The increasing importance of X-ray diffractometry with 2-d detectors has lead to a rising demand for highly intense X-ray sources enabling the analysis of very small and weakly scattering samples in the home laboratory within a reasonable time frame. Therefore, various microfocusing sealed tube X-ray sources with focal spot sizes below 100 μm are now available.

Figure 1: IμS™ for 2-d diffraction, combined with 2D VANTEC-2000 detector

For powder diffractometry IμS™ can be used either in a reflection or transmission set-up as shown in fig. 1, the IμS™ in combination with a Bruker GADDS-system with a VANTEC-2000 detector. In the transmission set-up, a focusing Quazar™ optics was used, which focused the beam into the detector. A measurement of LaB₆ showed an achievable resolution of 0.08°2θ. Measurements of a pharmaceutical powder sample (Ibuprofen) recorded with a typical parallel beam sealed tube set-up and with IμS™ with comparable 0.3 mm collimators showed that the IμS™ delivered 10 times more intensity in an 8 times shorter exposure time. Also, the spottiness of the pattern is much less for the measurement with the IμS™ because the focused beam led to a better crystallite statistics and a larger diffracting sample volume.

We have collected data of outstanding quality in applications such as protein and small molecule crystallography, phase identification, μ-diffraction, screening and small-angle scattering. The presented results demonstrate that we achieve much better data quality in XRD applications with an IμS™ coupled with a 2-d detector in comparison to the common sealed tube systems.

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1. Investigating phase transitions under non ambient conditions using the Incoatec Microfocus Source IμS™
2. The Incoatec Microfocus Source IμS™ for home-lab diffractometry