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X-ray Powder Diffraction:exposing the bare bones of solid forms

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The theory of powder diffraction X-ray Powder Diffraction. Instrumentation. Sources of error. Applications. Case studies.

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X-ray Powder Diffraction: exposing the bare bones of solid forms Dr. Noel Hamill
Welcome ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Contents ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Theory ,[object Object],[object Object],Bragg’s law: n  =2dsin  Constructive interference is detected when the path-length difference is equal to an integer number of wavelengths
Diffraction by crystal planes crystalline amorphous θ ~ 20º x-rays in x-rays out top of sample θ ~ 5º x-rays in x-rays out top of sample
Diffraction from powders ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
X-ray Powder Diffraction ,[object Object],[object Object],[object Object],[object Object]
X-ray Diffractometer ,[object Object],[object Object],Reflection mode (Bragg-Brentano geometry)
Transmission mode ,[object Object],[object Object],[object Object],[object Object]
Instrument capabilities ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Sources of error ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Sample Displacement Error ,[object Object],[object Object],sample focal plane Chen et al J. Pharm. Biomed. Analysis 2001 , 26 , 63 Incident X-rays peak shift Diffracted X-rays
Preferred Orientation ,[object Object],[object Object],[object Object],random orientation realistic orientation
Preferred Orientation calculated acetaminophen XRPD pattern (refcode HXACAN01) XRPD pattern from the (100) face of manually oriented acetaminophen single crystals (Wen et al J. Phys. Chem. B 2004 , 108 , 11219)
Particle Statistics ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Reducing measurement errors ,[object Object],[object Object],[object Object]
Applications ,[object Object],[object Object],[object Object],[object Object],[object Object]
Crystallinity
Phase identification ,[object Object],[object Object],[object Object],[object Object],erythromycin A R = OH erythromycin B R = H Stephenson et al J. Pharm. Sci. 1997 , 86 , 1239
Polymorph detection ,[object Object],[object Object],A D E
Unit cell indexing ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Crystal structure by XRPD ,[object Object],[object Object],[object Object],[object Object]
Mixture analysis Patterns are additive 5000 10000 Counts Position [°2Theta] 15 20 25 30 Position [°2Theta] 10 15 20 25 30 Counts 2000 4000 Crystalline Form A Crystalline Form B Amorphous Resulting XRD pattern Multi-phase sample
Quantitative analysis ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Method development & validation ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],Transmission
Method validation issues ,[object Object],[object Object],[object Object],[object Object]
Thank you for your time… ..any questions?

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X-ray Powder Diffraction:exposing the bare bones of solid forms

  • 1. X-ray Powder Diffraction: exposing the bare bones of solid forms Dr. Noel Hamill
  • 2.
  • 3.
  • 4.
  • 5. Diffraction by crystal planes crystalline amorphous θ ~ 20º x-rays in x-rays out top of sample θ ~ 5º x-rays in x-rays out top of sample
  • 6.
  • 7.
  • 8.
  • 9.
  • 10.
  • 11.
  • 12.
  • 13.
  • 14. Preferred Orientation calculated acetaminophen XRPD pattern (refcode HXACAN01) XRPD pattern from the (100) face of manually oriented acetaminophen single crystals (Wen et al J. Phys. Chem. B 2004 , 108 , 11219)
  • 15.
  • 16.
  • 17.
  • 19.
  • 20.
  • 21.
  • 22.
  • 23. Mixture analysis Patterns are additive 5000 10000 Counts Position [°2Theta] 15 20 25 30 Position [°2Theta] 10 15 20 25 30 Counts 2000 4000 Crystalline Form A Crystalline Form B Amorphous Resulting XRD pattern Multi-phase sample
  • 24.
  • 25.
  • 26.
  • 27. Thank you for your time… ..any questions?