Since a NanoSIMS high-resolution secondary ion mass spectrometry (SIMS) instrument was first used for cosmochemistry investigations over a decade ago, both interest in NanoSIMS and the number of instruments available have significantly increased. However, SIMS comes with a set of challenges that are of both technical and conceptual nature, particularly for complex samples such as soils. Here, we synthesize existing research and provide conceptual and technical guidance to those who wish to investigate soil processes at the submicron scale using SIMS, specifically with NanoSIMS. Our review not only offers advice resulting from our own operational experience but also intends to promote synergistic research on yet unresolved methodological issues. We identify and describe the basic setup of a NanoSIMS instrument, and important issues that may arise as a soil sample specimen are prepared for NanoSIMS analysis. This is complemented by discussions of experimental design, data analysis, and data representation. Next to experimental design, sample preparation is the most crucial prerequisite for successful NanoSIMS analyses. We discuss the requirements and limitations for sample preparation over the size range from individual soil particles to intact soil structures such as macroaggregates or intact soil cores. For robust interpretation of data obtained by NanoSIMS, parallel spatial, textural (scanning electron microscopy, atomic force microscopy), or compositional analyses (scanning transmission X-ray microscopy) are often necessary to provide necessary context. We suggest that NanoSIMS analysis is most valuable when applied in concert with other analytical procedures and can provide powerful inference about small-scale processes that can be traced via isotopic labeling or elemental mapping.

/pdf/advances-in-the-analysis-of-biogeochemical-interfaces-4sg0lnuiws.pdf

Advances in the Analysis of Biogeochemical Interfaces: NanoSIMS to Investigate Soil Microenvironments

The degree of aeolization of Quaternary deposits in Poland as a tool for stratigraphic interpretation

Abstract Since a NanoSIMS high-resolution secondary ion mass spectrometry (SIMS) instrument was first used for cosmochemistry investigations over a decade ago, both interest in NanoSIMS and the number of instruments available have significantly increased. However, SIMS comes with a set of challenges that are of both technical and conceptual nature, particularly for complex samples such as soils. Here, we synthesize existing research and provide conceptual and technical guidance to those who wish to investigate soil processes at the submicron scale using SIMS, specifically with NanoSIMS. Our review not only offers advice resulting from our own operational experience but also intends to promote synergistic research on yet unresolved methodological issues. We identify and describe the basic setup of a NanoSIMS instrument, and important issues that may arise as a soil sample specimen are prepared for NanoSIMS analysis. This is complemented by discussions of experimental design, data analysis, and data representation. Next to experimental design, sample preparation is the most crucial prerequisite for successful NanoSIMS analyses. We discuss the requirements and limitations for sample preparation over the size range from individual soil particles to intact soil structures such as macroaggregates or intact soil cores. For robust interpretation of data obtained by NanoSIMS, parallel spatial, textural (scanning electron microscopy, atomic force microscopy), or compositional analyses (scanning transmission X-ray microscopy) are often necessary to provide necessary context. We suggest that NanoSIMS analysis is most valuable when applied in concert with other analytical procedures and can provide powerful inference about small-scale processes that can be traced via isotopic labeling or elemental mapping.

Advances in the Analysis of Biogeochemical Interfaces: NanoSIMS to

The object of this study is to test the assumption that cryogenic weathering (here understood as in-situ disin- tegration of rock under cold-climate conditions including ice as a weathering agent) preferentially breaks up quartz grains. We apply the results of laboratory tests to a Quaternary sediment record. The combination of silt production, relative quartz enrichment in the silt fraction, and quartz grain micro- morphology is traced in a multi-100-kyr lake sediment archive as indicator data for cryogenic weathering. Constant cryogenic weathering conditions are inferred for at least the last 220 000 years from a lake sediment core of El'gygytgyn Crater, northeast Russia. This is the longest continuous ter- restrial archive currently known for the continental Arctic. Quartz enrichment in the fines evolves from seasonal freeze-thaw weathering as demonstrated in laboratory testing where over 100 freeze and thaw cycles crack quartz grains preferentially over feldspar. Microscopic grain fea- tures demonstrate that freeze-thaw cycling probably disrupts quartz grains along mineral impurities such as bubble trails, gas-liquid inclusions, or mineralogical sub- grain boundaries. Single-grain micromorphology (e.g. angular outlines, sharp edges, microcracks, brittle surfaces) illustrates how quartz becomes fragmented due to cryogenic cracking of the grains. The single-grain features stemming from the weathering dynamics are preserved even after a grain is transported off site (i.e. in mobile slope material, in seasonal river run-off, into a lake basin) and may serve as first-order proxy data for permafrost conditions in Quater- nary records.

