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A series of calibration measurements have been performed on Suanni – the first small-angle neutron scattering spectrometer entering into routine user operation in China – aiming to characterize instrument performance and to provide a reference for user experiments. Various calibration standards were used to verify the precise association of the scattering intensity I with the scattering vector magnitude q at short and medium sample–detector distances. The measurements recorded for silver behenate powder revealed a slight shift of the neutron wavelength (λ) at the sample position as compared to the nominal λ calculated by the selector constant. The deviation was more significant with λ > 0.8 nm owing to the shape of the incoming neutron spectrum incident on the selector. The measured dead time for the entire detection system is 2.7 µs, as determined by measurements with varying fluxes. A protonated/deuterated polystyrene blend was employed as the primary standard to calibrate the secondary standard H2O. The instrument covers an effective q range between 0.013 and 5 nm−1, as demonstrated by scattering curves obtained from a monodisperse poly(methyl methacrylate) nanoparticle suspension and a glassy carbon plate.

In order to make the most of the low photon flux in laboratory small-angle X-ray scattering instruments, the experimental geometry has to be chosen carefully, with special stress on the beam-shaping system. The optimum collimation scheme should enable accurate measurements over the desired range of the scattering variable, while yielding the highest flux and the lowest possible instrumental background. In order to identify the best setting, a phase-space optimization of the collimating scheme is carried out in the present work, including constraints on the beam size at the sample position and on the detector surface. The resulting formulae are implemented in a Python script with a graphical user interface, to aid the planning, construction and daily operation of pinhole small-angle scattering cameras.

The details of a newly constructed small-angle X-ray scattering instrument are presented. The geometry of the instrument is highly customizable, enabling it to address vastly different experimental situations from academic research to industrial problems. The high degree of motorization and automation compared to conventional laboratory-scale SAXS instruments facilitates the alignment and daily use. Data reduction routines are incorporated in the instrument control software, yielding fully corrected and calibrated results promptly after the end of measurements. Optimization of the fluxversus resolution balance can be done routinely for each measurement task. A wide, continuous range ofq= 4πsinθ/λ can be reached, from below 0.02 nm−1up to 30 nm−1, corresponding to periodic distances ofca 350 nm down to 0.2 nm. A few representative results obtained from samples of different research fields demonstrate the versatility of the instrument. Scattering curves are routinely calibrated into absolute units using a glassy carbon secondary standard. More information and recent developments can be found on the web page of the instrument at http://credo.ttk.mta.hu.

Time-resolved synchrotron small-angle X-ray scattering (SAXS) was used to study the structural changes during the osmotic shrinkage of a pharmacologically relevant liposomal drug delivery system. Sterically stabilized liposomes (SSLs) with a diameter of 100 nm and composed of hydrogenated soy phosphocholine, cholesterol and distearoyl-phosphoethanolamine-PEG 2000 prepared in a salt-free buffer were mixed with a buffered 0.3 MNaCl solution using a stopped flow apparatus. The changes in the liposome size and the bilayer structure were followed by using SAXS with a time resolution of 20 ms. A linear decrease in liposome size is observed during the first ∼4 s of the osmotic shrinkage, which reveals a water permeability value of 0.215 (15) µm s−1. The change in the size of the liposomes upon the osmotic shrinkage is also confirmed by dynamic light scattering. After this initial step, broad correlation peaks appear on the SAXS curves in theqrange of the bilayer form factor, which indicates the formation of bi- or oligolamellar structures. Freeze-fracture combined with transmission electron microscopy revealed that lens-shaped liposomes are formed during the shrinkage, which account for the appearance of the quasi-Bragg peaks superimposed on the bilayer form factor. On the basis of these observations, it is proposed that the osmotic shrinkage of SSLs is a two-step process: in the initial step, the liposome shrinks in size, while the area/lipid adapts to the decreased surface area, which is then followed by the deformation of the spherical liposomes into lens-shaped vesicles.