Development of freeze-thaw processing technique for disaggregation of indurated mudrocks and enhanced recovery of calcareous microfossils

Microfossil extraction from indurated mudrocks is widely acknowledged as challenging, especially for foraminifera. Here we report development of the freeze–thaw extraction method through the addition of rapid heating, detergent and ultrasound stages. We use indurated mudrock samples from the Toarcian (Early Jurassic) of Yorkshire, UK to assess the effectiveness and develop the freeze–thaw method. We compare our results from freeze–thaw with those from standard foraminifera processing techniques, including the use of hydrogen peroxide. Processing by freeze–thaw increased the degree of mudrock disaggregation and resulted in no damage or dissolution of foraminifera. Following the freeze–thaw method with treatment in white spirit and sodium hexametaphosphate aided the separation of foraminifera from the disaggregated clays and was twice as efficient as pressure washing. Samples processed with hydrogen peroxide contained damaged microfossils and an under representation of delicate calcareous foraminifera. Many other studies of indurated mudrocks have used hydrogen peroxide to extract foraminifera, and this might have resulted in apparently barren intervals. The freeze–thaw method outlined here provides a low-cost, low-risk and successful method of disaggregating and extracting calcareous microfossils from indurated mudrocks. We anticipate our method may be relevant for other fossil groups and merits further development

Portable X‐ray fluorescence spectroscopy as a tool for cyclostratigraphy

Cyclostratigraphic studies are used to create relative and high‐resolution timescales for sedimentary successions based on identification of regular cycles in climate proxy data. This method typically requires the construction of long high‐resolution datasets. In this study, we have demonstrated the efficacy of portable X‐ray fluorescence spectroscopy (pXRF) as a non‐destructive method of generating compositional data for cyclostratigraphy. The rapidity (100 samples per day) and low cost of pXRF measurements provide advantages over relatively time‐consuming and costly elemental and stable isotopic measurements that are commonly used for cyclostratigraphy. The non‐destructive nature of pXRF also allows other geochemical analyses on the same samples. We present an optimized protocol for pXRF elemental concentration measurement in powdered rocks. The efficacy of this protocol for cyclostratigraphy is demonstrated through analysis of 360 Toarcian mudrock samples from North Yorkshire, UK, that were previously shown to exhibit astronomical forcing of [CaCO3], [S] and δ13Corg. Our study is the first to statistically compare the cyclostratigraphic results of pXRF analysis with more established combustion analysis. There are strong linear correlations of pXRF [Ca] with dry combustion elemental analyzer [CaCO3] (r2=0.7616), and pXRF [S] and [Fe] with dry combustion elemental analyzer [S] (r2=0.9632 and r2=0.9274 respectively). Spectral and cross‐spectral analysis demonstrates that cyclicity previously recognized in [S], significant above the 99.99% confidence level, is present above the 99.92% and 99.99% confidence levels in pXRF [S] and [Fe] data respectively. Cyclicity present in [CaCO3] data above the 99.96% confidence level is also present in pXRF [Ca] above the 98.12% confidence level

Precise Re–Os ages of organic-rich mudrocks and the Os isotope composition of Jurassic seawater

