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Geochemical Instrumentation and Analysis Integrating Research and Education > Geochemical Instrumentation and Analysis > Browse Collection > Single-crystal X-ray Diffraction
1/25/13
Single-crystal diffractometers use either 3- or 4-circle goniometers. These circles refer to the four angles (2, , , and ) that define the relationship between the crystal lattice, the incident ray and detector. Samples are mounted on thin glass fibers which are attached to brass pins and mounted onto goniometer heads. Adjustment of the X, Y and Z orthogonal directions allows centering of the crystal within the X-ray beam. X-rays leave the collimator and are directed at the crystal. Rays are either transmitted through the crystal, Schematic of 4-circle diffractometer; the reflected off the surface, or diffracted angles between the incident ray, the detector by the crystal lattice. A beam stop is and the sample. Details located directly opposite the collimator to block transmitted rays and prevent burn-out of the detector. Reflected rays are not picked up by the detector due to the angles involved. Diffracted rays at the correct orientation for the configuration are then collected by the detector. Details for processing. M odern single-crystal diffractometers use CCD (charge-coupled device) technology to transform the X-ray photons into an electrical signal which are then sent to a computer
Applications
Single-crystal X-ray diffraction is most commonly used for precise determination of a unit cell, including cell dimensions and positions of atoms within the lattice. Bond-lengths and angles are directly related to the atomic positions. The crystal structure of a mineral is a characteristic property that is the basis for understanding many of the properties of each mineral. Specific applications of single-crystal diffraction include: New mineral identification, crystal solution and refinement Determination of unit cell, bond-lengths, bond-angles and site-ordering Characterization of cation-anion coordination Variations in crystal lattice with chemistry With specialized chambers, structures of high pressure and/or temperature phases can be determined Determination of crystal-chemical vs. environmental control on mineral chemistry Powder patterns can also be derived from single-crystals by use of specialized cameras (Gandolfi)
Limitations
M ust have a single, robust (stable) sample, generally between 50250 microns in size Optically clear sample Twinned samples can be handled with difficulty Data collection generally requires between 24 and 72 hours
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this must be corrected for during absorption corrections to the data. S ample Mounting Samples are mounted on the tip of a thin glass fiber using an epoxy or cement. Care should be taken to use just enough epoxy to secure the sample without embedding it in the mounting compound. The fiber may be ground to a point to minimize absorption by the glass. This fiber is attached to a brass mounting pin, usually by the use of modeling clay, and the pin is then inserted into the goniometer head. S ample Centering The goniometer head and Goniometer head. Details sample are then affixed to the diffractometer. Samples can be centered by viewing the sample under an attached microscope or video camera and adjusting the X,Y and Z directions until the sample is centered under the cross-hairs for all crystal orientations.
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Literature
The following literature can be used to further explore Single-crystal X-ray Diffraction Campana, C.F., Bruker Analytical Application Note Putnis, A. (1992). Introduction to Mineral Sciences. Cambridge, UK: Cambridge University Press. Chapter 3 (pp. 41-80).
Related Links
For more information about Single-crystal X-ray Diffraction follow the links below. X-ray Crystallography from the Bunsen Learner, University of Edinburgh. An Introduction to the Scope, Potential and Applications of X-ray Analysis, from the International Union of Crystallography American M ineralogist Crystal Structure Database International Centre for Diffraction Data X-ray Powder Diffraction--USGS Publication X-ray Instruments--University of California, Santa Barbara Crystallography Clearinghouse--IUCR Reciprocal Net--part of the National Science Digital Library. Use the "Learn About" link to find animations of the structures of common molecules (including minerals), crystallography learning resources (tutorials, databases and software), resources on crystallization, and tutorials on symmetry and point groups.
serc.carleton.edu/research_education/geochemsheets/techniques/SXD.html
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