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The characterization of nanoporous powders of highly absorbing compounds by small-angle X-ray scattering (SAXS) involves overcoming several difficulties before quantitative information related to the porous texture, such as the specific surface and the porous volume, can be derived. In this article, first, the contribution of the grain facet reflectivity and scattering from the bulk of a grain with the density of ThO2, a highly absorbing material, were calculated. Microporous ThO2 powder having micrometric grain size was characterized, in which the scattering signal is predominant. A high-resolution synchrotron instrument was used in order to cover a wider q range and minimize the absorption effect, and the results were compared with those obtained using a laboratory X-ray source. Concerning the absorption problem existing with a laboratory X-ray source, a new and robust experimental method was proposed to correctly determine the scattering intensity of the highly absorbing granular samples on an absolute scale. This method allows one to calculate accurately the porous volume and the specific surface via Porod's law and the invariant using a laboratory SAXS instrument. This last result opens new perspectives for the characterization of the volume and the specific surface of highly absorbing actinide oxide powders.

Ternary mixtures of medium-chain fatty alcohols, water and a hydrotrope (such as ethanol), near the immiscibility gap, make stable single phases at constant temperature. Interestingly, in this `pre-ouzo region' these single phases consist of two distinct nanoscopic pseudo-phases, one octanol-rich and one water-rich. This domain of composition, which is known to produce strong light scattering and to separate under ultracentrifugation into two phases, has been studied using contrast variation in small-angle neutron scattering (SANS) combined with small- and wide-angle X-ray scattering (SWAXS). The existence of fatty alcohol-rich domains of well defined size of the order of 2 nm radius is proven. The scattering can be approximated by an Ornstein–Zernike function, which is close to the general expression of Choi, Chen, Sottmann & Strey [Physica B, (1998),241–243, 976–978] with vanishing quadratic Porod term. Exploitation of the relative intensities at the vanishing scattering angle in SANS demonstrates that the distribution coefficient of ethanol between the octanol-rich and the water-rich domains is close to one. WAXS of the two coexisting pseudo-phases is compared with the corresponding binary water–ethanol and octanol–ethanol samples.

An experimental method to determine simultaneously the compaction and the total specific area between an inorganic oxide network and a material of low electronic density (organic surfactant or air) is presented. This method is applicable when both the Porod limit and the invariant can be extracted from the small-angle X-ray scattering pattern on an absolute scale. An example is given using a hybrid precipitate of zirconium oxide and a cationic surfactant (CTAB). In such a mesostructured material, the total measured interface and the geometrically modelled one differ by a factor of 4, while compaction is about 0.4, well below 1. This is attributed to the presence of microporosity, in addition to the mesoporosity. The validity of the method is demonstrated using goethite as a reference inorganic material of known compaction equal to 1.

A significant improvement in the sensitivity of a Huxley-Holmes design for a small angle X-ray scattering camera is obtained by separating the mirror and the monochromator. The "separated optics" camera described in this paper involves a long X-ray mirror close to a point X-ray source associated with a curved focusing crystal located close to the sample. The sample area is located at half the distance between the source and detector planes. Diffuse scattering produced by the mirror is not incident on the focusing crystal, thus reducing the background signal. Complete elimination of hard X-rays allows precise calibration and hence absolute determination of sample cross-section by means of a semi-transparent beam-stop. In pinhole geometry, the flux corresponds to a ca. 107 photons/s through the sample, collimated to q=10-2 Å-1 in scattering vector range. This allows determination of scattered intensities of the order of 10-3 cm-1, corresponding to the scattering related to isothermal compressibility of less than 0.1 mm of pure water. Values of absolute intensities for water as well as convenient widespread buffer solutions are shown, in order to be usable for calibration as secondary standards. As solid reference sample, the widely studied Lupolentm – a semi-crystalline polymer- is calibrated. The high-q limit (q ≃ 4.5 nm–1 ) of a porous calcite sample can be used as a secondary standard for specific area determination of solid/solid or solid-liquid dispersions.