X-Ray Diffractometry of Low-Mass Samples

1987 ◽  
Vol 2 (2) ◽  
pp. 78-81 ◽  
Author(s):  
L. S. Zevin ◽  
I. M. Zevin

AbstractThe intensity diffracted by a low-mass sample with negligible absorption may be expressed as It = I∞ (B/2μ*)/G, where I∞ = intensity diffracted by a bulk sample, B = cross section of the primary beam, μ* = mass absorption coefficient, and G = mass of the sample. Measurable intensity may be obtained from samples with less than 1 μg mass. In order to improve the limit of detection, the primary beam should be collimated so as to irradiate the sample and only a minimum volume of the sample support. The optimum spreading area of a low-mass sample is S sinθ≅10μ*. Comminution of low-mass samples to 1 — 2μm particles is adequate for reasonable intensity measurements.

1983 ◽  
Vol 16 (1) ◽  
pp. 11-13
Author(s):  
B. Birknes ◽  
L. K. Hansen

A procedure for collecting protein data by a simulated step-scan method is described for a CAD4 diffractometer. The method allows one to collect 100–150 reflections per hour without any significant loss in accuracy, thus reducing the time spent on each reflection by a factor of 2–3 compared with the ω–2θ scan technique. A comparison between data collected for the protein phospholipase C by the present method and by the ω–2θ technique gives a reliability factor of 2%. Prior to this work the homogeneity of the X-ray beam from a graphite monochromator was determined, and the intensity cross section of the monochromatized X-ray beam showed that the total X-ray illumination of the crystal is practically unchanged regardless of the orientation of the crystal in the primary beam.


1985 ◽  
Vol 38 (3) ◽  
pp. 427
Author(s):  
Andrew W Stevenson ◽  
Zwi Barnea

X-ray intensity measurements have been carried out with an extended-face single crystal of hexagonal CdSe using four different wavelengths. The wavelength dependence of moderate extinction effects (y > 0�7, where y is the secondary extinction factor) was investigated by analysing the Bragg intensities using Zachariasen's (1967) theory, with and without the sin 26 factor (6 being the Bragg angle), which was claimed to have been omitted from the original expression for the diffraction cross section in a perfect crystallite (Becker and Coppens 19740, 1974 b). The resulting Hamilton (1965) R factors for the different extinction models tested do not enable one to make conclusive statements in regard to the 'best' model, but the refined values of the domain radius r and the mosaic-spread parameter g suggest that the crystal is neither of type I (Le. r > Ag, where A is the wavelength) nor of type II (Le. r < Ag). The wavelength dependence of the extinction effects is adequately accounted for in terms of the models tested.


1988 ◽  
Vol 102 ◽  
pp. 47-50
Author(s):  
K. Masai ◽  
S. Hayakawa ◽  
F. Nagase

AbstractEmission mechanisms of the iron Kα-lines in X-ray binaries are discussed in relation with the characteristic temperature Txof continuum radiation thereof. The 6.7 keV line is ascribed to radiative recombination followed by cascades in a corona of ∼ 100 eV formed above the accretion disk. This mechanism is attained for Tx≲ 10 keV as observed for low mass X-ray binaries. The 6.4 keV line observed for binary X-ray pulsars with Tx&gt; 10 keV is likely due to fluorescence outside the He II ionization front.


Author(s):  
Thomas S. Leeson ◽  
C. Roland Leeson

Numerous previous studies of outer segments of retinal receptors have demonstrated a complex internal structure of a series of transversely orientated membranous lamellae, discs, or saccules. In cones, these lamellae probably are invaginations of the covering plasma membrane. In rods, however, they appear to be isolated and separate discs although some authors report interconnections and some continuities with the surface near the base of the outer segment, i.e. toward the inner segment. In some species, variations have been reported, such as longitudinally orientated lamellae and lamellar whorls. In cross section, the discs or saccules show one or more incisures. The saccules probably contain photolabile pigment, with resulting potentials after dipole formation during bleaching of pigment. Continuity between the lamina of rod saccules and extracellular space may be necessary for the detection of dipoles, although such continuity usually is not found by electron microscopy. Particles on the membranes have been found by low angle X-ray diffraction, by low temperature electron microscopy and by freeze-etching techniques.


