Feasibility of Be Analysis For Geologic Materials Using Epma

1997 ◽  
Vol 3 (S2) ◽  
pp. 893-894
Author(s):  
Joseph Evensen ◽  
Gregory P. Meeker

Microanalytical techniques for the analysis of beryllium using the electron probe have been evaluated for Be metal, Be-rich silicate minerals, and three Be-rich synthetic silicate glasses. Despite difficulties typical of ultra-light element analysis in geologic materials, quantitative data for Be may be obtainable through careful analytical measurements, determination of optimal operating conditions, and consideration of parameters such as sample orientation and beam-induced migration.Analyses for Be were obtained using a layered synthetic microstructure “crystal” (Mo/B4C) on the JEOL 8900 electron microprobe at the USGS, Denver, Colorado. The optimum accelerating voltage for Be detection was determined to be 8kV (Fig.l). Beryllium analyses in glass and mineral phases were successful using a beam current of 30nA and a 50 μm beam diameter. Due to low count rates, peak counting times of 10 minutes (beryl) and 30 minutes (glass) were required in order to achieve reasonable counting statistics and detection limits.

Author(s):  
Shuihe Mao

Owing to the invisibility of ultramicron gold (invisible gold) in “Carlin type” gold ore, it is extremely difficult to investigate its occurrence and distribution by conventional determinative means.EPMA has been proved to be very powerful instrument for doing research on this subject because it has advantages of high space resolution, nondestructive,getting quantitative analysis results and observing various kinds of images continuously with same equipment etc.The unoxidized ore sample is selected from drill cuttings at a “Carl in type” gold mine in Southwest China with gold tenor of 31.02 g/t and weighs 2438g. The operating conditions of EPMA are: accelerating voltage 25kV, beam current 1×10-8 A, beam diameter about 1 μm. AuLα but not AuMα is preferably chosen as analysed x-ray line, because AuMα1 (5.840A) is overlapping with the 3rd order line of FeKα (5.812A) to some extent and iron is the main component of pyrite matrix. According to the expression of detection limit(CDL ), the calculated value of CDL under the circumstances is 0.038%.


1994 ◽  
Vol 38 ◽  
pp. 711-723
Author(s):  
D. Bonvin ◽  
K. Juchli ◽  
B.W. Adamson

In the early years, the element range covered by the Wavelength Dispersive X-Ray fluorescence (WDXRF) technique was restricted by the quality of vacuum, crystals and detectors in the system. The lightest element detectable was Aluminium (Z = 13). The area of light element analysis had obvious potential for extension over the years. It created the barrier for XRP coverage of the Periodic Table because the naturally softer radiations lay out of range of the technique. In the middle of the 1980's, new technology became available for the manufacture of synthetic crystals with artificially created 2d spacings to suit the X-ray wavelength range of interest. These hyered synthetic microstructures (also called “multilayer crystals”) allowed more sensitivity to be achieved in this part of the spectrum, and the bottom element limit soon moved down towards lighter elements.


Author(s):  
Shuihe Mao

Owing to the invisibility of ultramicron gold (invisible gold) in “Carl in type” gold ore, it is extremely difficult to investigate its occurrence and distribution by conventional determinative means.EPMA has been proved to be very powerful instrument for doing research on this subject because it has advantages of high space resolution, nondestructive,getting quantitative analysis results and observing various kinds of images continuously with same equipment etc.The unoxidized ore sample is selected from drill cuttings at a “Carlin type” gold mine in Southwest China with gold tenor of 31.02 g/t and weighs 2438g. The operating conditions of EPMA are: accelerating voltage 25kV, beam current 1×l0-8 A, beam diameter about 1 μm. AuLα but not AuMα is preferably chosen as analysed x-ray line, because AuMα 1 (5.840Å) is overlapping with the 3rd order line of FeKα (5.812Å) to some extent and iron is the main component of pyrite matrix. According to the expression of detection limit(CDL ), the calculated value of CDL under the circumstances is 0.038%.


