Collecting data in the home laboratory: evolution of X-ray sources, detectors and working practices

Abstract

While the majority of macromolecular X-ray data are currently collected using highly efficient beamlines at an ever-increasing number of synchrotrons, there is still a need for high-performance reliable systems for in-house experiments. In addition to crystal screening and optimization of data-collection parameters before a synchrotron trip, the home system allows the collection of data as soon as the crystals are produced to obtain the solution of novel structures, especially by the molecular-replacement method, and is invaluable in achieving the quick turnover that is often required for ligand-binding studies in the pharmaceutical industry. There has been a continuous evolution of X-ray sources, detectors and software developed for in-house use in recent years and a diverse range of tools for structural biology laboratories are available. An overview of the main directions of these developments and examples of specific solutions available to the macromolecular crystallography community are presented in this paper, showing that data collection 'at home' is still an attractive proposition complementing the use of synchrotron beamlines.

X-ray scattering characterisation of nanoparticles

“…Due to their high electron density contrast, ρ (see Equation (4)), dilute suspensions can be measured, such as the early stages of particle nucleation. Downloaded by [New York University] at 06:05 08 June 2015 46 …”

“…The current state-ofthe-art laboratory X-ray sources use a molten liquid jet as the anode and can achieve brilliance values of up to 2.6 × 10 10 photons s −1 mm −2 mrad −2 . [46] This is approaching the brilliance of a second-generation synchrotron source. Third-generation synchrotron sources typically have brilliances of around 10 16 -10 20 photons s −1 mm −2 mrad −2 .…”

“…Standard sealed tube sources with a fixed anode have typical brilliance values of around 10 8 photons s −1 mm −2 mrad −2 , while rotating anode and microfocus anodes can be an order of magnitude higher. [46] The maximum brilliance obtainable from these anodes is limited by the need to dissipate heat from the anode. The current state-ofthe-art laboratory X-ray sources use a molten liquid jet as the anode and can achieve brilliance values of up to 2.6 × 10 10 photons s −1 mm −2 mrad −2 .…”

A compact light source providing high-flux, quasi-monochromatic, tunable X-rays in the laboratory

“…Alternatively, in micro/nanofocus transmission sources, the target is a thin metal film on a low-absorbing substrate, and the X-rays are extracted from the opposite side of the target. The limited spread of the electron beam in the thin target allows for spot sizes below 1 μm (albeit at very low power), and the geometry allows for very short working distances, useful for applications like micro-CT. To further overcome the limits of heat load on a stationary target, rotating anode sources 2 have been developed, where the heat load is spread over a larger surface, allowing for much higher power. More recent, advanced developments include liquid metal jet sources 3,4 and structured anode sources, 5 but all these developments are reaching the physics limit of what can be achieved with electron-impact sources.…”

Laboratory X-ray Diffraction Complex for In Situ Investigations of Structural Phase Evolution of Materials under Gaseous Atmosphere

“…X-ray detectors play an important role in diffraction measurements [22]. The first electronic detectors appeared in the early 1990s: multiwire proportional counters (Siemens/Bruker X-1000), television-camera detectors (FAST developed by Uli Arndt) and electronically controlled imaging plates (MAR Research and Rigaku) [23]. However, the data collection rate of such X-ray detectors was not high, which prevented their application for in situ measurements.…”