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We are a contract laboratory offering XRD analysis according to GMP
XRD is highly useful for identification of crystalline structures
X-Ray diffraction is primarily used for
- ID of crystalline material (used for regulatory purposes or during development)
- ID of different polymorphic forms
- Distinguishing between amorphous and crystalline material
- Quantification of the percent crystallinity of a sample
- For non-ambient structural analysis
- For stability studies
Diffractogram of chemical grade NaCl, with peak positions inserted, for 10 selected peaks. ID of a material is routinely determined by comparison of peak positions from XRD analysis with peak positions from reference material.
Types of Analysis we offer:
ID analysis: We conduct routine XRD analysis for identification purposes, according to Ph. Eur. 2.9.33., using a standard scan program over the interval: 2°-60° 2Θ. All 2Θ ranges between 2° – 153° are available upon request.
Quantitative analysis: Quantification of crystalline or amorphous content in a sample is determined by use of a calibration line, relating peaks intensities to crystalline sample content.
Why use XRD analysis?
Knowledge about crystallinity is highly relevant, as a crystalline form is usually preferred in development: In contrast to amorphous material, a crystal has well-defined properties (melting point, solubility and IDR) – parameters that should be known in order to control your final product.
The XRD method is described in Ph. Eur 2.9.33. The result from an XRD analysis is a diffractogram showing the intensity as a function of the diffraction angles. Positive ID of a material using XRD analysis is based on accordance between the diffraction angles of a reference material and the sample in question.
The principle behind XRD analysis
XRD analysis is based on constructive interference of monochromatic X-rays and a crystalline sample: The X-rays are generated by a cathode ray tube, filtered to produce monochromatic radiation, collimated to concentrate, and directed toward the sample. The interaction of the incident rays with the sample produces constructive interference (and a diffracted ray) when conditions satisfy Bragg’s Law (nλ=2d sin θ). This law relates the wavelength of electromagnetic radiation to the diffraction angle and the lattice spacing in a crystalline sample.
The characteristic x-ray diffraction pattern generated in a typical XRD analysis provides a unique “fingerprint” of the crystals present in the sample. When properly interpreted, by comparison with standard reference patterns and measurements, this fingerprint allows identification of the crystalline form.
Technical info
Instrument
Malvern Panalytical X’Pert3 Powder
Malvern Panalytical Empyrean Multipurpose Diffractometer
Operating range
2 – 60° 2-Theta (standard)
2 – 150° 2-Theta (if required)
Humidity
Ambient (standard)
5%RH – 95%RH (climate chamber)
Temperature
Room temperature (standard)
10 °C – 400 °C (climate chamber)
Sample amount
10 mg – 1000 mg
Looking for a X-Ray Diffraction analysis for your medical product?
X-ray diffraction (XRD analysis or XRPD analysis) is a unique method in determination of crystallinity of a compound.
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