Tag: convergent beam

Analysis of powder crystal structures of organic crystals using a high-resolution convergent beam optical system

Previously, it was typical to conduct crystal structure analysis using the single crystal method. However, analysis of crystal structure using the single crystal method is difficult in the case of samples for which it is hard to produce single crystals, and samples for which crystal growth is difficult even if single crystals can be produced. In recent years, the precision of powder X-ray diffractometers has been improving, and thus it is becoming possible to conduct crystal structure analysis using powder samples. Here we show an example where a powder sample was measured, and structural analysis was conducted based on the obtained diffraction pattern.

Identification of the crystal form of the active pharmaceutical ingredient in a tablet

Many active pharmaceutical ingredients have multiple crystal forms, and it is known that solubility and bioavailability vary depending on the crystal form. In the drug manufacturing process, active ingredients may sometimes undergo a crystalline phase transition to another crystal form, due to factors such as heat, light, humidity or pressure, and there is a need to check what crystal form the ingredient is in, in its final product state. With optical systems employing the Bragg-Brentano focusing method, of the type generally used with powder X-ray diffractometry, measurement of the powdered sample is done with a reflection arrangement, but if a tablet is crushed into a powdered state, there are worries that transitions will occur due to the crushing, and it will be impossible to evaluate the original crystal form. In addition, if measurement is done with a reflection arrangement without crushing the tablet, it may be impossible to obtain internal information. Therefore, we analyzed a tablet non-destructively by using a convergent optical system enabling non-destructive/transmission measurement of tablets.