Rhenium and osmium isotope and abundance data have been obtained on precisely-located samples from three suites of immature, organic-rich mudrocks from Jurassic coastal outcrops in England, The data provide accurate whole-rode ages of 207 +/- 12 Ma, 181 +/- 13 Ma and 155 +/- 4.3 Ma for suites of Hettangian, Toarcian (exaratum Subzone) and Kimmeridgian (sensu anglico, wheatleyensis Subzone) samples. These new Re-Os ages are indistinguishable, within the assigned analytical uncertainties, from interpolated depositional ages estimated from published geological timescales, and establish the importance of the Re-Os dating technique for chronostratigraphic studies. Early-diagenetic pyrite nodules possess levels of Re and Os which are similar to 1-2 orders of magnitude lower than in the enclosing organic-rich mudrocks, indicating that these elements had already been removed from sediment pore waters at the time of nodule formation. Thus the Re-Os isotope system in these organic-rich mudrocks has been closed since, or from very soon after, the time of sediment deposition. Because most of the Re (98+%) and Os (95-99.8+%) in the mudrocks is shown to be hydrogenous, the Os-187/Os-188((i)) of the samples is interpreted to be that of contemporaneous seawater. The data thereby provide the first estimates of the Os isotope composition of Jurassic seawater. During the earliest Jurassic (Hettangian), the seawater Os-187/Os-188 ratio was extremely unradiogenic (similar to 0.15); it had increased to similar to 0.8 at the end of the Early Jurassic (Toarcian) similar to 20 Ma later, while in the Late Jurassic (Kimmeridgian) the seawater Os-187/Os-188 ratio was similar to 0.59. The most likely explanation for the unradiogenic Os isotope composition of Hettangian seawater is that the contribution of unradiogenic Os to the oceans from the hydrothermal alteration of oceanic crust greatly exceeded the input of radiogenic Os from the continents at that time. This interpretation is in Line with observations suggesting that global weathering rates were low in the Hettangian, and that increased hydrothermal and volcanic activity preceded the break-up of Pangea. The Re/Os ratios of Hettangian mudrocks (and by inference, of contemporaneous seawater) are similar to those of mudrocks deposited at later times during the Jurassic, and argues against the unradiogenic Os in Hettangian seawater being derived from extraterrestrial meteoritic sources

Drivers of ecosystem and climate change in tropical West Africa over the past ∼540 000 years

A paucity of empirical non-marine data means that uncertainty surrounds the impact of climate change on terrestrial ecosystems in tropical regions beyond the last glacial period. The sedimentary fill of the Bosumtwi impact crater (Ghana) provides the longest continuous Quaternary terrestrial archive of environmental change in West Africa, spanning the last ∼1.08 million years. Here we explore the drivers of change in ecosystem and climate in tropical West Africa for the past ∼540 000 years using pollen analysis and the nitrogen isotope composition of bulk organic matter preserved in sediments from Lake Bosumtwi. Variations in grass pollen abundance (0−99%) indicate transitions between grassland and forest. Coeval variations in the nitrogen isotopic composition of organic matter indicate that intervals of grassland expansion coincided with minimum lake levels and low regional moisture availability. The observed changes responded to orbitally paced global climate variations on both glacial–interglacial and shorter timescales. Importantly, the magnitude of ecosystem change revealed by our data exceeds that previously determined from marine records, demonstrating for the first time the high sensitivity of tropical lowland ecosystems to Quaternary climate change

Integrated stratigraphy of the Kimmeridge Clay Formation (Upper Jurassic) based on exposures and boreholes in south Dorset, UK

For the purposes of a high-resolution multi-disciplinary study of the Upper Jurassic Kimmeridge Clay Formation, two boreholes were drilled at Swanworth Quarry and one at Metherhills, south Dorset, UK. Together, the cores represent the first complete section through the entire formation close to the type section. We present graphic logs that record the stratigraphy of the cores, and outline the complementary geophysical and analytical data sets (gamma ray, magnetic susceptibility, total organic carbon, carbonate, [delta]13Corg). Of particular note are the new borehole data from the lowermost part of the formation which does not crop out in the type area. Detailed logs are available for download from the Kimmeridge Drilling Project web-site at http://kimmeridge.earth.ox.ac.uk/. Of further interest is a mid-eudoxus Zone positive shift in the [delta]13Corg record, a feature that is also registered in Tethyan carbonate successions, suggesting that it is a regional event and may therefore be useful for correlation. The lithostratigraphy of the cores has been precisely correlated with the nearby cliff section, which has also been examined and re-described. Magnetic-susceptibility and spectral gamma-ray measurements were made at a regular spacing through the succession, and facilitate core-to-exposure correlation. The strata of the exposure and core have been subdivided into four main mudrock lithological types: (a) medium-dark–dark-grey marl; (b) medium-dark–dark grey–greenish black shale; (c) dark-grey–olive-black laminated shale; (d) greyish-black–brownish-black mudstone. The sections also contain subordinate amounts of siltstone, limestone and dolostone. Comparison of the type section with the cores reveals slight lithological variation and notable thickness differences between the coeval strata. The proximity of the boreholes and different parts of the type section to the Purbeck–Isle of Wight Disturbance is proposed as a likely control on the thickness changes

