Lignosulfonate is a colloidal polyelectrolyte that is obtained as a side product in sulfite pulping. In this work we wanted to study the noncovalent association of the colloids in different solvents, as well as to find out how the charged sulfonate groups are organized on the colloid surface. We studied sodium and rubidium lignosulfonate in water-methanol mixtures and in dimethyl formamide. The number average molecular weights of the Na- and Rb-lignosulfonate fractions were 7600 g/mol and 9100 g/mol, respectively, and the polydispersity index for both was 2. Anomalous small-angle X-ray scattering (ASAXS) was used for determining the distribution of counterions around the Rb-lignosulfonate macromolecules. The scattering curves were fitted with a model constructed from ellipsoids of revolution of different sizes. Counterions were taken into account by deriving an approximative formula for the scattering intensity of the Poisson-Boltzmann diffuse double layer model. The interaction term between the spheroidal particles was estimated using the local monodisperse approximation and the improved Hayter-Penfold structure factor given by the rescaled mean spherical approximation. Effective charge of the polyelectrolyte and the local dielectric constant of the solvent close to the globular polyelectrolyte were followed as a function of the methanol content in the solvent and lignosulfonate concentration. The lignosulfonate macromolecules were found to aggregate noncovalently in water-methanol mixtures with increasing methanol or lignosulfonate content in a specific directional manner. The flat macromolecule aggregates had a nearly constant thickness of 1-1.4 nm, while their diameter grew when counterion association onto the polyelectrolyte increased. These results indicate that the charged groups in lignosulfonate are mostly at the flat surfaces of the colloid, allowing the associated lignosulfonate complexes to grow further at the edges of the complex.

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Here, we describe the analysis of the nanostructure and average chemical compositions of each phase present in an oxyfluoride glass ceramic, which is composed of fluoride nanocrystals and an oxide glass matrix. The overall composition of the oxyfluoride glass ceramic as prepared is 21.1%SiO 2 6.5%B 2 O 3 7.0%Al 2 O 3 21.0%PbF 2 14.3%CdF 2 11.0%YbF 3 0.5%ErF 3 11.0%PbO 7.6%CdO ͑mole %͒. Nanocrystals begin to grow at temperatures above the glass transformation temperature at 678 K as observed by x-ray diffraction. We report results from anomalous small-angle x-ray scattering taken at energies of x-ray absorption edges of Er, Yb, Pb, and Cd. By nonlinear regression of the scattering curves obtained from different edges simultaneously, the nanocrystals were found to be describable as polydisperse spheroids. The length of the smaller axis was found to be 6.4Ϯ 1.4 nm while the larger axis was found to be 17.7Ϯ 3.9 nm. By analyzing the scattering contrast as a function of the x-ray energy we found cadmium only in the glass matrix.

Many materials used for energy conversion have a complex structure and chemical composition, knowledge of which is important for both understanding the function of materials and energy conversion systems and for their further development. Synchrotron radiation and neutrons can make an important contribution to understanding the function of such systems. Taking examples from the fields of fuel cells, gas separation membranes, batteries, solar cells, and catalysts, the use of radiography, tomography, diffraction, scattering, and absorption edge spectroscopy is demonstrated. The strength of such methods is the in situ characterization of processes and compositions, and so the focus is on these aspects.