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An interlaboratory study of Mg/Ca and Sr/Ca ratios in three commercially available carbonate reference materials (BAM RS3, CMSI 1767, and ECRM 752‐1) was performed with the participation of 25 laboratories that determine foraminiferal Mg/Ca ratios worldwide. These reference materials containing Mg/Ca in the range of foraminiferal calcite (0.8 mmol/mol to 6 mmol/mol) were circulated with a dissolution protocol for analysis. Participants were asked to make replicate dissolutions of the powdered samples and to analyze them using the instruments and calibration standards routinely used in their laboratories. Statistical analysis was performed in accordance with the International Standardization Organization standard 5725, which is based on the analysis of variance (ANOVA) technique. Repeatability (RSDr%), an indicator of intralaboratory precision, for Mg/Ca determinations in solutions after centrifuging increased with decreasing Mg/Ca, ranging from 0.78% at Mg/Ca = 5.56 mmol/mol to 1.15% at Mg/Ca = 0.79 mmol/mol. Reproducibility (RSDR%), an indicator of the interlaboratory method precision, for Mg/Ca determinations in centrifuged solutions was noticeably worse than repeatability, ranging from 4.5% at Mg/Ca = 5.56 mmol/mol to 8.7% at Mg/Ca = 0.79 mmol/mol. Results of this study show that interlaboratory variability is dominated by inconsistencies among instrument calibrations and highlight the need to improve interlaboratory compatibility. Additionally, the study confirmed the suitability of these solid standards as reference materials for foraminiferal Mg/Ca (and Sr/Ca) determinations, provided that appropriate procedures are adopted to minimize and to monitor possible contamination from silicate mineral phases.
Ancient human mobility at the individual level is conventionally studied by the diverse application of suitable techniques (e.g. aDNA, radiogenic strontium isotopes, as well as oxygen and lead isotopes) to either hard and/or soft tissues. However, the limited preservation of coexisting hard and soft human tissues hampers the possibilities of investigating high-resolution diachronic mobility periods in the life of a single individual. Here, we present the results of a multidisciplinary study of an exceptionally well preserved circa 3.400-year old Danish Bronze Age female find, known as the Egtved Girl. We applied biomolecular, biochemical and geochemical analyses to reconstruct her mobility and diet. We demonstrate that she originated from a place outside present day Denmark (the island of Bornholm excluded), and that she travelled back and forth over large distances during the final months of her life, while consuming a terrestrial diet with intervals of reduced protein intake. We also provide evidence that all her garments were made of non-locally produced wool. Our study advocates the huge potential of combining biomolecular and biogeochemical provenance tracer analyses to hard and soft tissues of a single ancient individual for the reconstruction of high-resolution human mobility.
[1] We present new annually resolved d18 O, d13 C, Mg/Ca, and Sr/Ca ratio records for two shells of the fast growing Mediterranean fan mussel Pinna nobilis, collected from proximal Spanish coast sea grass meadows. The relationship between the potential geochemical proxies and ontogenetic and environmental controlling factors is investigated. Specifically, the use of shell Mg/Ca and Sr/Ca ratios as potential calcification temperature proxies, the latter calculated from measured shell d
18O values, has been assessed. The d
18O cycles along the growth axis indicate that our P. nobilis specimens are $10.5 and $4.5 years old Shell Sr/Ca ratios do not exhibit any consistent interannual cyclicity and are not correlated to temperature. A subtle ontogenetic effect on shell Mg/Ca ratios was observed during the first 4.5 years of recorded growth but was highly evident during the organism's later growth years. In P. nobilis shells, different mechanisms influence ontogenetic variation in shell Mg/Ca and d 18 O records. Shell Mg/Ca ratios from the first 4.5 years of growth correlate significantly to temperature, in a best fit relationship described by the equation Mg/Ca = 17.16 ± 1.95 * exp(0.022 ± 0.004 * T). P. nobilis shell Mg/Ca records therefore are a valid temperature proxy only during an early growth phase. For the same range of temperatures, shell Mg/Ca ratios in P. nobilis are approximately 1/3 lower than those reported for inorganic calcite but 3 to 4 times higher than in another bivalve species, Mytilus trossulus, and 4 to 16 times higher than in foraminifera. We suggest these offsets are due to a higher degree of similarity between seawater and calcification-fluid composition in P. nobilis than in other bivalves and foraminifera. The observed shell Mg/Ca ratio change per°C of 2.2% also is lower than that observed for inorganic and other biogenic calcites. Our findings strongly support taxon-and species-specific Mg/Ca-temperature relationships for bivalves and other calcifying organisms. An appreciation of the physiology and calcification mechanisms of any biogenic carbonate archive therefore is paramount prior to the application of stable-isotope and element/Ca ratio proxies for paleotemperature reconstructions.
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