Chemotaxonomy as a tool for interpreting the cryptic diversity of Poaceae pollen

The uniform morphology of different species of Poaceae (grass) pollen means that identification to below family level using light microscopy is extremely challenging. Poor taxonomic resolution reduces recoverable information from the grass pollen record, for example, species diversity and environmental preferences cannot be extracted. Recent research suggests Fourier Transform Infra-red Spectroscopy (FTIR) can be used to identify pollen grains based on their chemical composition. Here, we present a study of twelve species from eight subfamilies of Poaceae, selected from across the phylogeny but from a relatively constrained geographical area (tropical West Africa) to assess the feasibility of using this chemical method for identification within the Poaceae family. We assess several spectral processing methods and use K-nearest neighbour (k-nn) analyses, with a leave-one-out cross-validation, to generate identification success rates at different taxonomic levels. We demonstrate we can identify grass pollen grains to subfamily level with an 80% success rate. Our success in identifying Poaceae to subfamily level using FTIR provides an opportunity to generate high taxonomic resolution datasets in research areas such as palaeoecology, forensics, and melissopalynology quickly and at a relatively low cost

Environmental controls on the distribution and diversity of lentic Chironomidae (Insecta: Diptera) across an altitudinal gradient in tropical South America

To predict the response of aquatic ecosystems to future global climate change, data on the ecology and distribution of keystone groups in freshwater ecosystems are needed. In contrast to mid- and high-latitude zones, such data are scarce across tropical South America (Neotropics). We present the distribution and diversity of chironomid species using surface sediments of 59 lakes from the Andes to the Amazon (0.1–17°S and 64–78°W) within the Neotropics. We assess the spatial variation in community assemblages and identify the key variables influencing the distributional patterns. The relationships between environmental variables (pH, conductivity, depth, and sediment organic content), climatic data, and chironomid assemblages were assessed using multivariate statistics (detrended correspondence analysis and canonical correspondence analysis). Climatic parameters (temperature and precipitation) were most significant in describing the variance in chironomid assemblages. Temperature and precipitation are both predicted to change under future climate change scenarios in the tropical Andes. Our findings suggest taxa of Orthocladiinae, which show a preference to cold high-elevation oligotrophic lakes, will likely see range contraction under future anthropogenic-induced climate change. Taxa abundant in areas of high precipitation, such as Micropsectra and Phaenopsectra, will likely become restricted to the inner tropical Andes, as the outer tropical Andes become drier. The sensitivity of chironomids to climate parameters makes them important bio-indicators of regional climate change in the Neotropics. Furthermore, the distribution of chironomid taxa presented here is a vital first step toward providing urgently needed autecological data for interpreting fossil chironomid records of past ecological and climate change from the tropical Andes

A new Liassophlebiidae (Odonata: Heterophlebioidea) from strata close to the Triassic-Jurassic boundary in Somerset, UK

Liassophlebiidae is an extinct family of damsel-dragonflies found in Upper Triassic and Lower Jurassic strata of Europe, Asia and Antarctica. Whilst Liassophlebiidae is well represented by Lower Jurassic fossils, their lowest occurrence in the Upper Triassic has hitherto only been suggested by three fragmentary specimens. These were originally ascribed to two species: Liassophlebia withersi and Liassophlebia batheri, but the latter is now considered nomen dubium. Here we describe a fourth, better preserved specimen that is likely to be Rhaetian (Late Triassic) in age. The specimen, BRSMG Cg3101 a+b, was collected from Bowdens Quarry, Somerset, UK, from the lower part of the White Lias Formation. The specimen comprises an incomplete forewing attributed to Liassophlebia due to: the small number of antenodals, antesubnodals and crossveins between RP and MA based RP3/4 in the base of RP2 opposite the subnodus; a straight and elongate secondary longitudinal vein in the postdiscoidal area; numerous cells and secondary veins in radial and median areas. The specimen is likely to represent a new species and provides stronger evidence than the previous three specimens of the presence of Liassophlebiidae during the late Rhaetian. Its stratigraphical position suggests that Liassophlebiidae arose in the immediate aftermath of the Triassic-Jurassic mass extinction

