S U M M A R YWith various low-temperature experiments performed on magnetic mineral extracts of marine sedimentary deposits from the Argentine continental slope near the Rio de la Plata estuary, a so far unreported style of partial magnetic self-reversal has been detected. In these sediments the sulphate-methane transition (SMT) zone is situated at depths between 4 and 8 m, where reductive diagenesis severely alters the magnetic mineral assemblage. Throughout the sediment column magnetite and ilmenite are present together with titanomagnetite and titanohematite of varying compositions. In the SMT zone (titano−)magnetite only occurs as inclusions in a siliceous matrix and as intergrowths with lamellar ilmenite and titanium-rich titanohematite, originating from high temperature deuteric oxidation within the volcanic host rocks. These abundant structures were visualized by scanning electron microscopy and analysed by energy dispersive spectroscopy. Warming of field-cooled and zero-field-cooled low-temperature saturation remanence displays magnetic phase transitions of titanium-rich titanohematite below 50 K and the Verwey transition of magnetite. A prominent irreversible decline characterizes zero-field cooling of room temperature saturation remanence. It typically sets out at ∼210 K and is most clearly developed in the lower part of the SMT zone, where low-temperature hysteresis measurements identified ∼210 K as the blocking temperature range of a titanohematite phase with a Curie temperature of around 240 K. The mechanism responsible for the marked loss of remanence is, therefore, sought in partial magnetic self-reversal by magnetostatic interaction of (titano-)magnetite and titanohematite. When titanohematite becomes ferrimagnetic upon cooling, its spontaneous magnetic moments order antiparallel to the (titano-)magnetite remanence causing an drastic initial decrease of global magnetization. The loss of remanence during subsequent further cooling appears to result from two combined effects (1) magnetic interaction between the two phases by which the (titano-)magnetite domain structure is substantially modified and (2) low-temperature demagnetization of (titano-)magnetite due to decreasing magnetocrystalline anisotropy. The depletion of titanomagnetite and superior preservation of titanohematite is characteristic for strongly reducing sedimentary environments. Typical residuals of magnetic mineral assemblages derived from basaltic volcanics will be intergrowths of titanohematite lamellae with titanomagnetite relics. Low-temperature remanence cycling is, therefore, proposed as a diagnostic method to magnetically characterize such alteration (palaeo-)environments.
S U M M A R YIn paleomagnetic and environmental magnetic studies the magnetomineralogical identification is usually based on a set of rock magnetic parameters, complemented by crystallographic and chemical information retrieved from X-ray diffraction (XRD), (electron) microscopy or energy dispersive spectroscopy (EDS) of selected samples. While very useful, each of these supplementary techniques has its limitations when applied to natural sample material which are related to low particle concentrations (down to the ppm range in marine sediments) and very fine grain sizes (down to the nm scale). Therefore, meaningful application of such techniques depends on sample quality. Electron backscatter diffraction (EBSD) of individual grains in scanning electron microscopy (SEM) enables mineralogical identification of grains down to ∼0.2 micrometer and is particularly powerful when combined with EDS. In this study, we show the merits of EBSD for rock magnetic investigations by analyzing titanomagnetites and hemoilmenites of various compositions and submicron lamella of titanomagnetite-hemoilmenite intergrowths. Such particles often occur in natural marine sediments where EDS often has a semi-quantitative character and compositionally similar intergrowths may be difficult to distinguish. With the mineralogical information provided by EBSD unambiguous identification of spinel-type and trigonal oxides is obtained. Optimal EBSD patterns are gathered from smooth, polished surfaces, but here we show that interpretable EBSD patterns can be obtained directly from the surface of unconsolidated, so called 'non-embedded' particles from marine sediments. This information enhances the interpretative value of rock magnetic parameters.
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