Testing the use of southern France and Cyprus mouflons as a reference to reconstruct birth season in sheep from oxygen isotope analysis in teeth

An analysis of the origin of an early medieval group of individuals from Gródek based on the analysis of stable oxygen isotopes

Mountain adaptation of caprine herding in the eastern Pyrenees during the Bronze Age: A stable oxygen and carbon isotope analysis of teeth

Recovery and identification of heavily burnt and fragmented skeletal remains pose significant challenges in fire and arson investigations. The ability to identify individuals is crucial in such cases, prompting extensive research into various techniques to aid in the identification process, including isotopic analysis. Although direct personal identification is not achievable through isotopic analysis of skeletal remains, it serves as a valuable tool for obtaining chemical elements of the biological profile. Strontium (Sr), oxygen (O), and carbon (C) isotope analyses have been widely used in archeological contexts but are relatively new approaches in the medicolegal domain. Oxygen isotope analysis, for instance, offers insights into the burning temperature, while strontium isotope analysis provides valuable information for tracing the individual's movement across geologically distinct landscapes. Consequently, the investigation of the impact of heat on the biogenic isotope composition of human bones in forensic contexts has gained significant attention. This article presents a comprehensive overview of the key archeological and forensic questions addressed by Sr–O–C isotope analysis of burnt skeletal remains. By examining the current state of the art and prospects, we aim to contribute to a broader understanding and potential advancements in the field of forensic isotope research.This article is categorized under: Forensic Biology > Interpretation of Biological Evidence Forensic Anthropology > Trauma Analysis

Secondary ion mass spectrometry (SIMS) measurement of oxygen isotopes in apatite has been employed more and more in petrogenetic, metallogenic, and climate change studies. Well‐characterised reference materials are needed due to the matrix effect, but they are yet to be well established. In this study, we conducted in‐situ oxygen isotopic and chemical analyses on six commonly used apatite reference materials (ie, Emerald, Kovdor, McClure, Mud Tank, Otter Lake, and Slyudyanka) and two in‐house apatite references (Qinghu and GEMS 203) to assess their oxygen isotope homogeneity and applicability for microbeam analyses. Our results show that all these apatite references are in general chemically homogeneous. In terms of oxygen isotopes, GEMS 203 (δ 18 O = 9.85 ± 0.40‰ [2SD], corrected by Durango 3), Kovdor (δ 18 O = 6.55 ± 0.38‰, 2SD), and McClure (δ 18 O = 5.94 ± 0.42‰, 2SD) are fairly homogeneous, whereas Emerald (δ 18 O = 10.37 ± 0.45‰, 2SD), Mud Tank (δ 18 O = 6.35 ± 0.46‰, 2SD), Otter Lake (δ 18 O = 9.71 ± 0.47‰, 2SD), Qinghu (δ 18 O = 5.44 ± 0.49‰, 2SD), and Slyudyanka (δ 18 O = 17.49 ± 0.43‰, 2SD) are less homogenous. This indicates that the former group represents better reference materials for in‐situ oxygen isotopic analyses, whilst the latter group can be used as secondary reference material for analytical quality control.

The nitrogen (δ(15)N) and oxygen isotope (δ(18)O) analysis of nitrate (NO(3)(-)) from aqueous samples can be used to determine nitrate sources and to study N transformation processes. For these purposes, several methods have been developed; however, none of them allows an accurate, fast and inexpensive analysis. Here, we present a new simple method for the isolation of nitrate, which is based on the different solubilities of inorganic salts in an acetone/hexane/water mixture. In this solvent, all major nitrate salts are soluble, whereas all other oxygen-bearing compounds such as most inorganic carbonates, sulfates, and phosphates are not. Nitrate is first concentrated by freeze-drying, dissolved in the ternary solvent and separated from insoluble compounds by centrifugation. Anhydrous barium nitrate is then precipitated in the supernatant solution by adding barium iodide. For δ(18)O analysis, dried Ba(NO(3))(2) samples are directly reduced in a high-temperature conversion system to CO and measured on-line using isotope ratio mass spectrometry (IRMS). For δ(15)N analysis, samples are combusted in an elemental analyzer (EA) coupled to an IRMS system. The method has been tested down to 20 µmol NO(3)(-) with a reproducibility (1SD) of 0.1‰ for nitrogen and 0.2-0.4‰ for oxygen isotopes. For nitrogen we observed a small consistent (15) N enrichment of +0.2‰, probably due to an incomplete precipitation process and, for oxygen, a correction for the incorporation of water in the precipitated Ba(NO(3))(2) has to be applied. Apart from being robust, this method is highly efficient and low in cost.

