Electron microscopy, analytical method

Asbestos by Transmission Electron Microscopy Analytical Method for the Determination of Asbestos Fibers in Water (EPA/600/4-83-043)... 

Watt, J., 1998. Automated characterisation of individual carbonaceous fly-ash particles by computer controlled scanning electron microscopy analytical methods and critical review of alternative methods. Wat. Air SoU Pollut. 105 309-327. 

Technical examination of objects coated with a protective covering derived from the sap of a shrubby tree produces information that can be used to determine the materials and methods of manufacture. This information sometimes indicates when and where the piece was made. This chapter is intended to present a brief review of the raw material urushi, and the history and study of its use. Analytical techniques have included atomic absorption spectroscopy, thin layer chromatography, differential thermal analysis, emission spectroscopy, x-ray radiography, and optical and scanning electron microscopy these methods and results are reviewed. In addition, new methods are reported, including the use of energy dispensive x-ray fluorescence, scanning photoacoustical microscopy, laser microprobe and nondestructive IR spectrophotometry. 

Other physical methods used in the investigation of N.a. structure are Hybridization (see), electron microscopy, analytical ultracentrifugation, CsQ density gradient centrifugation. X-ray diffraction analysis, infrared spectroscopy, optical rotatory dispersion, light scattering photometry and viscosity measurements. 

Analytical investigations may be undertaken to identify the presence of an ABS polymer, characterize the polymer, or identify nonpolymeric ingredients. Fourier transform infrared (ftir) spectroscopy is the method of choice to identify the presence of an ABS polymer and determine the acrylonitrile—butadiene—styrene ratio of the composite polymer (89,90). Confirmation of the presence of mbber domains is achieved by electron microscopy. Comparison with available physical property data serves to increase confidence in the identification or indicate the presence of unexpected stmctural features. Identification of ABS via pyrolysis gas chromatography (91) and dsc ((92) has also been reported. 

Materials characterization techniques, ie, atomic and molecular identification and analysis, ate discussed ia articles the tides of which, for the most part, are descriptive of the analytical method. For example, both iaftared (it) and near iaftared analysis (nira) are described ia Infrared and raman SPECTROSCOPY. Nucleai magaetic resoaance (nmr) and electron spia resonance (esr) are discussed ia Magnetic spin resonance. Ultraviolet (uv) and visible (vis), absorption and emission, as well as Raman spectroscopy, circular dichroism (cd), etc are discussed ia Spectroscopy (see also Chemiluminescence Electho-analytical techniques It unoassay Mass specthot thy Microscopy Microwave technology Plasma technology and X-ray technology). 

A detailed account is given in Reference 20. The techniques giving the most detailed 3-D stmctural information are x-ray and neutron diffraction, electron diffraction and microscopy (qv), and nuclear magnetic resonance spectroscopy (nmr) (see Analytical methods Magnetic spin resonance X-ray technology). 

The combined use of energy-dispersive X-ray spectroscopy and TEM/STEM is a routine method of analytical electron microscopy enabling both qualitative and quantitative chemical analysis of interfaces and interlayers with high lateral resolution. Reso-... 

The large size of CPOs allows their direct observation. For this purpose, scanning tunneling microscopy (STM) is the best method [32,34]. Electron microscopic analysis is used for phthalocyanine 3 and its derivatives however, most of the porphyrin derivatives are decomposed by electron beam irradiation. Presently, although only a limited number of researchers are able to perform atomic-scale resolution measurement, this powerful analytical method is expected to be used widely in the future. The author reported a summary of STM studies on porphyrins elsewhere [34]. 

Jose-Yacaman, M. and J. A. Ascencio (2000), Electron microscopy and its application to the study of archaeological materials and art preservation, in Ciliberto, E. and G. Spoto (eds.), Modern Analytical Methods in Art and Archaeology, Chemical Analysis Series, Vol. 155, Wiley, New York, pp. 405-443. 

The structure of the catalysts was characterized by X-ray diffraction, IR-spectroscopy and transmission electron microscopy, their thermal stability was followed by thermal analytical method. The specific surface area and pore size distribution of the samples were determined by nitrogen adsorption isotherms. 

