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During the burial of mudstones, the associated organic matter undergoes gradual thermal maturation, a key process that can influence the reactivity of organic matter during catagenesis, the formation of hydrocarbon deposits and the chemical weathering of mudstones. Conventional methods for assessing the thermal maturity of organic matter often fail to reflect the geochemical heterogeneity between individual organic phases in mudstone samples. Here, we report an alternative, non‐destructive, surficial and micro‐scale (analytical spot size of ~ 300 nm with about 4 μm diffusion depth for micrometre‐size organic grains) method to evaluate the thermal maturity of organic matter in mudstones using the carbonKα X‐ray spectrum measured by field emission‐electron probe microanalyser (FE‐EPMA). Using this method, we observed correlations between parameter values derived from FE‐EPMA spectra, including the peak position, the peak area and the intra‐sample heterogeneity of these measurements, and independently measured vitrinite/solid bitumen reflectance for a suite of mudstones, representing different age, geological context and burial depth. With the increased values in peak area and position, we identified an increase in the carbon mass fraction of organic matter and the mean nominal oxidation state of carbon approaching zero. These trends, which are consistent with aromatisation and graphitisation, provide the rationale for using FE‐EPMA to estimate the thermal maturity of organic matter. To explore some of these trends in more detail, we employed time‐of‐flight secondary ionisation mass spectrometry, X‐ray photoelectron spectroscopy and optical reflectance measurements on a subset of samples. 

Middle and Late Holocene sediments have not been extensively sampled in Lake Tanganyika, and much remains unknown about the response of the Rift Valley’s largest lake to major environmental shifts during the Holocene, including the termination of the African Humid Period (AHP). Here, we present an integrated study (sedimentology, mineralogy, and geochemistry) of a radiocarbon-dated sediment core from the Kavala Island Ridge (KIR) that reveals paleoenvironmental variability in Lake Tanganyika since the Middle Holocene with decadal to centennial resolution. Massive blue-gray sandy silts represent sediments deposited during the terminal AHP (~5880–4640 cal yr BP), with detrital particle size, carbon concentrations, light stable isotopes, and mineralogy suggesting an influx of river-borne soil organic matter and weathered clay minerals to the lake at that time. Enhanced by the AHP’s warm and wet conditions, chemical weathering and erosion of Lake Tanganyika’s watershed appears to have promoted considerable nutrient recharge to the lake system. Following a relatively gradual termination of the AHP over the period from ~4640 cal yr BP to ~3680 cal yr BP, laminated and organic carbon-rich sediments began accumulating on the KIR. δ¹⁵N_bulk, C/N, and hydrogen index data suggest high relative primary production from a mix of algae and cyanobacteria, most likely in response to nutrient availability in the water column under a cooler and seasonally dry climate from ~3680 to 1100 cal yr BP. Sediments deposited during the Common Era show considerable variability in magnetic susceptibility, total organic carbon content, carbon isotopes, and C/N, consistent with dynamic hydroclimate conditions that affected the depositional patterns, including substantial changes around the Medieval Climate Anomaly and Little Ice Age. Data from this study highlight the importance of sedimentary records to constrain boundary conditions in hydroclimate and nutrient flux that can inform long-term ecosystem response in Lake Tanganyika.