Diagnosis of Silica Induced Granulomatous Hypersensitivity

Author(s):  
C. W. Mehard ◽  
W. L. Epstein

The underlying cause of a disease may not he readily apparent but may have a long history in development. We report one such case which was diagnosed with the aid of the analytical electron microscope.The patient, a 48 yr. old white female, developed a tender nodule on the sole of her foot in December, 1981. Subsequently additional lesions developed on the same foot resulting in deep pain and tenderness. Superficial lesions also extended up to the knee on both legs. No abnormalities were revealed in blood tests or chest X-rays.

Author(s):  
C. E. Lyman ◽  
J. I. Goldstein ◽  
D.B. Williams ◽  
D.W. Ackland ◽  
S. von Harrach ◽  
...  

A major goal of analytical electron micrsocopy (AEM) is to detect small amounts of an element in a given matrix at high spatial resolution. While there is a tradeoff between low detection limit and high spatial resolution, a field emission electron gun allows detection of small amounts of an element at sub-lOnm spatial resolution. The minimum mass fraction of one element measured in another is proportional to [(P/B)·P]-1/2 where the peak-to-background ratio P/B and the peak intensity P both must be high to detect the smallest amount of an element. Thus, the x-ray detection performance of an analytical electron microscope may be characterized in terms of standardized measurements of peak-to-background, x-ray intensity, the level of spurious x-rays (hole count), and x-ray detector performance in terms of energy resolution and peak shape.This paper provides measurements of these parameters from Lehigh’s VG Microscopes HB-603 field emission AEM. This AEM was designed to provide the best x-ray detection possible.


Author(s):  
H. A. Freeman ◽  
Y. A. Peters

Considerably improved performance is provided by gypsum construction wallboard which has been formulated to enhance durability and water resistance in applications that are susceptible to high humidity and moisture. One ingredient that is economically added in small amounts for this purpose is a low viscosity methyl hydrogen silicone fluid. The silicone was found to provide the necessary hydrophobic character and strength improvement when it was incorporated with the gypsum slurry in early stages of wallboard manufacture. However, it remained unknown where the silicone became localized to achieve this effect. Microanalyses were therefore performed in the analytical electron microscope to define the distribution of silicone in commercial gypsum wallboard samples.Gypsum samples were obtained which included those containing silicone and others to which no silicone had been added during manufacture. Analyses were performed in a JEM 2000FX analytical electron microscope operated at 200 keV and equipped with Tracor Northern Micro-ZHV and Microtrace energy dispersive x-ray spectrometers. Scanning (SEM), transmission (TEM), and scanning transmission (STEM) images were correlated with the mapped distributions of as many as six different elements acquired simultaneously. Low Z substrates and tilting specimen holders effectively minimized incorporation of spurious x rays in the final spectra.


Author(s):  
L. Herman ◽  
T. Sato ◽  
B. A. Weavers

The analytical electron microscope, EMMA-4, is designed specifically to perform x-ray microanalysis of conventional transmission electron microscope specimens.The analysis facilities consist of two fully focussing crystal spectrometers each of which can be tuned to collect x-rays emitted from elements of atomic number greater than 11. In addition to the two crystal spectrometers there is a non-dispersive detector which can be used to monitor the total x-ray emission of the specimen and adds the facility for determination of the “continuum” radiation for quantitative analysis. The exact area of analysis is always located by direct observation of the viewing screen.


Author(s):  
N. Ridley ◽  
S.A. Al-Salman ◽  
G.W. Lorimer

The application of the technique of analytical electron microscopy to the study of partitioning of Mn (1) and Cr (2) during the austenite-pearlite transformation in eutectoid steels has been described in previous papers. In both of these investigations, ‘in-situ’ analyses of individual cementite and ferrite plates in thin foils showed that the alloying elements partitioned preferentially to cementite at the transformation front at higher reaction temperatures. At lower temperatures partitioning did not occur and it was possible to identify a ‘no-partition’ temperature for each of the steels examined.In the present work partitioning during the pearlite transformation has been studied in a eutectoid steel containing 1.95 wt% Si. Measurements of pearlite interlamellar spacings showed, however, that except at the highest reaction temperatures the spacing would be too small to make the in-situ analysis of individual cementite plates possible, without interference from adjacent ferrite lamellae. The minimum diameter of the analysis probe on the instrument used, an EMMA-4 analytical electron microscope, was approximately 100 nm.


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):  
Vinayak P. Dravid ◽  
H. Zhang ◽  
L.D. Marks ◽  
J.P. Zhang

A 200 kV cold field emission gun atomic resolution analytical electron microscope (ARAEM, Hitachi HF-2000) has been recently installed at Northwestern. The ARAEM offers an unprecedented combination of atomic structure imaging of better than 0.20 nm nominal point-to-point resolution and about 0.10 nm line resolution, alongwith nanoscale analytical capabilities and electron holography in one single instrument. The ARAEM has been fully functional/operational and this paper presents some illustrative examples of application of ARAEM techniques to oxide superconductors. Additional results will be presented at the meeting.


Author(s):  
T. Kaneyama ◽  
M. Naruse ◽  
Y. Ishida ◽  
M. Kersker

In the field of materials science, the importance of the ultrahigh resolution analytical electron microscope (UHRAEM) is increasing. A new UHRAEM which provides a resolution of better than 0.2 nm and allows analysis of a few nm areas has been developed. [Fig. 1 shows the external view] The followings are some characteristic features of the UHRAEM.Objective lens (OL)Two types of OL polepieces (URP for ±10' specimen tilt and ARP for ±30' tilt) have been developed. The optical constants shown in the table on the next page are figures calculated by the finite element method. However, Cs was experimentally confirmed by two methods (namely, Beam Tilt method and Krivanek method) as 0.45 ∼ 0.50 mm for URP and as 0.9 ∼ 1.0 mm for ARP, respectively. Fig. 2 shows an optical diffractogram obtained from a micrograph of amorphous carbon with URP under the Scherzer defocus condition. It demonstrates a resolution of 0.19 nm and a Cs smaller than 0.5 mm.


Author(s):  
K. Fukushima ◽  
T. Kaneyama ◽  
F. Hosokawa ◽  
H. Tsuno ◽  
T. Honda ◽  
...  

Recently, in the materials science field, the ultrahigh resolution analytical electron microscope (UHRAEM) has become a very important instrument to study extremely fine areas of the specimen. The requirements related to the performance of the UHRAEM are becoming gradually severer. Some basic characteristic features required of an objective lens are as follows, and the practical performance of the UHRAEM should be judged by totally evaluating them.1) Ultrahigh resolution to resolve ultrafine structure by atomic-level observation.2) Nanometer probe analysis to analyse the constituent elements in nm-areas of the specimen.3) Better performance of x-ray detection for EDS analysis, that is, higher take-off angle and larger detection solid angle.4) Higher specimen tilting angle to adjust the specimen orientation.To attain these requirements simultaneously, the objective lens polepiece must have smaller spherical and chromatic aberration coefficients and must keep enough open space around the specimen holder in it.


2011 ◽  
Vol 19 (3) ◽  
pp. 72-72
Author(s):  
Graham Cliff

I write this as a materials scientist concerned about the inadequacy of regulation, monitoring, and control of what are known as nanoparticles (NPs). This is not because present particulate legislation is “inadequate” but because it is inadequately policed and does NOT extend to small enough particulates. I have analyzed these very small particles in the analytical electron microscope (AEM) for over thirty-seven years. A graduate student, with whom I worked over thirty years ago, described in her thesis the conclusion that these particles would have “long-range environmental impact.” We did not then have the benefit of hindsight.


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