Electron probe and X-ray fluorescence methods of analysis are used for rather different but complementary purposes. The ability to provide an elemental spot analysis is the important characteristic of electron probe methods, which thus find use in analytical problems where the composition of the specimen changes over short distances. The examination of the distribution of heavy metals within the cellular structure of biological specimens, the distribution of metal crystallites on the surface of heterogeneous catalysts, or the differences in composition in the region of surface irregularities and faults in alloys, are all important examples of this application. Figure 8.45 illustrates the analysis of parts of a biological cell just 1 pm apart. Combination of electron probe analysis with electron microscopy enables visual examination to be used to identify the areas of interest prior to the analytical measurement. 

Improvements in the resolution and versatility of microscopic techniques have come about rapidly. TEM, STEM, and high-resolution electron microscopy have helped the catalytic chemist to analyze the effects of metal-support interactions and particle-size effects—developments that will probably lead to improvements in commercial technologies. Several novel analytical methods, arising from very clever experimentation, were discussed at the... 

This chapter discusses the range of analytical methods which use the properties of X-rays to identify composition. The methods fall into two distinct groups those which study X-rays produced by the atoms to chemically identify the elements present, and X-ray diffraction (XRD), which uses X-rays of known wavelengths to determine the spacing in crystalline structures and therefore identify chemical compounds. The first group includes a variety of methods to identify the elements present, all of which examine the X-rays produced when vacancies in the inner electron shells are filled. These methods vary in how the primary vacancies in the inner electron shell are created. X-ray fluorescence (XRF) uses an X-ray beam to create inner shell vacancies analytical electron microscopy uses electrons, and particle (or proton) induced X-ray emission (PIXE) uses a proton beam. More detailed information on the techniques described here can be found in Ewing (1985, 1997) and Fifield and Kealey (2000). 

A researcher in the field of heterogeneous catalysis, alongside the important studies of catalysts chemical properties (i.e., properties at a molecular level), inevitably encounters problems determining the catalyst structure at a supramolecular (textural) level. A powerful combination of physical and chemical methods (numerous variants x-ray diffraction (XRD), IR, nuclear magnetic resonance (NMR), XPS, EXAFS, ESR, Raman of Moessbauer spectroscopy, etc. and achievements of modem analytical chemistry) may be used to study the catalysts chemical and phase molecular structure. At the same time, characterizations of texture as a fairytale Cinderella fulfill the routine and very frequently senseless work, usually limited (obviously in our modem transcription) with electron microscopy, formal estimation of a surface area by a BET method, and eventually with porosimetry without any thorough insight. 

To characterize dendrimers, analytical methods used in synthetic organic chemistry as well as in macromolecular chemistry can be applied. Mass spectrometry and NMR spectroscopy are especially useful tools to estimate purity and structural perfection. To get an idea of the size of dendrimers, direct visualization methods such as atomic force microscopy (AFM) and transmission electron microscopy (TEM), or indirect methods such as size exclusion chromatography (SEC) or viscosimetry, are valuable. Computer aided simulation also became a very useful tool not only for the simulation of the geometry of a distinct molecule, but also for the estimation of the dynamics in a dendritic system, especially concerning mobility, shape-persistence, and end-group disposition. 

Table 5.2 Summary of selected analytical methods for molecular environmental geochemistry. AAS Atomic absorption spectroscopy AFM Atomic force microscopy (also known as SFM) CT Computerized tomography EDS Energy dispersive spectrometry. EELS Electron energy loss spectroscopy EM Electron microscopy EPR Electron paramagnetic resonance (also known as ESR) ESR Electron spin resonance (also known as EPR) EXAFS Extended X-ray absorption fine structure FUR Fourier transform infrared FIR-TEM Fligh-resolution transmission electron microscopy ICP-AES Inductively-coupled plasma atomic emission spectrometry ICP-MS Inductively-coupled plasma mass spectrometry. Reproduced by permission of American Geophysical Union. O Day PA (1999) Molecular environmental geochemistry. Rev Geophysics 37 249-274. Copyright 1999 American Geophysical Union...

---