Sulphur in Different Types of Keratohyalin Granules: A Quantitative Assay by X-Ray Microanalysis

1974 ◽  
Vol 15 (2) ◽  
pp. 359-377
Author(s):  
H. JESSEN ◽  
P. D. PETERS ◽  
T. A. HALL

The elemental composition of keratohyalin granules from the interpapillary and papillary lingual epithelium and the oesophageal epithelium of the rat were studied by X-ray microanalysis in an EMMA-4 analytical electron microscope, equipped with an energy dispersive detector. A quantitative assay of the sulphur concentration in keratohyalin granules was performed, using a suitable sulphur standard. The results demonstrate that different types of keratohyalin granule have different compositions. Single granules - a type of keratohyalin granule present in both nuclei and cytoplasm of the epithelial cells - are rich in sulphur, having a content of 3.6-3.8%. Another type of keratohyalin granule - composite granules - contains a sulphur-rich component and a sulphur-poor component. The sulphur-poor component contains 0.8-1.4% sulphur. It is suggested that the sulphur-rich keratohyalin granules are involved in the deposition of the peripheral envelope protein of cornified cells.

1976 ◽  
Vol 22 (1) ◽  
pp. 161-171
Author(s):  
H. Jessen ◽  
P.D. Peters ◽  
T.A. Hall

The elemental composition of different types of keratohyalin granules from the epidermis of newborn and adult rats was studied by means of an EMMA-4 analytical electron microscope, equipped with an energy-dispersive X-ray spectrometer. An absolute quantitation of the sulphur concentration in keratohyalin granules was performed. The results demonstrate that epidermal keratohyalin granules are chemically heterogeneous. A type of keratohyalin granule present in the nuclei and cytoplasm of epidermal cells from both newborn and adult rats - termed single granules - is rich in sulphur, having a content of 2-5-3-6%. Other types of keratohyalin granules, which differ in newborn and adult rats, contain a sulphur-poor component; they often have a sulphur-rich component as well. The sulphur-poor keratohyalin contains 0-6-0-9% sulphur. It is suggested that the sulphur-rich keratohyalin granules are the source of the peripheral envelope protein of cornified cells.


Author(s):  
E. F. Koch ◽  
E. L. Hall ◽  
S. W. Yang

The plane-front solidified eutectic alloys consisting of aligned tantalum monocarbide fibers in a nickel alloy matrix are currently under consideration for future aircraft and gas turbine blades. The MC fibers provide exceptional strength at high temperatures. In these alloys, the Ni matrix is strengthened by the precipitation of the coherent γ' phase (ordered L12 structure, nominally Ni3Al). The mechanical strength of these materials can be sensitively affected by overall alloy composition, and these strength variations can be due to several factors, including changes in solid solution strength of the γ matrix, changes in they γ' size or morphology, changes in the γ-γ' lattice mismatch or interfacial energy, or changes in the MC morphology, volume fraction, thermal stability, and stoichiometry. In order to differentiate between these various mechanisms, it is necessary to determine the partitioning of elemental additions between the γ,γ', and MC phases. This paper describes the results of such a study using energy dispersive X-ray spectroscopy in the analytical electron microscope.


Author(s):  
Zenji Horita ◽  
Ryuzo Nishimachi ◽  
Takeshi Sano ◽  
Minoru Nemoto

Absorption correction is often required in quantitative x-ray microanalysis of thin specimens using the analytical electron microscope. For such correction, it is convenient to use the extrapolation method[l] because the thickness, density and mass absorption coefficient are not necessary in the method. The characteristic x-ray intensities measured for the analysis are only requirement for the absorption correction. However, to achieve extrapolation, it is imperative to obtain data points more than two at different thicknesses in the identical composition. Thus, the method encounters difficulty in analyzing a region equivalent to beam size or the specimen with uniform thickness. The purpose of this study is to modify the method so that extrapolation becomes feasible in such limited conditions. Applicability of the new form is examined by using a standard sample and then it is applied to quantification of phases in a Ni-Al-W ternary alloy.The earlier equation for the extrapolation method was formulated based on the facts that the magnitude of x-ray absorption increases with increasing thickness and that the intensity of a characteristic x-ray exhibiting negligible absorption in the specimen is used as a measure of thickness.


Author(s):  
S. M. Zemyan ◽  
D. B. Williams

As has been reported elsewhere, a thin evaporated Cr film can be used to monitor the x-ray peak to background ratio (P/B) in an analytical electron microscope. Presented here are the results of P/B measurements for the Cr Ka line on a Philips EM430 TEM/STEM, with Link Si(Li) and intrinsic Ge (IG) x-ray detectors. The goal of the study was to determine the best conditions for x-ray microanalysis.We used the Fiori P/B definition, in which P/B is the ratio of the total peak integral to the average background in a 10 eV channel beneath the peak. Peak and background integrals were determined by the window method, using a peak window from 5.0 to 5.7 keV about Cr Kα, and background windows from 4.1 to 4.8 keV and 6.3 to 7.0 keV.


Author(s):  
R.D. Leapman

Extended X-ray Absorption Fine Structure (EXAFS) analysis makes use of synchrotron radiaion to measure modulations in the absorption coefficient above core edges and hence to obtain information about local atomic environments. EXAFS arises when ejected core electrons are backscattered by surrounding atoms and interfere with the outgoing waves. Recently, interest has also been shown in using inelastic electron scattering1-4. Some advantages of Extended X-ray-edge Energy Loss Fine Structure (EXELFS) are: a) small probes formed by the analytical electron microscope give spectra from μm to nm sized areas, compared with mm diameter areas for the X-ray technique, b) EXELFS can be combined with other techniques such as electron diffraction or high resolution imaging, and c) EXELFS is sensitive to low Z elements with K edges from ˜200 eV to ˜ 3000 eV (B to Cl).


1998 ◽  
Vol 4 (S2) ◽  
pp. 168-169
Author(s):  
D. B. Williams

Since its invention in 1968, the EDS has played an essential role in X-ray analysis of materials, at the micrometer level, in the electron probe microanalyzer (EPMA). In the EPMA, the characteristic X-ray intensity from bulk specimens is sufficient that, despite its very small collection angle, the wavelength dispersive spectrometer (WDS) can also be used. Given the excellent energy resolution of the WDS it has often been the spectrometer of choice for bulk quantitative X-ray microanalysis. Therefore, the most important role of the EDS has been in X-ray microanalysis of thin specimens in the analytical electron microscope (AEM) because, in an AEM, the limited confines of the stage mean that EDS is the only viable spectrometer. Since the pioneering work of Cliff and Lorimer in the 1970s, EDS has been the method by which all high spatial resolution X-ray microanalysis of thin foils has been performed.


2001 ◽  
Vol 7 (S2) ◽  
pp. 694-695
Author(s):  
Eric Lifshin ◽  
Raynald Gauvin ◽  
Di Wu

In Castaing’s classic Ph.D. dissertation he described how the limiting value of x-ray spatial resolution for x-ray microanalysis, of about 1 μm, was not imposed by the diameter of the electron beam, but by the size of the region excited inside the specimen. Fifty years later this limit still applies to the majority of measurement made in EMAs and SEMs, even though there is often a need to analyze much finer structures. When high resolution chemical analysis is required, it is generally necessary to prepare thin sections and examine them in an analytical electron microscope where the maximum diameter of the excited volume may be as small as a few nanometers. Since it is not always possible or practical, it is important to determine just what is the best spatial resolution attainable for the examination of polished or “as received” samples with an EMA or SEM and how to achieve it experimentally.


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