In situ spin coater for multimodal grazing incidence x-ray scattering studies.

We present herein a custom-made, in situ, multimodal spin coater system with an integrated heating stage that can be programmed with spinning and heating recipes and that is coupled with synchrotron-based, grazing-incidence wide- and small-angle x-ray scattering. The spin coating system features an adaptable experimental chamber, with the ability to house multiple ancillary probes such as photoluminescence and visible optical cameras, to allow for true multimodal characterization and correlated data analysis. This system enables monitoring of structural evolutions such as perovskite crystallization and polymer self-assembly across a broad length scale (2 Å-150 nm) with millisecond temporal resolution throughout a complete thin film fabrication process. The use of this spin coating system allows scientists to gain a deeper understanding of temporal processes of a material system, to develop ideal conditions for thin film manufacturing.

Implementation and application of the peak scaling method for temperature measurement in the laser heated diamond anvil cell.

A new design for a double-sided high-pressure diamond anvil cell laser heating set-up is described. The prototype is deployed at beamline 12.2.2 of the Advanced Light Source at Lawrence Berkeley National Lab. Our compact design features shortened mechanical lever arms, which results in more stable imaging optics, and thus more user friendly and more reliable temperature measurements based on pyrometry. A modification of the peak scaling method was implemented for pyrometry, including an iterative method to determine the absolute peak temperature, thus allowing for quasi-real time temperature mapping of the actual hotspot within a laser-heated diamond anvil cell without any assumptions on shape, size, and symmetry of the hotspot and without any assumptions to the relationship between fitted temperature and peak temperature. This is important since we show that the relationship between peak temperature and temperature obtained by fitting the Planck function against the thermal emission spectrum averaged over the entire hotspot is not constant but depends on variable fitting parameters (in particular, the size and position of the fitting window). The accuracy of the method is confirmed through measuring melting points of metal wires at ambient pressure. Having absolute temperature maps in real time allows for more differentiated analyses of laser heating experiments. We present such an example of the pressure variations within a heated hotspot of AgI at a loaded base pressure of 3.8 GPa.

High-throughput on-the-fly scanning ultraviolet-visible dual-sphere spectrometer.

We have developed an on-the-fly scanning spectrometer operating in the UV-visible and near-infrared that can simultaneously perform transmission and total reflectance measurements at the rate better than 1 sample per second. High throughput optical characterization is important for screening functional materials for a variety of new applications. We demonstrate the utility of the instrument for screening new light absorber materials by measuring the spectral absorbance, which is subsequently used for deriving band gap information through Tauc plot analysis.

A multichannel gel electrophoresis and continuous fraction collection apparatus for high-throughput protein separation and characterization.

To facilitate a direct interface between protein separation by PAGE and protein identification by mass spectrometry, we developed a multichannel system that continuously collects fractions as protein bands migrate off the bottom of gel electrophoresis columns. The device was constructed using several short linear gel columns, each of a different percent acrylamide, to achieve a separation power similar to that of a long gradient gel. A "Counter Free-Flow" elution technique then allows continuous and simultaneous fraction collection from multiple channels at low cost. We demonstrate that rapid, high-resolution separation of a complex protein mixture can be achieved on this system using SDS-PAGE. In a 2.5 h electrophoresis run, for example, each sample was separated and eluted into 48-96 fractions over a mass range of approximately 10-150 kDa; sample recovery rates were 50% or higher; each channel was loaded with up to 0.3 mg of protein in 0.4 mL; and a purified band was eluted in two to three fractions (200 microL/fraction). Similar results were obtained when running native gel electrophoresis, but protein aggregation limited the loading capacity to about 50 microg per channel and reduced resolution.

High-efficiency microarray printer using fused-silica capillary tube printing pins.

We describe a contact printing approach for microarrays that uses fused-silica capillary tubes with tapered tips for printing pins and a pressure/vacuum system to control pin loading, printing, and cleaning. The printing process is insensitive to variable environmental factors such as humidity, and the small diameter of the pins allows routine printing from 1536 well source plates. Pin load capacity, 0.2 microL in the current system, is adjustable by controlling pin length. More than 2000 spots can be printed per 0.2-microL pin load (<100 pl/spot), and densities of >12,000 spots/cm(2) are readily achievable. Solutions with a wide range of viscosities and chemical properties can be printed. The system can print tens of thousands of different solutions at high speed, due to the ability to use large numbers of pins simultaneously, and can produce a large number of replicate arrays since all of the solution picked up by the pins is available for deposition.

Automated sample mounting and alignment system for biological crystallography at a synchrotron source.

High-throughput data collection for macromolecular crystallography requires an automated sample mounting and alignment system for cryo-protected crystals that functions reliably when integrated into protein-crystallography beamlines at synchrotrons. Rapid mounting and dismounting of the samples increases the efficiency of the crystal screening and data collection processes, where many crystals can be tested for the quality of diffraction. The sample-mounting subsystem has random access to 112 samples, stored under liquid nitrogen. Results of extensive tests regarding the performance and reliability of the system are presented. To further increase throughput, we have also developed a sample transport/storage system based on "puck-shaped" cassettes, which can hold sixteen samples each. Seven cassettes fit into a standard dry shipping Dewar. The capabilities of a robotic crystal mounting and alignment system with instrumentation control software and a relational database allows for automated screening and data collection to be developed.