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Advantages of SR-XRPD

Solid state forms of complex molecular structures have diffraction patterns characterized by many and overlapped reflections. In such cases, data interpretation can be quite demanding and explains why for many years XRPD has been almost uniquely employed as a fingerprinting technique, both for qualitative and quantitative assessments.

During the last 10-15 years, an impressive development in instrumentation, computer technology and powder diffraction experimental techniques [13,14] and methodologies [15-22] took place, which upgraded XRPD from a support technique to a fundamental one. Furthermore, the recent development of total scattering techniques (i.e. techniques that interpret both Bragg and diffuse elastic scattering) has extended the use of powder diffraction to nano- or non-crystalline (i.e. liquid and amorphous) materials [23-25].

 

SR-XRPD has major advantages over laboratory XRPD

 

  • High photon wavelength resolution (∆λ/λ better than 2.10-4)
  • Highly collimated (residual divergence less than 20 μrad) and intense (> 1013photon/sec) photon beam
  • Tunable photon energy ideal to perform anomalous scattering experiments, collect fluorescence-free XRPD data and better diffraction peaks separation.
  • Angular (FWHM) resolution better than 0.01° 2θ obtained with new generation solid state microstrip detectors (e.g. MYTHEN II detector developed at the Swiss Light Source and available to Excelsus) and down to 0.002° 2θ using multicrystal analyser detectors
  • d-spacing resolution better than 0.35 Ǻ
  • Millions count counting statistics in reflection (Bragg-Brentano) as well as in transmission (Debye-Scherrer) modes even with low quantities of powder available
  • Reduced preferential orientation effects due to transmission geometry and very high-frequency sample spinning (>10 Hz)
  • Ultra-fast data acquisition (milliseconds scale) for efficient, dose-controlled and time-resolved XRPD
  • Very high signal-to-noise and signal-to-background
  • Very high counting statistics (millions of counts) in seconds/minutes

 

 

 

In conclusion

 

Laboratory XRPD is suitable for routine and structural analyses of medium difficulty. However, the identification of polymorphs with similar structure, their quantification in complex mixtures or the detection of low levels of impurities (less than a few %) require SR-XRPD.

The experimental artefacts that characterize laboratory XRPD prevent it in such cases to ascertain the structural and microstructural properties of pharmaceutical compounds [4, 22, 23]. Furthermore, SR-XRPD allows the detection of unexpected structural changes or unknown forms during manufacturing conditions, e.g. in the field of pharmaceuticals, kinetic studies at the msec scale and the application of XRPD to more complex systems, e.g. biologicals molecules.

Bibliography

 

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