A core of concrete taken from a major road bridge in the Strathclyde Region, Scotland, has been subjected to an applied mineralogical investigation, which involved stable isotope analysis, petrography, X-ray diffraction and scanning electron microscopy.

The structure is actively undergoing severe degradation due to mineral growth which is related to chemical reactions between the concrete and pore fluid. The physical growth of minerals causes disfigurement and structural weakening.

Pyrite and pyrrhotine hosted by dolerite aggregate appear to have been oxidized, providing sulphate for the deposition of ettringite and minor gypsum, in spheroidal cavities within the cement paste. The rainwater which passes through the structure mobilising sulphate from original gypsum in the paste and oxidizing the iron sulphides is also involved in the further leaching of elements from the cement paste and in the deposition of calcite. The isotopic values of calcites forming a crust on the concrete and a stalactite under the bridge are similar with δ13C= −19‰ PDB and δ18‰= +16‰ SMOW. We suggest that atmospheric carbon dioxide was the carbon source. The carbon isotopic fractionation of −12‰ from atmospheric carbon dioxide of δ13C= −7‰, (O'Neil and Barnes, 1971) can best be explained as due to a kinetic fractionation related to the hyper-basicity of the pore water. The equilibrium formation temperature of about 45°C calculated from the oxygen isotope values and assuming a δ18O value of meteoric water of −8‰ SMOW, is considered unreasonable. The exceptionally low δ18O values are attributed mainly to reaction kinetics and the calcite inheriting its oxygen, two-thirds from atmospheric carbon dioxide and one third from the meteoric formation water (O'Neil and Barnes, 1971). A δ18O value of atmospheric carbon dioxide of +41‰ SMOW and a δ18O value of meteoric water of −8‰ SMOW, lead to a calculated δ18O value for the calcites of +10‰ SMOW. The calcites analysed have a value of +16‰ and this may be due to partial re-equilibration towards a calculated value of +21‰ for calcite in equilibrium with the meteoric water at 20°C.

A revised structure model of ettringite is presented, in order to provide quantitative X-ray diffraction (QXRD) of this mineral in cement pastes. The model is derived from two different existing structure models, both of which are suitable for restricted use but are inferior to the refined ettringite structure presented. In the first published ettringite structure proposed by Moore and Taylor [Acta Crystallogr. B 26, 386–393 (1970)], none of the 128 positions for H are given in the unit cell, which results in reduced scattering power for use of this model for quantification purposes. For the precise quantification of ettringite in samples together with anhydrous phases, the scattering factors of all atoms including the H positions are indispensable. The revised structure model is based on the data of Moore and Taylor, supplemented by the H positions determined by Berliner (Material Science of Concrete Special Volume, The Sydney Diamond Symposium, American Ceramic, Society, 1998, pp. 127–141) on the basis of a neutron diffraction structural investigation of deuterated ettringite at 20 K. Berliner’s (Material Science of Concrete Special Volume, The Sydney Diamond Symposium, American Ceramic Society, 1998, pp. 127–141) thermal parameter should not, however, be used, since a normal application is at room temperature. In order further to improve the structure model of ettringite, Rietveld refinement with the rigid body approach for OH and H2O molecules and SO4 tetrahedra was employed. The refined and improved ettringite structure model was tested for quantitative phase analysis by the determination of actual ettringite contents in mixtures with an internal standard. Synthesized and orientation-free prepared ettringite powders were investigated by X-ray powder diffraction analysis and quantified in four different blends with zircon. The quantification results with the new structure model demonstrate the superior quality of the revised ettringite structure.

The two-dimensional XRD (GADDS) was used to characterize the microstructure of an applied self-leveling compound (SLC). A calcium aluminate cement based SLC was prepared on two different substrates (water absorbent and nonwater absorbent) to determine the vertical distribution of the crystalline phases. The application of the GADDS enables the detection of the phase composition of the hydrating mortar in horizontal slices. Thus the analysis could be carried out in position-sensitive mode at three different areas: near the bottom, in the center, and at the top of the mortar. For investigation of SLCs from the very early hydration stage up to 10 h of hydration, a custom-made in situ sample holder for the measurements was designed and constructed. The combination of the GADDS and the custom-made in situ sample holder provides the possibility to characterize additionally the time-dependent phase composition within the SLC. The nonabsorbent substrate has no effect on the hydration of the binder phases but the absorbent substrate influences the formation of ettringite. In the top layer of the SLC the ettringite content is reduced during the first hours of hydration. The absorbing forces of the substrate lead to migration of the mix water to the substrate. This lack of water results in the reduced formation of ettringite.