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Small-angle X-ray and small-angle neutron scattering measurements were carried out on a series of porous silica precursor (unsintered) bodies with different starting chemistries. The samples were prepared from mixtures containing 10 to 30 wt% colloidal silica sol and 90 to 70 wt% potassium silicate. Particle-size distributions were derived from the data using a maximum-entropy technique. Scattering data from the porous silica samples are especially suitable for such an analysis because the colloidal particles and clusters and aggregates of these particles are verified in detail to be spherical, and the scattering instrument use for this study covered the entire range of sizes in this material and was very well calibrated. It was found that the lower the amount of colloidal silica, the broader the size distribution of the silica aggregates.
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The design and operation of a new small-angle X-ray scattering instrument, optimized for high throughput at a synchrotron source, high angular and wavelength resolution, large sample cross-sectional area, accurate energy tuning, excellent signal-to-noise ratio and harmonic rejection are presented. The principles of design and implementation are given, as are the details of primary calibration of absolute intensity and experimental desmearing. The instrument has been tested for application to anomalous-scattering measurements near the chromium K edge. Preliminary results on samples of a heat-treated steel are presented as a demonstration of the capability of this experiment to separate the microstructure evolution as a function of temperature of a chromium-rich precipitate from the thermal behavior of other precipitates in the steel.