Open Access

Electron paramagnetic resonance (EPR) of Fe3+ ions in Al2O3 is studied in powder samples prepared by different routes and/or modified by thermal or mechanical treatments, with different doping levels and grain sizes. The measurements are performed in various frequency bands (S, X, K, Q and W) and with bimodal detection in X-band. Simulations of the spectra are achieved with a code designed for computing EPR powder spectra described by any spin Hamiltonian including second-, fourth-and sixth-order ZFS terms (S ? 7/2). The linewidths, intensities and lineshapes are accounted for. The lineshape is Gaussian at low Fe3+ concentration whereas it is Lorentzian for higher concentration. The linewidths are interpreted as the superimposition of three main contributions: intrinsic linewidth, dipolar broadening and broadening due to lattice imperfections. The latter is tentatively interpreted in terms of quadrupolar spin Hamiltonian parameter distributions treated using first-order perturbation theory. Whatever the sample, only the b22 spin Hamiltonian parameter is found to be distributed around a mean zero value which corresponds to rhombic distortions. Angle and bond length distributions are tentatively extracted from the b22 distributions which gives some insight into the local order around the spin probe in relation to the preparation and treatment of the samples.

Critical soil zones where large areas along a shear joint might begin to slip should be recognized. In order to avoid damage, monitoring of such unstable zones is necessary. First, soil movements must be detected as early as possible, second, the amount of deformation should be estimated. Because geodetical methods do not provide information about deformation in the underground in different depths, the only way to come to information from possible shear zones is the installation of deformation measurement systems. A special installation method was developed to bring a long-gauge length measurement system into a borehole and transfer data of soil deformations into an installed sensing rod. The mostly vertically installed sensing rod has an outer diameter of 3 mm to 6 mm and contains several optical fibres. One fibre provides integral strain information along the whole length of the rod. To get this information, the phase difference between the fibre input and output is measured and the change of the total length of the fibre can be derived. This easy and cheap online sensing system delivers an early warning of soil deformations respectively possible slip as well as landslides. In case of warning, the second sensing system based on Fibre Bragg Grating sensors located close to the expected shear zone purposefully. It records resulting deformations in detail. In this study, three main objectives were achieved: a) development of tiny pultruded sensing rods with integrated optical sensor fibres, b) installation technology which enables the integration of the sensing rod during drilling and pile driving, and c) development of a stiff but elastic racking material to fix the rod in the soil and to transfer soil deformation into the stiffer sensing rod. These three aspects including the fibre optical measurement systems are described; results from Press Deformation Test (PDT) are presented. Test results of the fibre optical online system are compared and evaluated with the results of conventional inclinometer measurements as well as numerical modelling. An outlook for further possibilities of usage of this monitoring system is given.

A series of crystalline aluminum hydroxy fluorides in cubic pyrochlore structure AlFx(OH)3-x·H2O with variable F-content x were investigated by solid-state NMR by applying different magnetic fields up to 21.1 T. Distinguishable octahedral species AlFx(OH)6-x (x = 1-6) were identified in the crystalline aluminum hydroxy fluorides. The subsequent analysis of the highfield 27Al MAS NMR data allows the derivation of the trend analysis graphs giving correlations between the 27Al chemical shifts and the quadrupolar frequencies and the F-content x in AlFx(OH)6-x. Clear trends were obtained for both, which are, along with the 19F MAS chemical-shift trend analysis presented earlier, valuable tools for the interpretation of MAS NMR spectra of amorphous AlFx(OX)3-x compounds (X = H, alkyl). Following the dehydration of the pyrochlores by solid-state NMR eventually reveals a remarkable influence of the incorporated solvent molecules (H2O) on the 19F chemical shift. On that basis, a new chemical-shift trend analysis for 19F chemical shifts in correlation with x in AlFx(OH)6-x units for proton-poor substances (in the Al, F, O, H system) was determined. By using this correlation, high-surface AlF3 has a mean bulk Al:F ratio similar to that found for ACF, namely, AlF2.8(O/OH)0.2.