scholarly journals Application of scanning electron microscopy to x-ray analysis of frozen-hydrated sections. I. Specimen handling techniques.

1981 ◽  
Vol 88 (2) ◽  
pp. 257-267 ◽  
Author(s):  
A J Saubermann ◽  
P Echlin ◽  
P D Peters ◽  
R Beeuwkes

X-ray microanalysis of frozen-hydrated tissue sections permits direct quantitative analysis of diffusible elements in defined cellular compartments. Because the sections are hydrated, elemental concentrations can be defined as wet-weight mass fractions. Use of these techniques should also permit determination of water fraction in cellular compartments. Reliable preparative techniques provide flat, smooth, 0.5 micrometers-thick sections with little elemental and morphological disruption. The specimen support and transfer system described permits hydrated sections to be transferred to the scanning electron microscope cold stage for examination and analysis without contamination or water loss and without introduction of extraneous x-ray radiation.

Author(s):  
R. J. Narconis ◽  
G. L. Johnson

Analysis of the constituents of renal and biliary calculi may be of help in the management of patients with calculous disease. Several methods of analysis are available for identifying these constituents. Most common are chemical methods, optical crystallography, x-ray diffraction, and infrared spectroscopy. The application of a SEM with x-ray analysis capabilities should be considered as an additional alternative.A scanning electron microscope equipped with an x-ray “mapping” attachment offers an additional dimension in its ability to locate elemental constituents geographically, and thus, provide a clue in determination of possible metabolic etiology in calculus formation. The ability of this method to give an undisturbed view of adjacent layers of elements in their natural state is of advantage in determining the sequence of formation of subsequent layers of chemical constituents.


Reproduction ◽  
2000 ◽  
pp. 331-336 ◽  
Author(s):  
L Holm ◽  
H Ekwall ◽  
GJ Wishart ◽  
Y Ridderstrale

Sperm storage tubules from the utero-vaginal junction of chickens, quails and turkeys were analysed for calcium and zinc using X-ray microanalysis of ultra-rapidly frozen tissue in a scanning electron microscope. This technique enabled the tubular fluid surrounding the stored spermatozoa and the intracellular content of the cells of the sperm storage tubules to be analysed separately and, by using standards with known concentrations, their elemental concentrations were estimated. The mean (+/- SEM) concentration of calcium in the tubular fluid from chickens, quails and turkeys was 17 +/- 3, 19 +/- 3 and 17 +/- 4 mmol kg(-1) wet weight, respectively. The intracellular calcium concentration of the cells of the tubules did not differ significantly from these values and was also similar in the mucosal epithelial cells of the utero-vaginal junction. Zinc was localized in the cells of turkey sperm storage tubules and tubular fluid, but at low concentrations. No zinc could be detected in corresponding structures from chickens and quails. The concentration of calcium in the tubular fluid is within the range known to inhibit the motility of spermatozoa, supporting this function for calcium during storage. Zinc is known to depress turkey sperm metabolism and it may also be involved in inducing quiescence of spermatozoa during storage in this species.


2003 ◽  
Vol 67 (2) ◽  
pp. 219-231 ◽  
Author(s):  
H. W. Langmi ◽  
J. Watt

Computer-controlled scanning electron microscopy (CCSEM) has been assessed for the determination of form and size distribution of heavy metals in urban contaminated soils. Metal distributions within individual particles were determined using X-ray element mapping. The sites selected for study were (1) around a landfill site, previously a colliery in Wolverhampton, UK and (2) a private garden adjacent to a railway in Nottingham, UK. Backscattered thresholding techniques were used to isolate the Pb-containing categories. The classification results for both Wolverhampton and Nottingham soils were generally similar but more Pb-containing classes were observed for the Nottingham samples when a comparison was made between results of the same size fractions. However, difficulties with the technique arose when particles showing chemically similar weathering crusts were assigned to the same class, despite having different internal compositions. The CCSEM data therefore need to be interpreted with caution and their application limited to situations in which particle internal complexity is not an issue.


2013 ◽  
Vol 12 (4) ◽  
pp. 095-105
Author(s):  
Beata Klimek

One of the main tasks in the study of historic buildings is the need to identify the original materials and extensions, which often have historic character. The next task concerns the determination of the composition and structure of the historical, diagnosis technique to develop original paint. The article presents the preliminary results of paintings. Methods were used with the scanning electron microscope was equipped with an energy dispersive X-ray spectrometer (SEM-EDS).


2017 ◽  
Vol 67 (5) ◽  
pp. 510 ◽  
Author(s):  
Han Gao ◽  
Wei Jiang ◽  
Jie Liu ◽  
Gazi Hao ◽  
Lei Xiao ◽  
...  

<p>An energetic co-crystal consisting of the most promising military explosive 2,4,6,8,10,12-hexanitro-2,4,6,8,10,12-hexaazaisowurtzitane (CL-20) and the most well-known oxidant applied in propellants ammonium perchlorate has been prepared with a simple solvent evaporation method. Scanning electron microscopy revealed that the morphology of co-crystal differs greatly from each component. The X-ray diffraction spectrum, FTIR, Raman spectra, and differential scanning calorimetry characterisation further prove the formation of the co-crystal. The result of determination of hygroscopic rate indicated the hygroscopicity was effectively reduced. At last, the crystallisation mechanism has been discussed.</p>


2006 ◽  
Vol 12 (5) ◽  
pp. 406-415 ◽  
Author(s):  
Marco Alvisi ◽  
Markus Blome ◽  
Michael Griepentrog ◽  
Vasile-Dan Hodoroaba ◽  
Peter Karduck ◽  
...  

A calibration procedure for the detection efficiency of energy dispersive X-ray spectrometers (EDS) used in combination with scanning electron microscopy (SEM) for standardless electron probe microanalysis (EPMA) is presented. The procedure is based on the comparison of X-ray spectra from a reference material (RM) measured with the EDS to be calibrated and a reference EDS. The RM is certified by the line intensities in the X-ray spectrum recorded with a reference EDS and by its composition. The calibration of the reference EDS is performed using synchrotron radiation at the radiometry laboratory of the Physikalisch-Technische Bundesanstalt. Measurement of RM spectra and comparison of the specified line intensities enables a rapid efficiency calibration on most SEMs. The article reports on studies to prepare such a RM and on EDS calibration and proposes a methodology that could be implemented in current spectrometer software to enable the calibration with a minimum of operator assistance.


2017 ◽  
Vol 2017 ◽  
pp. 1-7 ◽  
Author(s):  
Viera Homolová ◽  
Lucia Čiripová

The isothermal section of the B-Cr-Fe ternary system was studied experimentally at 1353 K. X-ray diffraction and scanning electron microscopy equipped with EDX analyzer were used for determination of phase equilibria and composition of the coexisting phases in the B-Cr-Fe model alloys after long-term annealing (1500–2205 h). Two iron borides FeB and Fe2B, six chromium borides Cr2B, Cr5B3, CrB, Cr3B4, CrB2, and CrB4 and also iron and chromium solid solutions (α(Fe,Cr), α(Cr,Fe), γ(Fe,Cr)) and β-rhombohedral B were observed in the alloys. High solubilities of the third element in binary borides and no ternary phase were found. Based on the experimental results, isothermal section of the B-Cr-Fe system at 1353 K was determined.


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