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The detection of auto-fluorescence in phytogenic, hydrated amorphous silica depositions (phytoliths) has been found to be a promising approach to verify if phytoliths were burnt or not, especially in archaeological contexts. However, it is unknown so far at what temperature and how auto-fluorescence is induced in phytoliths. We used fluorescence microscopy, scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDX), and Fourier transform infrared spectroscopy to analyze auto-fluorescence in modern phytoliths extracted from plant samples or in intact leaves of winter wheat. Leaves and extracted phytoliths were heated at different temperatures up to 600 degrees C. The aims of our experiments were i) to find out what temperature is needed to induce auto-fluorescence in phytoliths, ii) to detect temperature-dependent changes in the molecular structure of phytoliths related to auto-fluorescence, and iii) to derive a mechanistic understanding of auto-fluorescence in phytoliths. We found organic compounds associated with phytoliths to cause auto-fluorescence in phytoliths treated at temperatures below approx. 400 degrees C. In phytoliths treated at higher temperatures, i.e., 450 and 600 degrees C, phytolith auto-fluorescence was mainly caused by molecular changes of phytolith silica. Based on our results we propose that auto-fluorescence in phytoliths is caused by clusterization-triggered emissions, which are caused by overlapping electron clouds forming non-conventional chromophores. In phytoliths heated at temperatures above about 400 degrees C dihydroxylation and the formation of siloxanes result in oxygen clusters that serve as non-conventional chromophores in fluorescence events. Furthermore, SEM-EDX analyses revealed that extractable phytoliths were dominated by lumen phytoliths (62%) compared to cell wall phytoliths (38%). Our findings might be not only relevant in archaeological phytolith-based examinations, but also for studies on the temperature-dependent release of silicon from phytoliths and the potential of long-term carbon sequestration in phytoliths.
Soil landscape research is faced with wide-ranging questions of soil erosion, precision farming, and agricultural risk management. Digital Soil Morphometrics is a powerful tool to provide respective answers or recommendations but requires soil data from the pedon-to-field scale with high horizontal and vertical resolutions, including the subsoil. We present an efficient sampling and measurement method for easily obtainable soil driving cores with low-destructive preparation. Elemental contents and soil organic and mineral matter composition were measured rapidly and in large numbers using a multi-sensor approach, i.e., visible and near infrared (Vis-NIR), diffuse reflectance infrared Fourier transform (DRIFT), and X-ray fluorescence (XRF) spectroscopy. The suitability of the approach with respect to three-dimensional soil landscape models was tested using soils along a slope representing different stages of erosion and deposition in a hummocky landscape under arable land use (Calcaric Regosols, Calcic Luvisols, Luvic Stagnosols, Gleyic-Colluvic Regosols). The combination of soil core sampling, pedological description, and three spectroscopic techniques enabled rapid determination and interpretation of horizontal and vertical spatial distributions of soil organic carbon (SOC), soil organic and mineral matter composition, as well as CaCO3, Fe, and Mn contents. Depth profiles for SOC, CaCO3, and Fe contents were suitable indicators for site-specific degrees of erosion and matter transport processes at the pedon-to-field scale. Fe and Mn profiles helped identifying zones of reductive and oxic domains in subsoils (gleyzation). Further methodical developments should implement plant-availability of nutrients, characterization of Fe oxides, and calibration of the spectroscopic techniques to field-moist samples.