X-ray Diffraction Studies

X-ray powder diffraction (XRPD) is a powerful tool for the study of (partially) crystalline materials. Each crystalline material shows a distinct X-ray diffraction pattern due to the differences in the crystalline lattice parameters, different atom types and/or different packing of molecules.

Using diverse types of geometries (reflection or transmission) or sample stages (eg. humidity chamber, capillary spinner) the XRD scientist has a variety of analytical tools to find the best measurement conditions to answer specific questions.

Solvias offers a broad range of different X-ray powder diffraction techniques in combination with a long experience in analysis of API’s.

Certification

  •  ISO 9001, SQS 11237-04
  • GMP Compliance

 

XRPD instruments:

ModelGeometryStagesDetector
Bruker D8 AdvanceReflectionSpinnerLynxEye
STOE Stadi PReflection/TransmissionSpinner, Capillary spinnerMythen 1K
PANalytical X’Pert PRO-MPD*Reflection/TransmissionWell plates, TTK with temperature and humidity controlPixcel Detector

 *ISO measurements only

 

XRPD applications:

  • Analysis of Solids and Powders
  • Analysis of highly active samples in safety cell on the Stoe instrument in transmission mode (up to Safebridge class OEB 3, OEB 4 on request)
  • Temperature and humidity dependent XRPD studies in order to elucidate the stability of polymorphs or hydrates
  • Transmission geometry, capillary spinner: best suited for high resolution analysis, structure solution, polymorph identification and indexing
  • Reflection geometry: also suited for the estimation of amorphous contents
  • High-throughput diffraction analysis of micro titre well plates
  • Indexing of XRPD pattern can help to determine whether the analyzed sample represents a pure phase. Indexing is also a first step towards the structure solution out of powder diffraction data
  • Calculated powder pattern from single crystal data (provided by customer) can be compared with experimental pattern. Solvias uses several programs to calculate XRPD pattern
  • Rietveld refinement can be applied to quantify different crystalline components of mixtures which show a high degree of peak overlap. Prerequisite: the crystal structures of the components must be known

 

XRPD software:

  • Diffrac Suite (GMP/ISO), Bruker AXS, Germany
  •  HighScore Plus (GMP/ISO), PANalytical, The Netherlands
  • WinXPOW (GMP/ISO), Stoe & Cie, Germany
  • Diamand 3.2, Crystal Impact, Germany
  • The raw data can be supplied in all major X-ray file formats independent of the instrument used. In addition data can be supplied as Excel graph linked to a sheet containing all x-y data points

 

Additional Services / Features:

  • Method development and validation under GMP
  • Examination of patent infringements
  • The XRPD lab is embedded in the solid-state development department, a department with experts on polymorphism, co-crystals, salts and crystallization development

Bragg Equation

Bragg Equation

Bragg Equation

Stoe STADI P

Stoe STADI P

Stoe STADI P