Author(s):  
V. V. Damiano ◽  
R. P. Daniele ◽  
H. T. Tucker ◽  
J. H. Dauber

An important example of intracellular particles is encountered in silicosis where alveolar macrophages ingest inspired silica particles. The quantitation of the silica uptake by these cells may be a potentially useful method for monitoring silica exposure. Accurate quantitative analysis of ingested silica by phagocytic cells is difficult because the particles are frequently small, irregularly shaped and cannot be visualized within the cells. Semiquantitative methods which make use of particles of known size, shape and composition as calibration standards may be the most direct and simplest approach to undertake. The present paper describes an empirical method in which glass microspheres were used as a model to show how the ratio of the silicon Kα peak X-ray intensity from the microspheres to that of a bulk sample of the same composition correlated to the mass of the microsphere contained within the cell. Irregular shaped silica particles were also analyzed and a calibration curve was generated from these data.


Author(s):  
M.D. Ball ◽  
H. Lagace ◽  
M.C. Thornton

The backscattered electron coefficient η for transmission electron microscope specimens depends on both the atomic number Z and the thickness t. Hence for specimens of known atomic number, the thickness can be determined from backscattered electron coefficient measurements. This work describes a simple and convenient method of estimating the thickness and the corrected composition of areas of uncertain atomic number by combining x-ray microanalysis and backscattered electron intensity measurements.The method is best described in terms of the flow chart shown In Figure 1. Having selected a feature of interest, x-ray microanalysis data is recorded and used to estimate the composition. At this stage thickness corrections for absorption and fluorescence are not performed.


Author(s):  
Shawn Williams ◽  
Xiaodong Zhang ◽  
Susan Lamm ◽  
Jack Van’t Hof

The Scanning Transmission X-ray Microscope (STXM) is well suited for investigating metaphase chromosome structure. The absorption cross-section of soft x-rays having energies between the carbon and oxygen K edges (284 - 531 eV) is 6 - 9.5 times greater for organic specimens than for water, which permits one to examine unstained, wet biological specimens with resolution superior to that attainable using visible light. The attenuation length of the x-rays is suitable for imaging micron thick specimens without sectioning. This large difference in cross-section yields good specimen contrast, so that fewer soft x-rays than electrons are required to image wet biological specimens at a given resolution. But most imaging techniques delivering better resolution than visible light produce radiation damage. Soft x-rays are known to be very effective in damaging biological specimens. The STXM is constructed to minimize specimen dose, but it is important to measure the actual damage induced as a function of dose in order to determine the dose range within which radiation damage does not compromise image quality.


Author(s):  
J. M. Paque ◽  
R. Browning ◽  
P. L. King ◽  
P. Pianetta

Geological samples typically contain many minerals (phases) with multiple element compositions. A complete analytical description should give the number of phases present, the volume occupied by each phase in the bulk sample, the average and range of composition of each phase, and the bulk composition of the sample. A practical approach to providing such a complete description is from quantitative analysis of multi-elemental x-ray images.With the advances in recent years in the speed and storage capabilities of laboratory computers, large quantities of data can be efficiently manipulated. Commercial software and hardware presently available allow simultaneous collection of multiple x-ray images from a sample (up to 16 for the Kevex Delta system). Thus, high resolution x-ray images of the majority of the detectable elements in a sample can be collected. The use of statistical techniques, including principal component analysis (PCA), can provide insight into mineral phase composition and the distribution of minerals within a sample.


Author(s):  
Imre Pozsgai ◽  
Klara Erdöhalmi-Torok

The paintings by the great Hungarian master Mihaly Munkacsy (1844-1900) made in an 8-9 years period of his activity are deteriorating. The most conspicuous sign of the deterioration is an intensive darkening. We have made an attempt by electron beam microanalysis to clarify the causes of the darkening. The importance of a study like this is increased by the fact that a similar darkening can be observed on the paintings by Munkacsy’s contemporaries e.g Courbet and Makart. A thick brown mass the so called bitumen used by Munkacsy for grounding and also as a paint is believed by the art historians to cause the darkening.For this study, paint specimens were taken from the following paintings: “Studio”, “Farewell” and the “Portrait of the Master’s Wife”, all of them are the property of the Hungarian National Gallery. The paint samples were embedded in a polyester resin “Poly-Pol PS-230” and after grinding and polishing their cross section was used for x-ray mapping.


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