Introduction to the Service Facility

This laboratory provides the school with a complete structural chemistry service. Located on the ground floor on Noyes Laboratory, the 3M Materials Chemistry Laboratory is housed in 2,700 square feet of space and staffed by two crystallographers. State-of-art hardware and software systems allow for detailed X-ray analysis of materials from minerals to macromolecules.

The x-ray facility performs a wide variety of experiments including small and wide angle x-ray scattering, in addition to powder, fiber, and single crystal x-ray diffraction. This facility helps maintain structural database systems that provide electronic search, retrieval, analysis, data, and graphics for inorganic, organic, and macromolecular structures. Facility personnel help investigators correlate x-ray diffraction results with other single crystal and bulk sample experiments including laser, EPR, NMR, and microwave. The staff also offers instruction covering x-ray diffraction experiments from design and data collection to analysis and presentation of results. Experimental data for research groups is routinely provided in less than one week. Alternatively, faculty, staff, students, and visitors are welcome to use facility equipment to collect their own data.

The George L. Clark X-Ray Facility is the x-ray diffraction and scattering component of the Center for Complex Structures. The laboratory maintains several experimental systems.

 

Experimental Systems

  • The first is a Bruker D8 Venture Duo This dual source system is equipped with a four-circle kappa-axis diffractometer and motorized Photon 100 CMOS detector capable of shutter-less data collection.  This state-of-the-art multipurpose system used Cu or Mo radiation and is primarily used for variable temperature, single crystal experiments on samples with a minimum dimension of 0.01mm.  The system is also available for absolute structure determination of organics, wide-angle, powder, film, and fiber x-ray diffraction experiments on samples ranging from minerals to macromolecules.
  • The second system is a Bruker X8ApexII (APEX). The system is equipped with a four-circle kappa-axis diffractometer and motorized ApexII CCD detector. This state-of-the-art system uses Mo radiation and is primarily used for variable temperature, single crystal experiments on samples with a minimum dimension of 0.01mm.
  • The third system is a Rigaku Miniflex 600powder x-ray diffraction system.  The benchtop powder X-ray instrument is set up to collect PXRD in reflection mode with a 2θ scan range of 3° to 120°.  The instrument uses Cu radiation and a wide area scintillation counter detection system.  The instrument is operated at the maximum power 600W (40kV – 15mA) and data collection scans can be continuous or step-wise.  A variety of sample preparation techniques can be used and we have three zero background single crystal quartz sample holders.  The system is available for wide-angle, powder, and film x-ray diffraction experiments on samples ranging from minerals to macromolecules.

Additional systems are available for designer experiments that require unusual physical environments or peripherals. These user-designed systems perform very specialized experiments, like measuring molecular geometry as a function of temperature, pressure, or fluid properties.

Separately and in various combinations these systems have inspired a new generation of questions about molecular geometry in solids, liquid crystals, colloids, and solutions. Scientists in disciplines ranging from physics to food science are taking advantage of the expanded spectrum of x-ray diffraction and scattering experiments currently available.