MS18-P07 Integrated solutions for most efficient in house high-pressure single crystal experimentsWithin the last decade high pressure studies have received significant increase of interest. Present
typical applications range from the investigation of solid-state organics as part of the pharmaceutical
drug development to the study of rocks and minerals with applied pressures of up to 50 GPa. While in
the past it has been almost impossible to accommodate and extend standard in-house solutions, i.e.
hardware and software, to the needs of high-pressure crystallography, today this picture has changed
completely. Modern high-performance software, such as APEX3, has been developed to address the
intrinsic challenges of high pressure crystallography, particularly with respect to sample alignment,
indexing, data integration and scaling. This complements the significantly higher flexibility available in
the hardware setup. Current instrumentation can easily be used for routine low temperature data
collections, fully optimized with respect to minimizing air scattering and achieving full completeness and
desired data multiplicity. Within just a few minutes the same instrument can be converted into an
optimized solution for high pressure data collection, e.g. for the investigation of organic solid state
material in a diamond anvil cell (DAC). Electronic component recognition ensures automated
reconfiguration and validation of the instrument. This approach avoids invalid and useless configurations
on the one hand, while on the other hand taking the special requirements of a high-pressure experiment
into account. For example, even with the limitations implied by the DAC best possible, completeness and
data redundancy is automatically ensured.
Using a D8 VENTURE with a fixed-chi stage we will demonstrate the advanced hardware capabilities and
processing methods based on the monoclinic polymorph of the sulfonium ylid.
The high flexibility of the D8 VENTURE design will be further demonstrated in the second part of the
presentation: For the investigation of miniscule mineral crystals enclosed in diamond anvil cells,
functionality typically only available at synchrotron facilities has been added to the in-house system.
These features include highly accurate, motorized sample positioning and the ability to monitor intensity
of the X-ray beam passing through diamond anvil cell. The latter is used both for DAC alignment, as well
as for correcting measured intensity data. The availability of online pressure measurements based on
ruby fluorescence completes the extension of the D8 VENTURE, making the system “a little synchrotron
Lab-based experiments up to 50 GPa with synchrotron-sized high-pressure single-crystal samples of even
triclinic symmetry will be presented.References:
Keywords: in-house solution, synchrotron, automation