Specimen Preparation for Clinical Applications of X-Ray Microanalysis

Author(s):  
J.D. Shelburne ◽  
G.M. Roomans

Proper preparative procedures are a prerequisite for the validity of the results of x-ray microanalysis of biological tissue. Clinical applications of x-ray microanalysis are often concerned with diagnostic problems and the results may have profound practical significance for the patient. From this point of view it is especially important that specimen preparation for clinical applications is carried out correctly.Some clinical problems require very little tissue preparation. Hair, nails, and kidney and gallbladder stones may be examined and analyzed after carbon coating. High levels of zinc or copper in hair may be indicative of dermatological or systemic diseases. Nail clippings may be analyzed (as an alternative to the more conventional sweat test) to confirm a diagnosis of cystic fibrosis. X-ray microanalysis in combination with scanning electron microscopy has been shown to be the most reliable method for the identification of the components of kidney or gallbladder stones.A quantitatively very important clinical application of x-ray microanalysis is the identification and quantification of asbestos and other exogenous particles in lung.

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):  
D. A. Carpenter ◽  
M. A. Taylor

The development of intense sources of x rays has led to renewed interest in the use of microbeams of x rays in x-ray fluorescence analysis. Sparks pointed out that the use of x rays as a probe offered the advantages of high sensitivity, low detection limits, low beam damage, and large penetration depths with minimal specimen preparation or perturbation. In addition, the option of air operation provided special advantages for examination of hydrated systems or for nondestructive microanalysis of large specimens.The disadvantages of synchrotron sources prompted the development of laboratory-based instrumentation with various schemes to maximize the beam flux while maintaining small point-to-point resolution. Nichols and Ryon developed a microprobe using a rotating anode source and a modified microdiffractometer. Cross and Wherry showed that by close-coupling the x-ray source, specimen, and detector, good intensities could be obtained for beam sizes between 30 and 100μm. More importantly, both groups combined specimen scanning with modern imaging techniques for rapid element mapping.


Author(s):  
Steve Lindaas ◽  
Chris Jacobsen ◽  
Alex Kalinovsky ◽  
Malcolm Howells

Soft x-ray microscopy offers an approach to transmission imaging of wet, micron-thick biological objects at a resolution superior to that of optical microscopes and with less specimen preparation/manipulation than electron microscopes. Gabor holography has unique characteristics which make it particularly well suited for certain investigations: it requires no prefocussing, it is compatible with flash x-ray sources, and it is able to use the whole footprint of multimode sources. Our method serves to refine this technique in anticipation of the development of suitable flash sources (such as x-ray lasers) and to develop cryo capabilities with which to reduce specimen damage. Our primary emphasis has been on biological imaging so we use x-rays in the water window (between the Oxygen-K and Carbon-K absorption edges) with which we record holograms in vacuum or in air.The hologram is recorded on a high resolution recording medium; our work employs the photoresist poly(methylmethacrylate) (PMMA). Following resist “development” (solvent etching), a surface relief pattern is produced which an atomic force microscope is aptly suited to image.


Author(s):  
U. Aebi ◽  
R. Millonig ◽  
H. Salvo

To date, most 3-D reconstructions of undecorated actin filaments have been obtained from actin filament paracrystal data (for refs, see 1,2). However, due to the fact that (a) the paracrystals may be several filament layers thick, and (b) adjacent filaments may sustantially interdigitate, these reconstructions may be subject to significant artifacts. None of these reconstructions has permitted unambiguous tracing or orientation of the actin subunits within the filament. Furthermore, measured values for the maximal filament diameter both determined by EM and by X-ray diffraction analysis, vary between 6 and 10 nm. Obviously, the apparent diameter of the actin filament revealed in the EM will critically depend on specimen preparation, since it is a rather flexible supramolecular assembly which can easily be bent or distorted. To resolve some of these ambiguities, we have explored specimen preparation conditions which may preserve single filaments sufficiently straight and helically ordered to be suitable for single filament 3-D reconstructions, possibly revealing molecular detail.


Author(s):  
A. LeFurgey ◽  
P. Ingram ◽  
L.J. Mandel

For quantitative determination of subcellular Ca distribution by electron probe x-ray microanalysis, decreasing (and/or eliminating) the K content of the cell maximizes the ability to accurately separate the overlapping K Kß and Ca Kα peaks in the x-ray spectra. For example, rubidium has been effectively substituted for potassium in smooth muscle cells, thus giving an improvement in calcium measurements. Ouabain, a cardiac glycoside widely used in experimental and clinical applications, inhibits Na-K ATPase at the cell membrane and thus alters the cytoplasmic ion (Na,K) content of target cells. In epithelial cells primarily involved in active transport, such as the proximal tubule of the rabbit kidney, ouabain rapidly (t1/2= 2 mins) causes a decrease2 in intracellular K, but does not change intracellular total or free Ca for up to 30 mins. In the present study we have taken advantage of this effect of ouabain to determine the mitochondrial and cytoplasmic Ca content in freeze-dried cryosections of kidney proximal tubule by electron probe x-ray microanalysis.


