Diffraction instrumentation

The other type of x-ray source is an electron syncluotron, which produces an extremely intense, highly polarized and, in the direction perpendicular to the plane of polarization, highly collimated beam. The energy spectrum is continuous up to a maximum that depends on the energy of the accelerated electrons, so that x-rays for diffraction experiments must either be reflected from a monochromator crystal or used in the Laue mode. Whereas diffraction instruments using vacuum tubes as the source are available in many institutions worldwide, there are syncluotron x-ray facilities only in a few major research institutions. There are syncluotron facilities in the United States, the United Kingdom, France, Genuany and Japan. 

Present day techniques for structure determination in carbohydrate chemistry are sub stantially the same as those for any other type of compound The full range of modern instrumental methods including mass spectrometry and infrared and nuclear magnetic resonance spectroscopy is brought to bear on the problem If the unknown substance is crystalline X ray diffraction can provide precise structural information that m the best cases IS equivalent to taking a three dimensional photograph of the molecule... 

Another approach to multielemental analysis is to use a multichannel instrument that allows for the simultaneous monitoring of many analytes. A simple design for a multichannel spectrometer consists of a standard diffraction grating and 48-60 separate exit slits and detectors positioned in a semicircular array around the diffraction grating at positions corresponding to the desired wavelengths (Figure 10.50). 

Instrumental Methods for Bulk Samples. With bulk fiber samples, or samples of materials containing significant amounts of asbestos fibers, a number of other instmmental analytical methods can be used for the identification of asbestos fibers. In principle, any instmmental method that enables the elemental characterization of minerals can be used to identify a particular type of asbestos fiber. Among such methods, x-ray fluorescence (xrf) and x-ray photo-electron spectroscopy (xps) offer convenient identification methods, usually from the ratio of the various metal cations to the siUcon content. The x-ray diffraction technique (xrd) also offers a powerfiil means of identifying the various types of asbestos fibers, as well as the nature of other minerals associated with the fibers (9). 

The final set of magnetic lenses beneath the specimen are jointly referred to as post-specimen lenses. Their primary task is to magnify the signal transferred by the objective lens. Modern instruments typically contain four post-specimen lenses diffraction, intermediate, projector 1, and projector 2 (in, order of appearance below the specimen). They provide a TEM with its tremendous magnification flexibility. 

The STEM instrument itself can produce highly focused high-intensity beams down to 2 A if a field-emission source is used. Such an instrument provides a higher spatial resolution compositional analysis than any other widely used technique, but to capitalize on this requires very thin samples, as stated above. EELS and EDS are the two composition techniques usually found on a STEM, but CL, and even AES are sometimes incorporated. In addition simultaneous crystallographic information can be provided by diffraction, as in the TEM, but with 100 times better spatial resolution. The combination of diffraction techniques and analysis techniques in a TEM or STEM is termed Analytical Electron Microscopy, AEM. A well-equipped analytical TEM or STEM costs well over 1,000,000. 

The major STEM analysis modes are the imaging, diffraction, and microanalysis modes described above. Indeed, this instrument may be considered a miniature analytical chemistry laboratory inside an electron microscope. Specimens of unknown crystal structure and composition usually require a combination of two or more analysis modes for complete identification. 

Measurements of surface disorder require a high resolving power (the ability to distinguish two close-lying points in the diffraction pattern). Quantitative measurements of surface disorder are limited in the following manner, the worse the resolving power, the smaller the maximum scale of surface disorder that can be detected. For example, if the maximum resolvable distance of the diffractometer is 100 A, then a surface that has steps spaced more than 100 A apart will look perfect to the instrument. The theoretical analysis of disorder is much simpler than that for atomic positions. 

In electron-optical instruments, e.g. the scanning electron microscope (SEM), the electron-probe microanalyzer (EPMA), and the transmission electron microscope there is always a wealth of signals, caused by the interaction between the primary electrons and the target, which can be used for materials characterization via imaging, diffraction, and chemical analysis. The different interaction processes for an electron-transparent crystalline specimen inside a TEM are sketched in Eig. 2.31. 

Instrument Based on Fraunhofer Diffraction of Laser Light... 

A laser diffraction spectrometer can measure particles as small as 0.2 pm and up to about 1000 pm. Some instruments allow the operation of the analyzer for... 

Heuer, M. and Lesclioiiski, K., 1985. Results obtained with a new instrument for the measurement of particle size distributions from diffraction patterns. Particle Characterisation, 2, 7-15. 

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