The fossil insect assemblage associated with the Toarcian (Lower Jurassic) oceanic anoxic event from Alderton Hill, Gloucestershire, UK

Extreme global warming and environmental changes associated with the Toarcian (Lower Jurassic) Oceanic Anoxic Event (T-OAE, ∼183 Mya) profoundly impacted marine organisms and terrestrial plants. Despite the exceptionally elevated abundances of fossil insects from strata of this age, only assemblages from Germany and Luxembourg have been studied in detail. Here, we focus on the insect assemblage found in strata recording the T-OAE at Alderton Hill, Gloucestershire, UK, where <15% of specimens have previously been described. We located all known fossil insects (n = 370) from Alderton Hill, and used these to create the first comprehensive taxonomic and taphonomic analysis of the entire assemblage. We show that a diverse palaeoentomofaunal assemblage is preserved, comprising 12 orders, 21 families, 23 genera and 21 species. Fossil disarticulation is consistent with insect decay studies. The number of orders is comparable with present-day assemblages from similar latitudes (30°-40°N), including the Azores, and suggests that the palaeoentomofauna reflects a life assemblage. At Alderton, Hemiptera, Coleoptera and Orthoptera are the commonest (56.1%) orders. The high abundance of Hemiptera (22.1%) and Orthoptera (13.4%) indicates well-vegetated islands, while floral changes related to the T-OAE may be responsible for hemipteran diversification. Predatory insects are relatively abundant (∼10% of the total assemblage) and we hypothesise that the co-occurrence of fish and insects within the T-OAE represents a jubilee-like event. The marginally higher proportion of sclerotised taxa compared to present-day insect assemblages possibly indicates adaptation to environmental conditions or taphonomic bias. The coeval palaeoentomofauna from Strawberry Bank, Somerset is less diverse (9 orders, 12 families, 6 genera, 3 species) and is taphonomically biased. The Alderton Hill palaeoentomofauna is interpreted to be the bestpreserved and most representative insect assemblage from Toarcian strata in the UK. This study provides an essential first step towards understanding the likely influence of the TOAE on insects

Mounds in Oxia Planum: The Burial and Exhumation of the ExoMars Rover Landing Site

Oxia Planum, the planned landing site of the ExoMars ‘Rosalind Franklin’ rover, is a low relief clay-bearing plain, of which approximately 1% is covered by 396 upstanding isolated landforms (‘mounds’). The mounds are continuous with a circum-Chryse mound population representing the remnants of a regionally significant Noachian-aged deposit. This detailed study suggests that the Oxia Planum mounds are also erosional remnants of this deposit, with little evidence to suggest they are constructional landforms such as sedimentary volcanoes. We calculate that up to 130 meters of mound-forming material has been removed from the landing site through erosion. The mound-forming layer lies unconformably on the clay-bearing plains with the upper surface severely truncated by significant erosion resulting in the topography we see today. The mounds themselves comprise at least three members, distinct in color and texture, separated stratigraphically by further unconformities. Calculated minimum erosion/deposition rates of the removed mound material are comparable to previous Noachian estimates, suggesting a more erosive (and probably therefore warmer and/or wetter) environment than today. The clay-bearing materials which remain buried directly under the mounds have been continually protected from the martian environment since the Noachian, and are likely to represent some of the most pristine clay-rich materials in the landing site. By inference, the plains directly adjacent to the mounds are most likely to have been exposed for less time than areas further from the mounds. These are therefore amongst the most likely locations where Rosalind Franklin could sample recently exposed materials and hence detect biosignatures