Quantitative selection of sample structures in small-angle scattering using Bayesian methods.

Small-angle scattering (SAS) is a key experimental technique for analyzing nanoscale structures in various materials. In SAS data analysis, selecting an appropriate mathematical model for the scattering intensity is critical, as it generates a hypothesis of the structure of the experimental sample. Traditional model selection methods either rely on qualitative approaches or are prone to overfitting. This paper introduces an analytical method that applies Bayesian model selection to SAS measurement data, enabling a quantitative evaluation of the validity of mathematical models. The performance of the method is assessed through numerical experiments using artificial data for multicomponent spherical materials, demonstrating that this proposed analysis approach yields highly accurate and interpretable results. The ability of the method to analyze a range of mixing ratios and particle size ratios for mixed components is also discussed, along with its precision in model evaluation by the degree of fitting. The proposed method effectively facilitates quantitative analysis of nanoscale sample structures in SAS, which has traditionally been challenging, and is expected to contribute significantly to advancements in a wide range of fields.

Size of elementary clusters and process period in silver nanoparticle formation.

The time dependence of small-angle X-ray scattering (SAXS) curves for silver nanoparticle formation was followed in situ at a time resolution of 0.18 ms, which is 3 orders of magnitude higher than that used in previous reports (ca. 100 ms). The starting materials were silver nitrate solutions that were reacted with reducing solutions containing trisodium citrate. The SAXS analyses showed that silver nanoparticles were formed in three distinct periods from a peak diameter of ca. 0.7 nm (corresponding to the size of a Ag(13) cluster) during the nucleation and the early growth period. The Ag(13) clusters are most likely elementary clusters that agglomerate to form silver nanoparticles.

Radiation damage to a protein solution, detected by synchrotron X-ray small-angle scattering: dose-related considerations and suppression by cryoprotectants.

In small-angle X-ray scattering experiments at high-brilliant synchrotron sources, protein aggregation results from radiation damage. The radiation-induced aggregation of lysozyme in solution was qualitatively evaluated based on forward scattering and radii of gyration. The scattering did not change below 400 Gy and increased exponentially above this dose. The aggregation is only seen beyond the critical dose rate, and the 'dilution effect' known in radiology was also observed. Mass spectroscopy of the lysozyme solution exposed to a monochromatic X-ray beam did not show any cleavage of the polypeptide chain. Small-angle X-ray scattering patterns suggested that the radiation-induced aggregation should be a non-specific association of intact lysozyme, without substantial alterations of the folding topologies. It was found that the addition of small amounts of cryoprotectants, such as glycerol, ethylene glycol and sucrose, effectively reduced the radiation damage. Glycerol and ethylene glycol were identically effective in the 100 mM concentration range. A similar effective concentration was observed for sucrose. The damage reduction by the cryoprotectants was mainly ascribed to changes in the protein-protein interactions, and rarely to decreases in the diffusion rates of activated species.