Electron probe

The elemental composition of the fish otoliths is a potential source of the useful information to recreate environment history of the individual fish in some of the species. In-depth study of the chemical composition of the otolith center (formed eaidy in fish life) and otolith edge (formed later in fish life) ensures chronological and environmental information stored in the otoliths [1]. This infoiTnation may be achieved by X-ray electron probe microanalysis (EPMA). EPMA is the analytical method to determine the elemental composition of different otolith s parts, their sizes varying from ten up to some tens of microns. 

The complex of the following destmctive and nondestmctive analytical methods was used for studying the composition of sponges inductively coupled plasma mass-spectrometry (ICP-MS), X-ray fluorescence (XRF), electron probe microanalysis (EPMA), and atomic absorption spectrometry (AAS). Techniques of sample preparation were developed for each method and their metrological characteristics were defined. Relative standard deviations for all the elements did not exceed 0.25 within detection limit. The accuracy of techniques elaborated was checked with the method of additions and control methods of analysis. 

INVESTIGATION OF INDIVIDUAL PARTICLES OF ZEOLITE POWDER BY X-RAY ELECTRON PROBE MICROANALYSIS... 

The powders of zeolites of various trademarks are used to produce petroleum-refining catalysts. In this connection, it is very important to have complete information concerning not only chemical composition and distribution of impurity elements, but also shape, surface, stmcture and sizes of particles. It allows a more detailed analysis of the physical-chemical characteristics of catalysts, affecting their activity at different stages of technological process. One prospective for solving these tasks is X-ray microanalysis with an electron probe (EPMA). 

ELECTRON PROBE MICRO ANALYSIS OF THE METALLIC WARE OF THE BRONZE AGE... 

Figures 4c and 4d illustrate what happens when the incident electron probe is focused to illuminate alternately a crystallite in the center of the image (labelled twin) (Figure 4c) and another crystallite adjacent to the twin (Figure 4d). This focused-probe technique is sometimes referred to as micro-diffi-action. Two effects are evident in these micro-diffraction patterns. First, the diffraction patterns consist...

Electron Probe Microanalysis, EPMA, as performed in an electron microprobe combines EDS and WDX to give quantitative compositional analysis in the reflection mode from solid surfaces together with the morphological imaging of SEM. The spatial resolution is restricted by the interaction volume below the surface, varying from about 0.2 pm to 5 pm. Flat samples are needed for the best quantitative accuracy. Compositional mapping over a 100 x 100 micron area can be done in 15 minutes for major components Z> 11), several hours for minor components, and about 10 hours for trace elements. 

Quantitative Electron-Probe Microanalysis. (V. D. Scott and G. Love, eds.) John Wiley Sons, New York, 1983. Taken from a short course on the electron microprobe for scientists working in the field. A thorough discussion of EDS and WDS is given, including experimental conditions and specimen requirements. The ZAF correction factors are treated extensively, and statistics, computer programs and Monte Carlo methods are explained in detail. Generally, a very useftd book. 

CL is the only contaedess method (in an electron probe instrument) that provides microcharacterization of electronic properties of luminescent materials. 

The spatial resolution of the CI SEM mode depends mainly on the electron-probe size, the size of the excitation volume, which is related to the electron-beam penetration range in the material (see the articles on SEM and EPMA), and the minority carrier diffusion. The spatial resolution also may be afiFected by the signal-to-noise ratio, mechanical vibrations, and electromagnetic interference. In practice, the spatial resolution is determined basically by the size of the excitation volume, and will be between about 0.1 and 1 pm ... 

An electron gun produces and accelerates the electron beam, which is reduced in diameter (demagnified) by one or more electromagnetic electron lenses. Electromagnetic scanning coils move this small electron probe (i.e., the beam) across the specimen in a raster. Electron detectors beyond the specimen collect a signal that is used to modulate the intensity on a cathode-ray tube that is scanned in synchronism with the beam on the specimen. A schematic of the essential components in a dedicated STEM system is shown in Figure 2. 

The most important criterion for a STEM instrument is the amount of current in the small electron probe. Generally, 1 nA of probe current is required for high-... 

Electron Probe X-Ray Microanalysis (EPMA) is a spatially resolved, quantitative elemental analysis technique based on the generation of characteristic X rays by a focused beam of energetic electrons. EPMA is used to measure the concentrations of elements (beryllium to the actinides) at levels as low as 100 parts per million (ppm) and to determine lateral distributions by mapping. The modern EPMA instrument consists of several key components ... 

The analyst has two practical means of measuring the energy distribution of X rays emitted from the specimen energy-dispersive spectrometry and wavelength dispersive spectrometry. These two spectrometers are highly complementary the strengths of each compensate for the weaknesses of the other, and a well-equipped electron probe instrument will have both spectrometers. 

The keystone of practical quantitative electron probe microanalysis is Castaing s first approximation, which relates the concentration for a constituent in the unknown to the concentration in a standard in terms of the ratio of X-ray intensities generated in the target ... 

Because X-ray counting rates are relatively low, it typically requires 100 seconds or more to accumulate adequate counting statistics for a quantitative analysis. As a result, the usual strategy in applying electron probe microanalysis is to make quantitative measurements at a limited collection of points. Specific analysis locations are selected with the aid of a rapid imaging technique, such as an SEM image prepared with backscattered electrons, which are sensitive to compositional variations, or with the associated optical microscope. 

The electron probe X-ray microanalyzer provides extraordinary power for measuring the elemental composition of solid matter with pm lateral spatial resolution. The spatial resolution, limited by the spread of the beam within the specimen, permits pg samples to be measured selectively, with elemental coverage from boron to the actinides. By incorporating the imaging capability of the SEM, the electron probe X-ray microanalyzer combines morphological and compositional information. 

R. Castaing. Application of Electron Probes to Local Chemical and Crystallographic Analysis. Ph.D. thesis. University of Paris, 1951. 

D. E. Newbury, C. E. Fiori, R. B. Marinenko, R. L. Myklebust, C. R. Swyt, and D. S. Bright. Compositional Mapping with the Electron Probe Microanalyzer. Anal. Ghent. 1990, 62, Parti, 1159A PartII, 1245A. 

G. F. Bastin and H. J. M. Heijligers. Quantitative Electron Probe Microanalysis of Ultralight Elements (Boron—Oxygen). Scanning. 12, 225, 1990. 

Laser ionization mass spectrometry or laser microprobing (LIMS) is a microanalyt-ical technique used to rapidly characterize the elemental and, sometimes, molecular composition of materials. It is based on the ability of short high-power laser pulses (-10 ns) to produce ions from solids. The ions formed in these brief pulses are analyzed using a time-of-flight mass spectrometer. The quasi-simultaneous collection of all ion masses allows the survey analysis of unknown materials. The main applications of LIMS are in failure analysis, where chemical differences between a contaminated sample and a control need to be rapidly assessed. The ability to focus the laser beam to a diameter of approximately 1 mm permits the application of this technique to the characterization of small features, for example, in integrated circuits. The LIMS detection limits for many elements are close to 10 at/cm, which makes this technique considerably more sensitive than other survey microan-alytical techniques, such as Auger Electron Spectroscopy (AES) or Electron Probe Microanalysis (EPMA). Additionally, LIMS can be used to analyze insulating sam-... 

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