/pdf/quartz-weathering-in-freeze-thaw-cycles-experiment-and-4cut4m8276.pdf

Quartz weathering in freeze–thaw cycles: experiment and application to the El’gygytgyn Crater Lake record for tracing Siberian permafrost history

Brittle and fragile sand and silt is produced in near surface frozen ground. It makes up much of the re-golith in permafrost areas such as Arctic Siberia. Microscopical grain features (e.g. angular outlines, surficial microcracks) illustrate grooves of cryogenic destruction in the course of numerous seasonal freezing and thawing events. Even after a grain is transported off place (i.e. in mobile slope material, in seasonal melt water run-off, into a lake basin), it still keeps the particular weathering traces.This is also valid for a mineralogical peculiarity; quartz is more susceptible to frost weathering than e.g. feldspar, another ubiquitous mineral. Quartz quickly reacts to cryogenic break-up and small grains disintegrate due to thermal fluctuations and the explosive power of expanding ice in micro-meter scale fissures. Quartz enriches in the fines and this anomaly when compared to low latitude weathering is linked to cryogenic weathering. This is demon-strated in an experimental set-up, where after more than 100 freeze and thaw cycles quartz-rich silt is produced in initially fine sandy samples of perma-frost and non-permafrost origins (Figure 1 A). The preferential crack of quartz grains (with reference to feldspar) can be expressed using the so-called Cryo-genic Weathering Index (CWI). This quartz-to-feldspar ratio highlights quartz enrichment in the fines when values are >1 (Konishchev and Rogov, 1993) and marks a zone, which is indicative for ma-terial resulting from cryogenic break-up.The combination of silt abundance, quartz grain micromorphology, and quartz enrichment is used as a proxy data set for frost weathering history in sedi-mentary archives. It has been examined in a 5 m core composed of frozen slope deposits and weath-ered bedrock (P2), in surface samples and along a lake sediment core from Elgygytgyn Impact Crater, Central Chukotka (Figure 1 B+C). This site provides the longest continuous terrestrial archive available for the continental Arctic. The basin was non-glaciated in Quaternary times and studied layers are dating back 220.000 years according to the available age model (Juschus et al., 2007). All frozen ground samples and also the upper 12 meters of the lake sediment core are characterised by silt abundance, cryogenic grain micromorphology, and quartz en-richment in the silt fraction. This argues for persis-tent permafrost conditions in the area as reflected by the continuous input of cryogenic weathering detri-tus into the basin. Even when periods were as warm as or warmer than today (i.e. during the Eemian In-terglacial) the permafrost signal does not disappear according to the lake record.

Quartz Weathering in Freeze-Thaw Cycles; Experiment and Application to Elgygytgyn Crater Lake Record for Tracing Siberian Permafrost History

Morphoscopic studies were conducted with the aid of SEM and TEM microscopes, on quartz grains and fractions not exceeding 2 μm, on soil samples from the continental tundra, alpine meadow and arid steppe. The aim of these studies was to define the features and properties of the quartz grains and fractions, produced by the environment of the cryoarid continental climate of Central Asia. It has been established that in cold and humid climates processes of cryogenic and hydrothermic splitting occur on the surface of quartz grains and in cold and dry climates processes of cryothermic scalling. The increase in the surface area of disintegrated minerals under continental climate conditions is accompanied by cryochemical coating by mineral-organic compounds.

Features of cryogenic environment in soils of continental tundra and arid steppe on the southern Khangai slope under electron microscope

Morphoscopic investigations of quartz grains (0,6–0,8 mm) were carried out with the use of scanning electron microscope. The grains originated from the liquefied horizon of the strongly alkaline permafrost solonchaks of the arid steppe zone of Central Mongolia. The grain surface in this horizon is smoothed due to various processes of chemical corrosion and by deposition of silicate crusts of variable thickness. The record of the preceding abrasion resulting from transportation of weathered material to their deposition site was blurred by the above mentioned processes. The permanently hydrated cool environment favoured moreover the cryohydrothermal block- and granular disintegration as well as the cryothermal and cryomechanical fracture and chipping.

Weathering of quartz grains in the liquefied horizon of permafrost solonchaks in the arid steppe zone, Central Mongolia

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Features of cryogenic environment in soils of continental tundra and arid steppe on the southern Khangai slope under electron microscope

Weathering of quartz grains in the liquefied horizon of permafrost solonchaks in the arid steppe zone, Central Mongolia