The δ18O of carbonate minerals that formed at Earth's surface is widely used to investigate paleoclimates and paleo-elevations. However, a multitude of hydrologic processes can affect δ18O values, including mixing, evaporation, distillation of parent waters, and carbonate growth temperatures. We combined traditional carbon and oxygen isotope analyses with clumped (Δ47) and triple oxygen isotopes (Δ′17O) analyses in oyster shells (Acutostrea idriaensis) of the Goler Formation in southern California (USA) to obtain insights into surface temperatures and δ18O values of meteoric waters during the early Eocene hothouse climate. The Δ47-derived temperatures ranged from 9 °C to 20 °C. We found a correlation between the δ18O of growth water (δ18Ogw) (calculated using Δ47 temperatures and δ18O of carbonate) and the δ13C values of shells. The Δ′17O values of shell growth waters (0.006‰–0.013‰ relative to Vienna standard mean ocean water–standard light Antarctic precipitation [VSMOW-SLAP]) calculated from Δ′17O of carbonate (−0.087‰ to −0.078‰ VSMOW-SLAP) were lower than typical meteoric waters. These isotopic compositions are consistent with oyster habitation in an estuary. We present a new triple oxygen isotope mixing model to estimate the δ18O value of freshwater supplying the estuary (δ18Ofw). The reconstructed δ18Ofw of −11.3‰ to −14.7‰ (VSMOW) is significantly lower than the δ18Ogw of −4.4‰ to −9.9‰ that would have been calculated using “only” Δ47 and δ18O values of carbonate. This δ18Ofw estimate supports paleogeographic reconstructions of a Paleogene river fed by high-elevation catchments of the paleo–southern Sierra Nevada. Our study highlights the potential for paired Δ47 and Δ′17O analyses to improve reconstructions of meteoric water δ18O, with implications for understanding ancient climates and elevations.

Microfacies analysis and paleoenvironmental significance of palustrine carbonates in the Thakkhola-Mustang Graben (Nepal Himalaya)

Specifying recharge zones and mechanisms of the transitional geothermal field through hydrogen and oxygen isotope analyses with consideration of water-rock interaction

A number of distinct methodologies are available for determining the oxygen isotope composition of minerals and rocks, these include laser-assisted fluorination, secondary ion mass spectrometry (SIMS) and UV laser ablation. In this review we focus on laser-assisted fluorination, which currently achieves the highest levels of precision available for oxygen isotope analysis. In particular, we examine how results using this method have furthered our understanding of early-formed differentiated meteorites. Due to its rapid reaction times and low blank levels, laser-assisted fluorination has now largely superseded the conventional externally-heated Ni “bomb” technique for bulk analysis. Unlike UV laser ablation and SIMS analysis, laser-assisted fluorination is not capable of focused spot analysis. While laser fluorination is now a mature technology, further analytical improvements are possible via refinements to the construction of sample chambers, clean-up lines and the use of ultra-high resolution mass spectrometers.High-precision oxygen isotope analysis has proved to be a particularly powerful technique for investigating the formation and evolution of early-formed differentiated asteroids and has provided unique insights into the interrelationships between various groups of achondrites. A clear example of this is seen in samples that lie close to the terrestrial fractionation line (TFL). Based on the data from conventional oxygen isotope analysis, it was suggested that the main-group pallasites, the howardite eucrite diogenite suite (HEDs) and mesosiderites could all be derived from a single common parent body. However, high precision analysis demonstrates that main-group pallasites have a Δ17O composition that is fully resolvable from that of the HEDs and mesosiderites, indicating the involvement of at least two parent bodies. The range of Δ17O values exhibited by an achondrite group provides a useful means of assessing the extent to which their parent body underwent melting and isotopic homogenization. Oxygen isotope analysis can also highlight relationships between ungrouped achondrites and the more well-populated groups. A clear example of this is the proposed link between the evolved GRA 06128/9 meteorites and the brachinites.The evidence from oxygen isotopes, in conjunction with that from other techniques, indicates that we have samples from approximately 110 asteroidal parent bodies (∼60 irons, ∼35 achondrites and stony-iron, and ∼15 chondrites) in our global meteorite collection. However, compared to the likely size of the original protoplanetary asteroid population, this is an extremely low value. In addition, almost all of the differentiated samples (achondrites, stony-iron and irons) are derived from parent bodies that were highly disrupted early in their evolution.High-precision oxygen isotope analysis of achondrites provides some important insights into the origin of mass-independent variation in the early Solar System. In particular, the evidence from various primitive achondrite groups indicates that both the slope 1 (Y&R) and CCAM lines are of primordial significance. Δ17O differences between water ice and silicate-rich solids were probably the initial source of the slope 1 anomaly. These phases most likely acquired their isotopic composition as a result of UV photo-dissociation of CO that took place either in the early solar nebula or precursor giant molecular cloud. Such small-scale isotopic heterogeneities were propagated into larger-sized bodies, such as asteroids and planets, as a result of early Solar System processes, including dehydration, aqueous alteration, melting and collisional interactions.There is increasing evidence that chondritic parent bodies accreted relatively late compared to achondritic asteroids. This may account for the fact that apart from a few notable exceptions’ such as the aubrite-enstatite chondrite association, known chondrite groups could not have been the parents to the main achondrite groups.

