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X-Ray Crystallography

Data collection, structure analysis, and crystallography consultation services.

 

Major Equipment

  • Panalytical Empyrean Powder X-ray diffractometer. Installed May 2016. Equipped with both parallel beam and focusing optics and a high speed PIXcel 3D Medipix detector for analysis of powders, multicrystalline materials and thin films. Users can choose between a reflection/transmission spinner for collection of data in Bragg Brentano mode, a capillary transmission spinner for use with a parallel beam, a five axis cradle stage for analysis of thin films and mapping, or a high temperature stage and vacuum system for measurements up to 1000 °C and/or under inert gases. Domed sample cups available for easy analysis of air sensitive materials. ICDD and ICSD databases are available.

  • Installed December 2016: Bruker D8 Quest Single Crystal Diffractometer with Mo sealed tube and curved triumph monochromator with a 10 cm x 10 cm Photon-100 detector and fixed chi angle. Equipped with an Oxford Cryostream 800 plus variable temperature device (80-500K). This instrument is ideal for fast, high throughput data collection of well to weakly diffracting samples, and for heavily absorbing samples. Typical samples include metal-organic complexes, metals, ceramics, well diffracting organic crystals. For software, procedures and publication items see here.
  • Installed December 2016: Bruker D8 Quest Single Crystal Diffractometer with Cu microsource, laterally graded X-ray optics (Goebel mirror) and kappa geometry, equipped with a Photon-II detector (10 cm x 14 cm). Equipped with an Oxford Cryostream 800 variable temperature device (80-400K). Featuring a copper radiation microsource this instrument is ideal for samples that are very weakly diffracting, for very small crystals (< 0.1 mm), and for determination of absolute structure of organic compounds (no atoms heavier than fluorine). For software, procedures and publication items see here. The instrument can also be used for powder XRD analysis when only very small sample amounts are available, or for WAXS-like analysis of solid samples.
  • Installed August 2019: Malvern Panalytical Epsilon 4 benchtop energy dispersive X-ray fluorescence (XRF) spectometer for elemental analysis from fluorine (F) to americium (Am). For bulk and trace analysis of inorganic and organic-inorganic hybrid materials, minerals, building materials as well as trace element analysis in oils and fuels, polymers, plastics, food, pharmaceuticals cosmetics and the environment. It handles a wide variety of sample types, including solids, pressed and loose powders, liquids and filters and performs non-destructive quantitative analysis in concentrations from 100% down to sub-ppm levels (for heavier elements), on samples weighing anything from a few milligrams to kilograms. Elemental screening and element ratios are available using the Omnian standardless analysis solution. The Ag anode X-ray tube guarantees best performance of P, S and Cl analysis. The spectrometer features a 10-position removable sample changer and can accommodate samples up to 52 mm (2 inch) in diameter.
  • Binder Model FD23 programmable drying and heating oven for hydrothermal synthesis as well as growing and drying of single crystals and powder samples. Temperature range from 5°C above ambient to +300 °C, forced convection, adjustable exhaust air flap, controller timer functions, interior lighting. 11.82 x 8.75 in (height 13 in), 0.7 cu.ft. 1-10 °C/min heating ramp. When working at hydrothermal conditions users need to provide pressure save autoclave reactors.

 

Other Resources on site

  • Computers for data processing and structure refinements.
  • Single Crystal and Powder XRD databases: CSD (Cambridge Structural Database), ICDD (data bases of the International Center for Diffraction Data), ICSD (Inorganic Crystal Structure Database).
  • Sample preparation tables for packing and mounting of powder and single crystal XRD samples.
  • Carl Zeiss Discoery.V8 crystal mounting microscope on a dedicated crystal mounting table with adjustable eyepieces and a magnification range between 10 and 80 times. Equipped with a digital camera and large video screen.
  • Carl Zeiss AxioCam crystal mounting microscope. This microscope is placed inside a chemical fumehood for save handling of volatile solvents and samples.
  • Fridge/freezer, fumehood and flammable cabinet for save storage and handling of crystal specimens.

Purdue University, West Lafayette, IN 47907 (765) 494-4600

Department of Chemistry, 560 Oval Drive, West Lafayette, Indiana 47907-2084 | Telephone: (765) 494-5200 | Fax: (765) 494-0239

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