An automatic sample changer system for measurements of large numbers of liquid samples – the µDrop Sample Changer – is presented. It is based on a robotic arm equipped with a pipetting mechanism, which is combined with a novel drop-based sample holder. In this holder a drop of liquid is suspended between two parallel plates by surface tension. The absence of a transfer line benefits the cleaning, improving the background as well as making it faster and more efficient than most comparable capillary-based systems. The µDrop Sample Changer reaches cycle times below 35 s and can process up to 480 samples in a single run. Sample handling is very reliable, with a drop misplacement chance of about 0.2%. Very low sample volumes (<20 µl) are needed and repeatable measurements were performed down to 6 µl. Using measurements of bovine serum albumin and lysozyme, the performance of the instrument and quality of the gathered data of low and high concentrations of proteins are presented. The temperature of samples can also be controlled during storage and during measurement, which is demonstrated by observing a phase transition of a mesophase-forming lipid solution. The instrument has been developed for use in small-angle X-ray scattering experiments, which is a well established technique for measuring (macro-)molecules. It is commonly used in biological studies, where often large sets of rare samples have to be measured.
Microfluidic mixing is an important means for in-situ sample preparation and handling while Small Angle X-Ray Scattering (SAXS) is a proven tool for characterising (macro-)molecular structures. In combination those two techniques enable investigations of fast reactions with high time resolution (<1 ms). The goal of combining a micro mixer with SAXS, however, puts constraints on the materials and production methods used in the device fabrication. The measurement channel of the mixer needs good x-ray transparency and a low scattering background. While both depend on the material used, the requirement for low scattering especially limits the techniques suitable for producing the mixer, as the fabrication process can induce molecular orientations and stresses that can adversely influence the scattering signal. Not only is it important to find a production method that results in a device with low background scattering, but it also has to be versatile enough to produce appropriate mixer designs. Here we discuss two methods -laser ablation of polycarbonate and injection moulding of Topas -which were found suitable for our needs, provided care is taken in aligning the mixing/reaction channel, where the actual measurements will be carried out. We find injection moulding to be the better of the two methods.
Understanding and control of thermal transport in solids at the nanoscale are crucial in engineering and enhance the properties of a new generation of optoelectronic, thermoelectric and photonic devices. In this regard, semiconductor superlattice structures provide a unique platform to study phenomena associated with phonon propagations in solids such as heat conduction. Transient X-ray diffraction can directly probe atomic motions and therefore is among the rare techniques sensitive to phonon dynamics in condensed matter. Here, optically induced transient heat conduction in GaAs/AlAs superlattice structures is studied using the EIGER2 detector. Benchmark experiments have been performed at the Austrian SAXS beamline at Elettra–Sincrotrone Trieste operated in the hybrid filling mode. This work demonstrates that drifts of experimental conditions, such as synchrotron beam fluctuations, become less essential when utilizing the EIGER2 double-gating mode which results in a faster acquisition of high-quality data and facilitates data analysis and data interpretation.
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