Oxygen isotope analysis of archaeological skeletal remains is an increasingly popular tool to study past human migrations. It is based on the assumption that human body chemistry preserves the δ18O of precipitation in such a way as to be a useful technique for identifying migrants and, potentially, their homelands. In this study, the first such global survey, we draw on published human tooth enamel and bone bioapatite data to explore the validity of using oxygen isotope analyses to identify migrants in the archaeological record. We use human δ18O results to show that there are large variations in human oxygen isotope values within a population sample. This may relate to physiological factors influencing the preservation of the primary isotope signal, or due to human activities (such as brewing, boiling, stewing, differential access to water sources and so on) causing variation in ingested water and food isotope values. We compare the number of outliers identified using various statistical methods. We determine that the most appropriate method for identifying migrants is dependent on the data but is likely to be the IQR or median absolute deviation from the median under most archaeological circumstances. Finally, through a spatial assessment of the dataset, we show that the degree of overlap in human isotope values from different locations across Europe is such that identifying individuals’ homelands on the basis of oxygen isotope analysis alone is not possible for the regions analysed to date. Oxygen isotope analysis is a valid method for identifying first-generation migrants from an archaeological site when used appropriately, however it is difficult to identify migrants using statistical methods for a sample size of less than c. 25 individuals. In the absence of local previous analyses, each sample should be treated as an individual dataset and statistical techniques can be used to identify migrants, but in most cases pinpointing a specific homeland should not be attempted.

The isotopic composition of water in hydrated minerals, such as gypsum and jarosite, has numerous applications in studies of recent climate change, ore formation, and soil development. However, oxygen and hydrogen isotope analysis of water of crystallization is currently a complex procedure. Commonly used techniques involve offline extraction of water from hydrated minerals and subsequent isotope analysis. Such methods are time-consuming, require relatively large sample sizes, and the stepwise procedure has to be carried out with extreme caution to avoid erroneous results. We present a novel online method for the oxygen and hydrogen isotope analysis of water of crystallization in hydrous minerals. Gypsum (CaSO 4.2H 2O) samples, 2 mg in size, are reacted in a simply modified carbon reducing furnace connected to a continuous-flow mass spectrometer system. Analysis time is less than 10 min/sample. The precision (2 std dev mean) of our method for 2-mg gypsum (30 mumol of H 2O) samples is 0.3 per thousand for oxygen and less than 1.4 per thousand for hydrogen isotope measurements. For oxygen isotope analysis alone, samples as small as 0.2 mg of gypsum can be analyzed with a precision of 0.3 per thousand.

Oxygen Isotope Analysis of Animal Bone Phosphate: Method Refinement, Influence of Consolidants, and Reconstruction of Palaeotemperatures for Holocene Sites

The accumulation of non-formula elements in zircons during weathering: Ancient zircons from the Jack Hills, Western Australia

Tin and tungsten are important metals for the industrializing society. Deciphering the origin and evolution of hydrothermal fluids responsible for their formation is critical to underpin genetic models of ore formation. Traditional approaches obtain isotopic information mainly from bulk analysis of both ore and gangue minerals, or less frequently from in situ analysis of gangue minerals, which either bear inherited complexities and uncertainties or are indirect constraints. Hence, directly obtaining isotopic information from ore minerals such as cassiterite by in situ techniques is warranted. However, this has been hampered by challenges from both analytical and applicational aspects. In this study, we first demonstrate a lack of crystallographic orientation effects during cassiterite ion microprobe oxygen isotope analysis. Along with our newly developed matrix-matched reference material, the Yongde-Cst, which has a recommended δ18O value of 1.36 ± 0.16‰ (VSMOW) as defined by gas source isotope ratio mass spectrometry, in situ oxygen isotope analysis of cassiterite now is possible. We further refine the oxygen isotope fractionation (1000 ln α) for quartz-cassiterite by first-principles calculations, which is given by the equation of 1.259 × 106/T2 + 8.15 × 103/T − 4.72 (T is temperature in Kelvin). The 1000 ln α for quartz-cassiterite has a sensitive response to temperature, and makes cassiterite-quartz an excellent mineral pair in oxygen isotope thermometry, as described by the equation of T (℃) = 2427 × (δ18Oqtz − δ18Ocst)−0.4326 − 492.4. Using the well-established 1000 ln α of quartz-water, 1000 ln α of cassiterite-water is derived as 2.941 × 106/T2 − 11.45 × 103/T + 4.72 (T in Kelvin), which shows a weak response to temperature. This makes cassiterite an ideal mineral from which to derive δ18O of fluids as robust temperature estimates are no longer a prerequisite. We have applied oxygen isotope analysis to cassiterite samples from six Sn(-W) deposits in China. The results show considerable variability in δ18O values both within a single deposit and among studied deposits. Combining the δ18O of cassiterite samples and the equilibrium oxygen isotope fractionation, we find that the δ18O values of ore-forming fluids show a strong magmatic affinity with variable but mostly no to low degree involvements (~0-10%) of meteoric water, hence our results invite a reassessment on the extent and role of meteoric water in Sn-W mineralization. This study demonstrates that in situ oxygen isotope analysis of cassiterite is a promising tool to refine sources of ore-forming fluids, and to decode hydrothermal dynamics controlling tin and tungsten mineralization.

Holocene Climate Inferred from Oxygen Isotope Ratios in Lake Sediments, Central Brooks Range, Alaska