Small-area detector

Prompted by the success of the DAC, opposed-anvil cells equipped with large, normally sapphire, anvils have been used in a number of high-resolution diffraction studies that have used classical four-circle diffractometers [187-189] to perform high quality studies to above 2 GPa. The quality of the data is excellent, particularly if collected using small area detectors which became available in the late 1980s [190], and the use of which is now widespread. 

Small-Area Detector. In the collimated beam mode the detector is a small-area single-cell device and the specimen is pointwise scanned, in the manner of conventional light microscopy, to record a single frame for each projection (Fig. 26.43). The advantage is that single-cell Si(Li), or HPGe,... 

FIGURE 26.43 Raster scan imaging with small-area detector. 

Microdiffraction. By concentrating the incident x-ray beam on a small portion of a sample it is possible to get a complete diffraction pattern of very small regions of a sample. Of course, the intensity from such small regions is weak and an area detector that can coUect a large portion of the diffraction pattern at one time makes this appHcation practical. A typical region size is about 50 p.m in diameter. 

FIG. 33 X-Ray Diffraction Patterns of Ammonium Dodecane 1-Sulfonate. 2-D (a) and 3-D plots (b) of oriented samples. Both pictures show the presence of a nonordered smectic phase, since the diffuse, weak, wide-angle diffraction indicates only an average distance between the molecules and the sharp, intense small angle reflections a very well defined layer distance. The reflections are perpendicular to each other, so the structure should correspond to an orthogonal smectic A type. The pictures were obtained using an x-1000 area detector from Siemens. 

Figure 3. Example of XRPD on small Au clusters supported on silica. Total diffraction intensity has been measured with area detector (IP) on BM08-GILDA beamline at the ESRF with A = 0.6211 A and 2min exposure time. Diffraction patterns were collected on Au-supported sample (Exp) and on silica support (Support). Difference patterns, corrected for fluorescence, IP efficiency, etc., are shown (n-Au).

Infrared microscopy combines an optical microscope with an FT-IR spectrometer enabling pico- to femtogram (10 12—10 15 g) quantities of substances to be characterized or very small areas of larger samples to be analysed. Beam-condensing optics focus the radiation onto an area of the sample identified using the optical microscope and either reflectance or transmittance spectra can be recorded. The highly-sensitive MCT detector (p. 283) is normally used as its size can be matched to that of the radiation beam to maximize its response. 

Optical examination of etched polished surfaces or small particles can often identify compounds or different minerals hy shape, color, optical properties, and the response to various etching attempts. A semi-quantitative elemental analysis can he used for elements with atomic number greater than four by SEM equipped with X-ray fluorescence and various electron detectors. The electron probe microanalyzer and Auer microprobe also provide elemental analysis of small areas. The secondary ion mass spectroscope, laser microprobe mass analyzer, and Raman microprobe analyzer can identify elements, compounds, and molecules. Electron diffraction patterns can be obtained with the TEM to determine which crystalline compounds are present. Ferrography is used for the identification of wear particles in lubricating oils. 

Oscillation photography can be used in tandem with area detectors, but detector resolution limits the size of the unit cell from which data can be collected. Large unit cells, such as those of virus capsids, mean small reciprocal unit cells and large numbers of closely spaced reflections. Image plates are commonly used in such cases because of their greater spatial resolution. 

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