Author(s):  
G.F. Bastin ◽  
H.J.M. Heijligers ◽  
J.M. Dijkstra

For the calculation of X-ray intensities emitted by elements present in multi-layer systems it is vital to have an accurate knowledge of the x-ray ionization vs. mass-depth (ϕ(ρz)) curves as a function of accelerating voltage and atomic number of films and substrate. Once this knowledge is available the way is open to the analysis of thin films in which both the thicknesses as well as the compositions can usually be determined simultaneously.Our bulk matrix correction “PROZA” with its proven excellent performance for a wide variety of applications (e.g., ultra-light element analysis, extremes in accelerating voltage) has been used as the basis for the development of the software package discussed here. The PROZA program is based on our own modifications of the surface-centred Gaussian ϕ(ρz) model, originally introduced by Packwood and Brown. For its extension towards thin film applications it is required to know how the 4 Gaussian parameters α, β, γ and ϕ(o) for each element in each of the films are affected by the film thickness and the presence of other layers and the substrate.


Author(s):  
S. Lehner ◽  
H.E. Bauer ◽  
R. Wurster ◽  
H. Seiler

In order to compare different microanalytical techniques commercially available cation exchange membrane SC-1 (Stantech Inc, Palo Alto), was loaded with biologically relevant elements as Na, Mg, K, and Ca, respectively, each to its highest possible concentration, given by the number concentration of exchangeable binding sites (4 % wt. for Ca). Washing in distilled water, dehydration through a graded series of ethanol, infiltration and embedding in Spurr’s low viscosity epoxy resin was followed by thin sectioning. The thin sections (thickness of about 50 nm) were prepared on carbon foils and mounted on electron microscopical finder grids.The samples were analyzed with electron microprobe JXA 50A with transmitted electron device, EDX system TN 5400, and on line operating image processing system SEM-IPS, energy filtering electron microscope CEM 902 with EELS/ESI and Auger spectrometer 545 Perkin Elmer.With EDX, a beam current of some 10-10 A and a beam diameter of about 10 nm, a minimum-detectable mass of 10-20 g Ca seems within reach.


Author(s):  
D. Goyal ◽  
A. H. King

TEM images of cracks have been found to give rise to a moiré fringe type of contrast. It is apparent that the moire fringe contrast is observed because of the presence of a fault in a perfect crystal, and is characteristic of the fault geometry and the diffracting conditions in the TEM. Various studies have reported that the moire fringe contrast observed due to the presence of a crack in an otherwise perfect crystal is distinctive of the mode of crack. This paper describes a technique to study the geometry and mode of the cracks by comparing the images they produce in the TEM because of the effect that their displacement fields have on the diffraction of electrons by the crystal (containing a crack) with the corresponding theoretical images. In order to formulate a means of matching experimental images with theoretical ones, displacement fields of dislocations present (if any) in the vicinity of the crack are not considered, only the effect of the displacement field of the crack is considered.The theoretical images are obtained using a computer program based on the two beam approximation of the dynamical theory of diffraction contrast for an imperfect crystal. The procedures for the determination of the various parameters involved in these computations have been well documented. There are three basic modes of crack. Preliminary studies were carried out considering the simplest form of crack geometries, i. e., mode I, II, III and the mixed modes, with orthogonal crack geometries. It was found that the contrast obtained from each mode is very distinct. The effect of variation of operating conditions such as diffracting vector (), the deviation parameter (ω), the electron beam direction () and the displacement vector were studied. It has been found that any small change in the above parameters can result in a drastic change in the contrast. The most important parameter for the matching of the theoretical and the experimental images was found to be the determination of the geometry of the crack under consideration. In order to be able to simulate the crack image shown in Figure 1, the crack geometry was modified from a orthogonal geometry to one with a crack tip inclined to the original crack front. The variation in the crack tip direction resulted in the variation of the displacement vector also. Figure 1 is a cross-sectional micrograph of a silicon wafer with a chromium film on top, showing a crack in the silicon.


Author(s):  
Nestor J. Zaluzec

The application of electron energy loss spectroscopy (EELS) to light element analysis is rapidly becoming an important aspect of the microcharacterization of solids in materials science, however relatively stringent requirements exist on the specimen thickness under which one can obtain EELS data due to the adverse effects of multiple inelastic scattering.1,2 This study was initiated to determine the limitations on quantitative analysis of EELS data due to specimen thickness.


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