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X-Ray Diffraction Laboratory

X-ray crystal structure determination is an important technique for most inorganic and organic chemists. The X-ray Diffraction Laboratory at UMSL supports the research programs of several research groups in the department. Also, we collaborate with a number of groups elsewhere in the USA and in other countries in their solid-state structure determination research. The Laboratory is equipped with state-of-the-art instrumentation and computational facilities for solid state three dimensional crystal and molecular structure determinations. The facility is located in custom-designed laboratory space in the Center for Nanoscience, opened in November 1996, and currently houses single crystal and powder diffractometers.

For more information please contact Dr. Nigam Rath at (314) 516-5333 or by email: rathn@umsl.edu

SINGLE CRYSTAL X-RAY DIFFRACTION INSTRUMENTATION

The Bruker Venture-Duo PHOTON-II Kappa Diffractometer is the state-of-the art single crystal instrument purchased with funding from NSF in 2019. This instrument is equipped with two Incotec micro-focus X-ray sources (Cu and Mo) and a PHOTON-II CPAD (Charge-integrating Pixel Array Detector) detector. Shutter-less, very fast data collections can be carried out using this Kappa geometry diffractometer at 100-300K using the Oxford Cryostream-800 low temperature device. Structure determination of all weakly diffracting samples and most research samples are carried out using this system.

 

 NEw XRD 2019

 

The Bruker APEX II Kappa Dffractometer is equipped with an Oxford Cryostream low temperature device. Fast data collections can be carried out using this Kappa geometry diffractometer equipped with a 4K CCD (Charge Coupled Device) chip at 100-300K. This instrument uses a sealed tube Mo x-ray source. Currently, this diffractometer is primarily used for teaching and user training.

 

The Bruker APEX II Kappa Dffractometer

 


POWDER DIFFRACTION INSTRUMENATION

A Rigaku Ultima IV Powder Diffractometer is used primarily for bulk material characterization, including air- and moisture-sensitive samples. This provides a valuable analytical tool for the identification of single and multi-component solids by comparison with known published powder patterns. It is also used to determine the homogeneity of crystalline samples from which single crystals have been used for crystal structure determination. This instrument is also capable of data collection for small angle x-ray scattering (SAXS) experiments.

 

A Rigaku Ultima IV Powder Diffractometer

 

COMPUTER FACILITIES AND OTHER INSTRUMENTATION

The X-ray Laboratory Computing Facility has several workstations running crystallographic software. All computers in the lab are integrated with the university computer network. The Cambridge Structural Database is available to all students, faculty and staff for their teaching and research projects.

The sample preparation laboratory is equipped with stereo microscopes with digital video capabilities for screening and mounting crystals; fume hood, refrigerator and freezer for crystallization and sample storage, together with other necessary facilities for crystallization and crystal handling.