2020 ◽  
Vol 71 (8) ◽  
pp. 21-26
Author(s):  
Elena-Emilia Oprescu ◽  
Cristina-Emanuela Enascuta ◽  
Elena Radu ◽  
Vasile Lavric

In this study, the SO42-/TiO2-La2O3-Fe2O3 catalyst was prepared and tested in the conversion of fructose to ethyl levulinate . The catalyst was characterized from the point of view of the textural analysis, FT-IR analysis, acid strength distribution, X-ray powder diffraction and pyridine adsorption IR spectra. The influence of the reaction parameters on the ethyl levulinate yield was study. The maximum yield of 37.95% in levulinate esters was obtained at 180 �C, 2 g catalyst and 4 h reaction time. The effect of ethyl levulinate addition to diesel-biodiesel blend in different rates, i.e, 0.5, 1, 2.5, 5 (w.t %) on density, kinematic viscosity and flash point was evaluated and compared with the European specification.


2018 ◽  
Vol 21 (7) ◽  
pp. 495-500 ◽  
Author(s):  
Hassan A. Almarshad ◽  
Sayed M. Badawy ◽  
Abdalkarem F. Alsharari

Aim and Objective: Formation of the gallbladder stones is a common disease and a major health problem. The present study aimed to identify the structures of the most common types of gallbladder stones using X-ray spectroscopic techniques, which provide information about the process of stone formation. Material and Method: Phase and elemental compositions of pure cholesterol and mixed gallstones removed from gallbladders of patients were studied using energy-dispersive X-ray spectroscopy combined with scanning electron microscopy analysis and X-ray diffraction. Results: The crystal structures of gallstones which coincide with standard patterns were confirmed by X-ray diffraction. Plate-like cholesterol crystals with laminar shaped and thin layered structures were clearly observed for gallstone of pure cholesterol by scanning electron microscopy; it also revealed different morphologies from mixed cholesterol stones. Elemental analysis of pure cholesterol and mixed gallstones using energy-dispersive X-ray spectroscopy confirmed the different formation processes of the different types of gallstones. Conclusion: The method of fast and reliable X-ray spectroscopic techniques has numerous advantages over the traditional chemical analysis and other analytical techniques. The results also revealed that the X-ray spectroscopy technique is a promising technique that can aid in understanding the pathogenesis of gallstone disease.


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.


Coatings ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 570
Author(s):  
Olga Sánchez ◽  
Manuel Hernández-Vélez

ZnOTe compounds were grown by DC magnetron cosputtering from pure Tellurium (Te) and Zinc (Zn) cathodes in O2/Ar atmosphere. The applied power on the Zn target was constant equal to 100 W, while the one applied on the Te target took two values, i.e., 5 W and 10 W. Thus, two sample series were obtained in which the variable parameter was the distance from the Te targets to the substrate. Sample compositions were determined by Rutherford Backscattering Spectroscopy (RBS) experiments. Structural analysis was done using X-Ray diffraction (XRD) spectrometry and the growth of the hexagonal w-ZnO phase was identified in the XRD spectra. RBS results showed high bulk homogeneity of the samples forming ZnOTe alloys, with variable Te molar fraction (MF) ranging from 0.48–0.6% and from 1.9–3.1% for the sample series obtained at 5 W and 10 W, respectively. The results reflect great differences between the two sample series, particularly from the structural and optical point of view. These experiments point to the possibility of Te doping ZnO with the permanence of intrinsic defects, as well as the possibility of the formation of other Te solid phases when its content increases. The results and appreciable variations in the band gap transitions were detected from Photoluminescence (PL) measurements.


Synlett ◽  
2021 ◽  
Author(s):  
Vinod Kumar

Hydantoin and its analogs such as thiohydantoin and iminohydantoin have received substantial attention both from a chemical and biological point of view. Several compounds of this class have shown useful pharmacological activities such as anticonvulsant, antitumor, antiarrhythmic, herbicidal, and others that lead in some cases to clinical applications. Because of broad-spectrum activities, intensive research efforts have been dedicated in industry and academia to the synthesis and structural modifications of hydantoin and its derivatives. Realizing the importance of hydantoin in organic and medicinal chemistry, we also initiated a research program to successfully design and develop the new routes/methods resulting in the formation of hydantoin, thiohydantoin, and iminohydantoin substituted at different positions particularly at the N-1 position without following protection-deprotection strategy. Given the fact that the combination of two or more pharmacophoric groups may lead to hybrid molecules which result in a mixed mechanism of action on the biological target. We, therefore, further extended the developed strategy for the synthesis of new types of hydantoin-based hybrid molecules by combining hydantoin with a triazole, isoxazoline, and phosphate scaffolds as another pharmacophoric group to exploit diverse biological functions.


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