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Electron microscope-thin film microprobe techniques in biomaterial studies of chemical segregation, species diffusion and small particle analysis
Absorption tables for electron probe microanalysis
We used quantitative electron-probe energy-dispersive x-ray microanalysis to localize endogenous Na, Cl, K, P, S, Mg and Ca in cryofixed and freeze-dried cryosections of the cap (i.e. the putative site of graviperception) and elongating zone (i.e. site of gravicurvature) of horizontally oriented roots of Zea mays. Ca, Na, Cl, K and Mg accumulate along the lower side of caps of horizontally oriented roots. The most dramatic asymmetries of these ions occur in the apoplast, especially the mucilage. We could not detect any significant differences in the concentrations of these ions in the central cytoplasm of columella cells along the upper and lower sides of caps of horizontally-oriented roots. However, the increased amounts of Na, Cl, K and Mg in the longitudinal walls of columella cells along the lower side of the cap suggest that these ions may move down through the columella tissue of horizontally-oriented roots. Ca also accumulates (largely in the mucilage) along the lower side of the elongating zone of horizontally-oriented roots, while Na, P, Cl and K tend to accumulate along the upper side of the elongating zone. Of these ions, only K increases in concentration in the cytoplasm and longitudinal walls of cortical cells in the upper vs lower sides of the elongating zone. These results indicate that (1) gravity-induced asymmetries of ions differ significantly in the cap and elongating zone of graviresponding roots, (2) Ca accumulates along the lower side of the cap and elongating zone of graviresponding roots, (3) increased growth of the upper side of the elongating zone of horizontally-oriented roots correlates positively with increased amounts of K in the cytoplasm and longitudinal walls of cortical cells, and (4) the apoplast (especially the mucilage) may be an important component of the pathway via which ions move in graviresponding rots of Zea mays. These results are discussed relative to mechanisms for graviperception and gravicurvature of roots.
Electron probe microanalysis of orgueil meteorite for extraterrestrial life
Electron probe x-ray microanalysis of organized elements in the orgueil carbonaceous meteorite
Preparation of electron probe microanalyzer standards using rapid quench method
Electron probe X ray microanalyzer applied to material failure study, bonding, and other metallurgical analysis
Accurate electron probe values for Mg, Al, and Si in silicate minerals may be obtained with pure-element standards. Analysis must be done at low (6 kV) accelerating potential and for best results, the average atomic number of the sample should be within about plus or minus 1 of the atomic number of the pure-element standard. This last requirement is automatically fulfilled for most common silicate minerals, as their average atomic numbers usually fall within the 11 to 15 range. Examples studied include a wet-chemically analyzed cordierite containing 17.71 weight percent Al, for which a value of 17.6 plus or minus 0.3 percent was obtained with the electron probe, and a hornblende containing 19.15 percent Si, which gave 19.0 plus or minus 0.3 percent using the probe method.
Quantitative electron-probe microanalysis (EPMA) has improved due to better instrument design and X-ray correction methods. Design improvement of the electron column and X-ray spectrometer has resulted in measurement precision that exceeds analytical accuracy. Wavelength-dispersive spectrometer (WDS) have layered-dispersive diffraction crystals with improved light-element sensitivity. Newer energy-dispersive spectrometers (EDS) have Si-drift detector elements, thin window designs, and digital processing electronics with X-ray throughput approaching that of WDS Systems. Using these systems, digital X-ray mapping coupled with spectrum imaging is a powerful compositional mapping tool. Improvements in analytical accuracy are due to better X-ray correction algorithms, mass absorption coefficient data sets,and analysis method for complex geometries. ZAF algorithms have ban superceded by Phi(pz) algorithms that better model the depth distribution of primary X-ray production. Complex thin film and particle geometries are treated using Phi(pz) algorithms, end results agree well with Monte Carlo simulations. For geological materials, X-ray absorption dominates the corretions end depends on the accuracy of mass absorption coefficient (MAC) data sets. However, few MACs have been experimentally measured, and the use of fitted coefficients continues due to general success of the analytical technique. A polynomial formulation of the Bence-Albec alpha-factor technique, calibrated using Phi(pz) algorithms, is used to critically evaluate accuracy issues and can be also be used for high 2% relative and is limited by measurement precision for ideal cases, but for many elements the analytical accuracy is unproven. The EPMA technique has improved to the point where it is frequently used instead of the petrogaphic microscope for reconnaissance work. Examples of stagnant research areas are: WDS detector design characterization of calibration standards, and the need for more complete treatment of the continuum X-ray fluorescence correction.
Technique for indirect calibration in electron-probe microanalysis reduces number of measurements needed without significantly degrading precision of measurement data. Advantageous when many analyses must be performed; for example, determining varying chemical composition at many positions across specimen of multicomponent alloy. Time spent acquiring data reduced considerably.
Computed tomography (CT) imaging and electron-probe microanalysis (EPMA) have been used to study samples of the Mundrabilla and Colomera iron meteorites in order to perform structural, textural, and mineralogical analysis. Both gamma-ray (Co-60 source, essentially monochromatic 1.25MeV avg.) and x-ray (420 KeV, continuous) sources have been used, with effective resolution of approximately 1 mm and 0.25 mm, respectively. The gamma-ray source provides approx. 15 cm penetration through steel and is used for larger samples, whereas the x-ray source provides superior resolution at reduced penetration but exhibits beam hardening artifacts. Here we present a combined approach where CT and EPMA imaging and microanalysis aid in the identification of structural and compositional features in iron meteorites.
Electron probe microanalyses in metallurgy and geology performed by FORTRAN program
Quantitative electron probe microanalyzer standards preparation apparatus, discussing metal alloys rapid quenching and X ray flux data
Standard compositions suitable for electron probe microanalysis of various silicates are prepared by coprecipitation of specified salts with colloidal silica to form a gel which is decomposed into a powdered oxide mixture and compressed into thin pellets. These pellets of predetermined standard are compared with a silicate sample to determine its composition.
Quantitative optical and electron probe studies of opaque phases in Apollo 11 lunar rocks
Electron-probe microanalysis standards and issues related to measurement and accuracy of microanalysis will be discussed. Critical evaluation of standards based on homogeneity and comparison with wet-chemical analysis will be made. Measurement problems such as spectrometer dead-time will be discussed. Analytical accuracy issues will be evaluated for systems by alpha-factor analysis and comparison with experimental k-ratio databases.
Improvement in the accuracy of electron-probe microanalysis (EPMA) has been accomplished by critical assessment of standards, correction algorithms, and mass absorption coefficient data sets. Experimental measurement of relative x-ray intensities at multiple accelerating potential highlights errors in the absorption coefficient. The factor method has been applied to the evaluation of systematic errors in the analysis of semiconductor and silicate minds. Accurate EPMA of Martian soil stimulant is necessary in studies that build on Martian rover data in anticipation of missions to Mars.
The utility of an indirect calibration approach in electron probe microanalysis is explored. The methodology developed is based on establishing a functional relationship between the uncorrected k-ratios and the corresponding concentrations obtained using one of the ZAF correction schemes, for all the desired elements in the concentration range of interest. In cases where a very large number of analyses are desired, such a technique significantly reduces the total time required for the microprobe analysis without any significant loss of precision in the data. A typical application of the method in the concentration mapping of the transverse cross-section of a dendrite in directionally solidified PWA-1480, a nickel-based superalloy, is described.