Empyrean Series 3 Pre-Installation manual
Version number: 3
Overview
The Empyrean Nano edition is a hybrid laboratory X-ray scattering instrument. It uniquely enables a variety of techniques for the structural characterization of (nano)materials on multiple length scales. Applications include:
- SAXS and WAXS: Small-and wide-angle X-ray scattering
- Bio-SAXS: SAXS on biological macromolecules
- USAXS: Ultra small-angle X-ray scattering
- Total scattering: Atomic pair distribution function (PDF) analysis
Several other applications, such as powder diffraction, thin film analysis, and CT can be included. These can also be added later as upgrades.
The high performance and flexibility of the instrument are driven by a high-resolution goniometer platform, a modular concept, and the latest detector technology.
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(Nano)material analysis on multiple length scales
Like no other lab instrument on the market, the Empyrean Nano edition covers Bragg spacings from sub-Ångströms to microns and a scattering vector q-range spanning over almost five decades - without any gaps.
The combination of USAXS with SAXS/WAXS and PDF measurements on the Empyrean Nano edition uniquely enables for the characterization of hierarchical structures on multiple length scales, covering Bragg spacings from sub-Ångström to micron(s).
Key applications
Empyrean supports variety of X-ray scattering techniques:
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- SAXS (Small-angle X-ray scattering)
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SAXS is the main application on the Empyrean Nano edition. It is one of the most versatile tools to analyze nanoscale structures and dimensions on a variety of sample types (liquids, powders, solids, gels, etc). Samples may be amorphous, crystalline or semi-crystalline.
Typical samples that can be investigated with SAXS include colloidal dispersions, surfactants, polymers, biomacromolecules, membranes, nanocomposites, nanopowders and porous materials. The orientation of anisotropic nanoscale structures can be investigated by measuring 2D SAXS patterns.
- Bio-SAXS (SAXS on biomacromolecules)
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Small-angle X-ray scattering applied to dilute protein solutions has become an accepted and rapidly growing structural biology technique. It provides information e.g. about the overall protein size and shape, folding and unfolding, aggregation behavior, stability and molecular weight.
Measurements can be done under near native conditions, and under variation of e.g. protein concentration, pH, ionic strength or temperature. SAXS ultimately also allows for a low-resolution molecular shape envelope reconstruction and thus delivers information that is complementary to that obtained from single crystal XRD or NMR.
Malvern Panalytical's EasySAXS software is available for basic bio-SAXS data analysis. Data can be exported in a format that is compatible with the EMBL ATSAS software, which can be used for 3D protein shape reconstruction and other advanced tasks.
- WAXS (Wide-angle X-ray scattering)
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Based on the diffraction pattern measured at the higher angles one can identify and quantify crystalline phases that are present in a given sample, as well as estimate the size of nanocrystallites.
The orientation of the crystal lattice in anisotropic structures, e.g. in polymers, can be investigated by measuring 2D WAXS patterns.
- USAXS (Ultra-small-angle X-ray scattering)
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For the characterization of samples containing particles or structural features in the size range of several hundreds of nanometers the resolution of a conventional SAXS setup is insufficient.
On the Empyrean Nano edition high-resolution optics in combination with the high-resolution goniometer enable for accessing ultra-small angles, down to as low as 0.005 deg 2theta.
The characteristic oscillations in the scattering curve from highly monodisperse particles can be readily resolved, even with a particle diameter as large as 1.5 µm.
- Total scattering
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Total scattering experiments use hard X-ray radiation and scans up to very high 2theta angles so as to acquire data up to highest possible scattering vectors. From the deduced atomic pair distribution function (PDF) the short-range atomic order in nanocrystalline and disordered materials can be deduced.
The Empyrean Nano edition equipped with the GaliPIX3D detector and with effective anti-scatter devices enables for obtaining very high-quality experimental data, and optionally under non-ambient conditions. Results are in good agreement with those that are obtained at synchrotron radiation facilities.
- Additional applications - inclusions or upgrades
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Depending on your specific research interest the Empyrean Nano edition can be further upgraded, e.g. by adding thin film techniques such as GISAXS and X-ray reflectivity, classical powder X-ray diffraction or computed tomography.
Malvern Panalytical also constantly develops additional options, improvements and analytical solutions that are back-compatible with the existing Malvern Panalytical instrument platforms.
Features
Maximum flexibility
The unique flexibility to easily and quickly configure the Empyrean Nano edition for the different X-ray scattering techniques is enabled by a 2-circle goniometer platform on which quickly interchangeable, pre-aligned X-ray modules (PreFIX) and sample stages can be mounted.
Whereas SAXS measurements can be readily done with a static detector, the goniometer comes into play for accessing the extended angular range that is required for WAXS and ultimately for total scattering (PDF) measurements.
With a smallest 2theta step width of 0.0001 deg the high-resolution goniometer also readily supports the USAXS application. For accessing highest possible scattering vectors, the standard Cu X-ray tube can be easily exchanged against a Ag or Mo one.
High-performing detectors
The performance of the X-ray detector is critical for obtaining high-quality X-ray scattering data.
Our hybrid pixel area detectors, GaliPIX3D and PIXcel3D, excel by their very low intrinsic noise and a high dynamic range. Their high spatial resolution enables for experimental setups that are rather compact and conveniently fit within the 240 mm goniometer radius.
The GaliPIX3D detector, having 100% absorption efficiency for Cu, Mo and Ag radiation, is the detector of choice when you want to perform not only SAXS/WAXS but also fast PDF measurements.
SAXS/WAXS with ScatterX78
With the ScatterX78 module, you can perform small- and wide-angle X-ray scattering (SAXS/WAXS) measurements on nanomaterials.
The SAXS signal allows for the dimensional and structural analysis of a material on the nanoscale. Complementary information about the crystalline phases, the size of nanocrystallites and their orientation can be obtained from the WAXS signal. ScatterX78 can be used for the characterization of a variety of samples, such as colloidal dispersions, polymers, protein solutions, surfactants, nanopowders and liquid crystals.
USAXS option for ultimate small-angle resolution
On the Empyrean Nano edition the resolution can be pushed to ultra-small angles by using a Bonse-Hart type of experimental setup based on pre-aligned, high-resolution optical components.
With such a USAXS setup the smallest accessible scattering angle is approximately 0.005°, with a corresponding largest Bragg spacing of 1700 nm.
Easily accessible, radiation-safe enclosure
The Empyrean Nano edition meets all relevant worldwide regulations regarding electrical, mechanical and X-ray safety, by default also for hard X-rays.
The experimental setup is within a radiation-safe enclosure that has large see-through windows.
Wide-opening doors enable for easy access to the setup when required.
If I moved to another company, and have chance to purchase, Empyrean would be the one.
Raeann Wu — Teva Pharmaceuticals
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