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Simultaneous XRD-DSC – the sum is much greater than the parts:

Almost all analytical labs supporting the Pharmaceutical industry will have both Thermal analysis tools and X-ray powder diffraction. So, what is the benefit of combining simultaneous DSC and XRD measurements into a single attachment. It turns out that having the simultaneous thermal and powder data on the same sample yields a wealth of information that is often not easily accessible using each analytical technique separately. In addition to a discussion on the system itself, some of the benefits that will be introduced include:

  1. The DSC – XRD data are collected on the same sample at the same time so unusual thermal events can be directly associated with a powder pattern to assess any structural changes, and conversely, unusual changes in the powder pattern can be associated with a thermal trace to determine if the changes are truly structural (polymorphic) or just preferred orientation or ripening.
  2. Broad thermal events like re-crystallization can contain multiple transitions through various metastable polymorphs. Using the thermal trace as a guide, more detailed XRD scans can be performed to tease out metastable polymorph structure and powder pattern fingerprints. This can be a rapid screening approach for novel solid forms.
  3. The XRD-DSC unit also has controlled humidity which can be used to quickly bracket stability and storage conditions for APIs, intermediates, and drug products. In addition to opening a huge playground of thermodynamic conditions for solid form investigation.


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Simon Bates | VP of Science and Technology

Rigaku Americas Corporation | Texas, USA

Simon Bates is V.P. of Science and Technology at Rigaku Americas Corp., where he nurtures collaborative relationships between industry partners and academia in the discovery of new technologies and methodologies for the next generation analytical systems. His fascination with materials science and analytics has led Dr. Bates on an interesting career path. Having received his Ph.D. from the University of Hull for his neutron diffraction studies on the magnetic properties of rare earth materials, Dr. Bates completed his postdoctoral work at the University of Edinburgh where he first started to design and build specialized high resolution X-ray diffraction system for materials characterization. He continued working on X-ray analytical systems and software design throughout his career at Philips, Shimadzu (Kratos), Bede Scientific, and Rigaku. However, before joining Rigaku, Dr. Bates explored a different career direction and spent 17 years working in pharmaceutical contract research at SSCI and then Triclinic Labs., where he expanded his toolkit for materials analysis to embrace thermal methods and IR/Raman spectroscopy while experimenting in organic chemistry and molecular modeling. Dr. Bates has continued his relationship with academia, volunteering as an Adjunct Professor at Purdue University, University of Hawaii Hilo and more recently at the University of Long Island. Want to learn more? Connect with Simon on LinkedIn.