. In this work, we present a phenomenological model in which specific damage is understood as the result of a single process, the steady excitation of crystal electrons caused by X-ray absorption, which acts as a trigger for the bulk effects that manifest themselves in the form of global damage and obscure the interpretation of chemical information from XFEL and synchrotron structural research.


Author(s):  
José Brandão-Neto ◽  
Leonardo Bernasconi

Macromolecular crystallography at cryogenic temperatures has so far provided the majority of the experimental evidence that underpins the determination of the atomic structures of proteins and other biomolecular assemblies by means of single crystal X-ray diffraction experiments. One of the core limitations of the current methods is that crystal samples degrade as they are subject to X-rays, and two broad groups of effects are observed: global and specific damage. While the currently successful approach is to operate outside the range where global damage is observed, specific damage is not well understood and may lead to poor interpretation of the chemistry and biology of the system under study. In this work, we present a phenomenological model in which specific damage is understood as the result of a single process, the steady excitation of crystal electrons caused by X-ray absorption, which acts as a trigger for the bulk effects that manifest themselves in the form of global damage and obscure the interpretation of chemical information from XFEL and synchrotron structural research.


The measurement of the intensity of an X-ray beam in absolute units is in theory most satisfactorily accomplished by a determination of its heating effect. The method, however, is attended by considerable experimental difficulties, so that its application is very limited, and in practice it is usual to replace it by a determination of the ionization produced when the beam is passed through a gas. To correlate the ionization with an absolute intensity requires a quantitative knowledge of the details of the interaction between the X-rays and the molecules concerned and of the ionization of the gas by the ejected electrons. It sometimes happens that the processes involved about which we know least are relatively unimportant, so that a fairly reliable correlation can be made; and much work has been done on the application of the ionization method to X-ray dosimetry. But in general a quantitative correlation between ionization and intensity is not possible. A further study of the ionization of gases by X-rays is therefore desirable; moreover it may be made to yield important information concerning the processes involved. The early development of the physics of X-rays contains many examples of this, and more recently an important contribution has been made by Stockmeyer. The events leading to the ionization of a heavy gas are exceedingly complicated, whereas in the light gases (hydrogen and helium) some of these events are absent or else occur to a negligible extent, so that the interpretation of experiments with the latter becomes simpler and more reliable. These gases are therefore specially worthy of study. Moreover, for them the application of quantum mechanics leads to the most definite results for comparison with experiment, and in particular permits of a direct test of some aspects of Dirac’s theory of recoil scattering. The ionization due to the gas itself is, however, very small, and may even be less than the secondary ionization due to electrons liberated from the chamber walls. The technique used in ionization measurements with heavy gases is therefore unsuitable. Hitherto the only attempt made to extend such measurements to light gases is an experiment carried out in 1915 on hydrogen by Shearer who, however, obtained very variable results and an ionization markedly smaller than that to be expected from recoil electrons alone. Moreover his experimental method is now open to criticism in view of our greater knowledge of X-rays, and in particular the fluorescent radiation used was of doubtful homogeneity. The present paper will describe a new technique suitable for quantitative measurements of the ionization produced by X-rays in light gases, and in another paper it will be applied to a re-investigation of hydrogen.


1926 ◽  
Vol 22 (5-6) ◽  
pp. 737
Author(s):  
I. Friedland

Arikhbaev (Vesti. Khir., 1926, book 17-18), having established the normal state of the lipolytic index in 30 people with various diseases and then proceeding to the determination of lipase in the blood of 9 various patients and 1 healthy subject exposed to irritating doses of X-ray rays on the adrenal gland, which caused its hyperfunction, finished his research by observing 5 patients with various forms of surgical tuberculosis, of whom three underwent simultaneous x-rays of the adrenal glands with subcutaneous injections of fish oil neutralized from fatty acids, one - only injections of neutralized fish oil and one - only an operational aid.


Author(s):  
Marc de Boissieu ◽  
Sonia Francoual

AbstractWe review results obtained in the study of the diffuse scattering in the i-AlPdMn quasicrystal. Most of the diffuse scattering is the result of long wavelength phason modes. The shape and intensity distribution of the diffuse scattering is well reproduced using the generalised elasticity theory and two phason elastic constants. The temperature dependence of the diffuse scattering indicates a softening of the phason elastic constant as the temperature is lowered. Using coherent X-rays and photo-correlation X-ray spectroscopy, it is shown that phason modes are collective diffusive modes, in agreement with the hydrodynamic theory of long wavelength fluctuations in quasicrystals.


2008 ◽  
Vol 4 (S256) ◽  
pp. 20-29 ◽  
Author(s):  
Yaël Nazé

AbstractIn the study of stars, the high energy domain occupies a place of choice, since it is the only one able to directly probe the most violent phenomena: indeed, young pre-main sequence objects, hot massive stars, or X-ray binaries are best revealed in X-rays. However, previously available X-ray observatories often provided only crude information on individual objects in the Magellanic Clouds. The advent of the highly efficient X-ray facilities XMM-Newton and Chandra has now dramatically increased the sensitivity and the spatial resolution available to X-ray astronomers, thus enabling a fairly easy determination of the properties of individual sources in the LMC.


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