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scattered dots in x-ray

X-ray techniques

Specialised capabilities for X-ray-based analytical research
The X-ray facility at Sydney Analytical provides specialist capabilities for sample analysis through X-ray diffraction, scattering and spectroscopy techniques.
rainbow x-ray scattering

X-ray scattering

Small angle X-ray scattering (SAXS) and wide-angle X-ray scattering (WAXS) techniques yield structural insights on length scales of 1-200 nm, both in situ and non-destructively. It has thus become an important technique for studying soft, deformable and self-assembled materials, such as those found in drug delivery systems and structural biology. For structural biology, SAXS is a complementary technique to other standard characterisation techniques such as X-ray crystallography, allowing characterisation of structural changes in solution. For drug delivery, SAXS has long been a standard technique for accessing the size, shape and transitions of many common drug delivery vehicles such as micelles, emulsion drops, liquid crystals, vesicles, and microgels. X-ray scattering also is used to study defect structures and pores in metals, ceramics and rocks.

The SAXSpoint is on its way! We expect it will be operational in June 2018.

The SAXSpoint is the latest generation point collimated benchtop SAXS instrument from Anton Paar, which takes advantage of recent advances in both X-ray tube and detector technologies to give both an order of magnitude increase in intensity and an order of magnitude reduction in minimum q. In addition to the capabilities of the SAXSess, the SAXSpoint makes possible benchtop experiments - such as kinetics and grazing incidence SAXS - that were previously only available on synchrotron SAXS lines.

The Anton-Paar SAXSess instrument has a copper X-ray source with two evacuated beamlines: a point collimated beamline that uses image plates and has a q range of 0.2 - 7 nm-1, and a line collimated beamline that uses a CCD camera and has a q range of 0.05 - 7 nm-1. Both beamlines are extendable to q = 40 nm-1 with the use of a wide angle scattering attachment. Both beamlines can be used with a range of samples such as liquids, solutions, pastes, powders, gels and solids. 

The point collimated beamline is optimal for strong scattering samples in the colloidal size domain and is routinely used for the study of concentrated micellar solutions, liquid crystals, suspensions of both organic and inorganic particles, polymers, gels, pastes, ionic liquids and mesoporous materials. The line collimated beamline in optimal for weakly scattering samples. It is routinely used to study solutions of proteins, polymers and micelles.

single crystal x-ray diffraction

Single crystal X-ray diffraction

Single crystal X-ray diffraction (SCXRD) is used to determine the structure of crystalline materials on an atomic scale, using a single sub-millimetre sized crystal. The ordered atoms cause an X-ray beam to be scattered in many different directions, and by measuring the angles and intensities of the diffracted beams the three-dimensional atomic structure of the crystal can be determined.

The Rigaku Oxford Diffraction SuperNova provides a choice of a copper or a molybdenum X-ray source, and is equipped with a large Atlas CCD ‘area’ detector mounted on a four circle goniometer. The shorter wavelength molybdenum source allows higher resolution and reduces absorption effects. The longer copper source is much more intense and facilitates absolute structure determinations for light atom structures. The instrument is equipped with an Oxford Cryosystems Cyrostream 700 Plus liquid nitrogen based cryosystem for low temperature data collections.

This instrument, optimised for data collections from crystals containing relatively small molecules, has a Bruker FR591 molybdenum rotating anode x-ray generator, equipped with a D85 four circle kappa goniometer, a Montel focussing optic and an ApexII CCD area detector, making it the most powerful Mo-based single crystal x-ray diffraction instrument in Australia. Sample screening is facilitated by a Bruker BruNo2 sample mounting robot and the instrument is equipped with an Oxford Cryosystems Cyrostream 700 Plus liquid nitrogen based cryosystem.

This macromolecular single crystal X-ray diffraction instrument is comprised of a dual port Rigaki 007HF copper rotating-anode generator, with each port equipped with an Osmic confocal optic, a Marreseach mardtb ‘desk top beamline’ with Mar 345 image plate detector and an Oxford Cryosystems Cryostream 700 liquid nitrogen based crystal cooling device. The system enables the determination of atomic resolution macromolecular structures ‘in-house’ and the identification of samples that require a synchrotron source.

The following sample environments are offered:

  • Data collections can be undertaken at temperatures between 90 K and 500 K with Oxford Cryosystems Cyrostream 700 Plus liquid nitrogen low temperature data collection systems.
  • Highly volatile samples are routinely mounted at dry ice temperatures. Mounting at lower temperatures is facilitated by an X-Temp2 liquid nitrogen based cryostat.
  • A wide aperture diamond anvil cell for data collections at high pressures of up to 20 GPa (197,385 times Earth’s atmospheric pressure at sea level).

powder x-ray diffraction

Powder X-ray diffraction

Powder X-ray diffraction also measures the structure of crystalline materials, however in this case fine powders or flat solids are used, broadening the application to wide range of materials. Crystal structure, phase composition, and residual stress can be determined.

The Stadi P is the most advanced laboratory powder diffractometer available. Configured with molybdenum or copper X-ray sources, this instrument has two beamlines equipped with accessories to control sample temperature from 12 K to 1000°C:

  • Transmission (Debye-Scherrer) geometry for capillary samples, with Oxford Cryosystems Cryostream (80 – 500 K) and FMB Oxford hot air blower (to 1000°C)
  • Flat-plat (Bragg-Brentano) geometry with Oxford Cryosystems PheniX (to 12 K)

Equipped with a robot sample changer, and configured with a copper X-ray source and Bragg-Brentano geometry, this instrument is ideal for routine powder diffraction measurements.

This instrument, configured with a copper x-ray source and Bragg-Brentano geometry, is equipped with two high temperature stages:

  • Anton-Paar XRK900 vacuum furnace, capable of 900 °C and 10 bar, with a rotating sample holder. This furnace usually operates under a rough vacuum.
  • Anton-Paar HTK2000N vacuum furnace, capable of 2000 °C, with a strip heater.

X-ray spectroscopy

The elemental composition of a specimen can be determined by the characteristic radiation emitted after the sample is excited by X-rays. Two techniques that take advantage of this phenomenon are X-ray Fluorescence (XRF) and X-ray photoelectron spectroscopy (XPS).

The PANalytical energy-dispersive x-ray fluorescence (XRF) bench-top spectrometer performs non-destructive analysis of elements from sodium to uranium, in concentrations from 100% down to ppm levels. This instrument is specifically configured for the analysis of heavy metals.

The Thermo Fisher Scientific K-Alpha+ instrument for x-ray Photoelectron Spectroscopy and Ultraviolet Photoelectron Spectrscopy (XPS/UPS) is currently managed by the Vibrational Spectroscopy facility, and is located in the Sydney Nanoscience Hub.