Electron Probe Microanalysis EPMA

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. 

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. 

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-... 

Bi2S3 Bi2Te3 Bi(N03)3 Na2S Te02 XRD, SEM, electron probe microanalysis (EPMA), FESEM 162-166... 

As indicated in Fig. 7.2, X-rays are among the by-products in an electron microscope. Already at the beginning of this century, people knew that matter emits X-rays when it is bombarded with electrons. The explanation of the phenomenon came with the development of quantum mechanics. Nowadays, it is the basis for determining composition on the submicron scale and, with still increasing spatial resolution, is used in the technique referred to as Electron Microprobe Analysis (EMA), Electron Probe Microanalysis (EPMA) or Energy Dispersive Analysis of X-rays (EDAX, EDX) [21]. 

Miura and Yoshida also investigated the changes in the microstructure of 1100 EW Nafion sulfonate membranes, in alkali, ammonium, and alkylammonium cation forms, that were induced by swelling in ethanol using DSC, dynamic mechanical analysis (DMA), SAXS, and electron probe microanalysis (EPMA). These studies were performed within the context of liquid pervaporation membranes that could potentially be used to separate ethanol from water... 

To understand the wear mechanism in valve train wear tests, samples of the worn tappet surface were analyzed for surface elements by electron probe microanalysis (EPMA) and X-ray photo electron spectroscopy (XPS). Results of EPMA analysis of the worn surface in terms of concentration of phosphorus and sulfur atoms for oil with primary ZnDDP without MoDTC, showed an increase of zinc and sulfur intensity after 100 hrs of test time, in spite of decreasing phosphorus intensity. Examination of the worn surface by XPS with primary and secondary ZDDP with addition of MoDTC showed the presence of MoS2 in the tribofilm. Using mixtures of ZDDP and MoDTC, the friction coefficient is reduced, and wear is comparable to that of using ZDDP alone (Kasrai et ah, 1997). 

The compound layer formed in the transition zone between nickel and bismuth was investigated metallographically, by X-rays and electron probe microanalysis (EPMA). X-ray patterns were taken both from the cross-sections in the planes parallel to the initial Ni-Bi interface (after successive removal of the specimen material and polishing its surface) and the powdered phases using Cu Ka radiation. Two methods of obtaining X-ray patterns were employed. Firstly, X-ray photographs were obtained in a 57.3 mm inner diameter Debye-Scherrer camera. Secondly, use was made of a DRON-3 diffractometer to record X-ray diffractograms. 

Electron microprobes permit chemical microanalysis as well as SEM and BSE detection, often referred to as analytical electron microscopy (AEM), or electron probe microanalysis (EPMA)56 57. This is because another product of the surface interaction with an incident electron beam is X-ray photons which have wavelengths and energies dependent on element identity and on the electron shell causing the emission. Analysis of these photons can give a local chemical analysis of the surface. Resolution of 1 pm is attainable. Two types of X-ray spectrometer can be employed ... 

Figure 4. Micrographs of the cross section of a vanadyl phosphate porous microsphere with 10% amorphous silica obtained by electron probe microanalysis (EPMA). Left backscattered electron image showing average atomic number across the specimen. Right X-ray image showing silicon distribution.

Isothermal techniques, by contrast, are inherently better suited for allowing a sample to reach equilibrium. These methods are typically what are used to identify the phase(s) present. These methods include optical microscopy (metallography), electron probe microanalysis (EPMA), and XRD. In each method, sample analysis can be performed at a series of different temperamres, or isotherms. It should be noted, however, that these techniques could also result in inaccurate phase boundaries if an inadequate number of isotherms are made. 

Since carbides are extensively nsed in spatially restricted sizes (thin films, powder particles in cemented carbides), microanalytical techniqnes of local carbon analysis are of special interest for sample characterization. Electron probe microanalysis (EPMA) is the most snccessful method for the qnantitative analysis of carbon when the lateral resolntion needs not to be better than abont 2 xm. 

The use of electron probe microanalysis (EPMA) is rapidly becoming standard practice. This gives us a relatively rapid and unambiguous method for investigating the location, not only of active materials but also potential catalyst poisons. The use of ESCA for characterizing surface-metal concen-... 

Sample preparation for electron probe microanalysis (EPMA) requires sample chips or friable material to be impregnated in an epoxy resin. Sample surfaces are polished using progressively finer grades of diamond paste, with samples mounted onto aluminium stubs and coated with carbon prior to analysis. Samples should be clean, flat polished (2.5 cm diameter,... 

Emission of X-rays characteristic of individual elements Electron probe microanalysis EPMA... 

The microstructure of the samples was examined by the x-ray diffraction (XRD), the scanning electron microscope (SEM), and the electron probe microanalysis (EPMA). The electrical conductivity and Seebeck coefficient were measured from 300 to 1200 K. The thermal conductivity was measured by the laser-flash method at room temperature. 

---