he X-ray diffraction laboratory is housed within the Department of Chemistry, Room 107. Two types of diffraction services available:
- diffraction spectra of powder (microcrystalline materials) and films
- single crystal diffraction data
Instrumentation
The XRD system is a Rigaku rotating anode (Ru-2000) X-ray diffractometer. It generates high intensity X-rays with a wavelength of 1.54 A (Cu-anode) at a line focus. There is a secondary beam graphite monochromator and a scintillation counter detector. The maximum power is 8 kW (40 kV and 200 mA). The software for data collection and analysis is MDI's JADE and DATASCAN. The JCPDS powder diffraction database is available for search/match and archival information on the computer associated with driving the XRD instrument.
At all times safety is paramount in operating this equipment. Only qualified users may have access to this instrument. New users must pass the radiation safety class conducted at the WSU Health Physics department (7-9505) and receive a radiation monitoring dosimeter badge. This badge must be exchanged according to WSU's Health Physics calendar and worn at all times in the X-ray lab. Basic training in the use of the instrument is given by M.J.Heeg (7-2587) by appointment only. The use of the XRD is restricted to normal working ours. Weekend use is possible with advance permission and the guaranteed presence of someone expressed approved for independent operation and maintenance, along with the user, at all times.
The single crystal diffractometer is a Bruker APEXII/Kappa installed in Apr 2004. It currently produces MoK radiation from a conventional tube and is equipped with a graphite monochromator and APEX-II detector. The low temperature option is routinely used at 100 K at the sample site. Single crystals in size ranging from 0.2 mm to 0.002 mm are optimal. The GADDS option for collecting powder diffraction data on this instrument has been purchased but not yet delivered by the manufacturer.
The APEX diffractometer is currently accessible only through M.J.Heeg as the operator. Samples may be submitted at Lab 107 during normal working hours. The successful completion of a project generally involves the complete data collection and refinement to generate a crystal structure report suitable for publication. It is possible to request data collection without processing and this data can be emailed to persons adept at crystal structure analyses.
All X-ray equipment in WSU's CIF X-ray laboratory is licensed by the State of Michigan and under continual monitoring by WSU's Health Physics.
