This paper presents a systematic evaluation of a commercially available strontium-specific extraction chromatographic resin based on a crown ether (Sr specÔ), for use in applications of Sr isotope ratio analysis dealing with samples displaying a complex and/or Ca-rich matrix composition. A protocol, consisting of (i) loading a sample digest in 7 M HNO 3 onto the resin, (ii) rinsing the resin with 7 M HNO 3 to remove concomitant matrix elements and (iii) rinsing the resin with 0.05 M HNO 3 to strip off the purified Sr fraction, was found to provide the best results. The performance in terms of (i) the purity of the Sr fraction obtained, (ii) the efficiency of Rb/Sr and Ca/Sr separation, (iii) the Sr recovery from samples with a complex and Ca-rich matrix composition and (iv) the Sr isotope ratios obtained using multi-collector ICP-MS, was evaluated for various amounts (250, 500, 750 and 2000 mL) of resin using digests of bone and soil certified reference materials, dental tissues, fluorite and glass samples. Further, it was investigated whether or not the isolation protocol introduces Sr isotopic fractionation. Also the possibility of regenerating the resin after use, allowing multiple use of the resin, was assessed. Finally, the Sr isotopic composition of 2 bone (NIST SRM 1400 Bone Ash and NIST SRM 1486 Bone Meal) and 2 soil (BCR CRM 141 Calcareous Loam Soil and BCR CRM 142 Light Sandy Soil) certified reference materials was determined. The method was shown to be fit-for-purpose for population migration studies and provenancing of archaeological artefacts, and is expected to be suited for a broad range of Sr isotope ratio applications.
This study presents the first ever lead isotope ratio data for copper ore samples (malachite and azurite) from the Sierra El Aramo (Asturias, northwestern Spain). The aim of this study was to supplement information in the existing reference database on the lead isotopic composition of Spanish ores. The Sierra El Aramo is particularly important because, while no data for the Asturian ores have been published so far, this northern province of Spain has played a significant role in terms of copper exploitation and metallurgy since the Copper Age.
The present study focuses on the development and evaluation of an individual-specific transgenerational marking procedure using two enriched barium isotopes, (135)Ba and (137)Ba, mixed at a given and selectable molar ratio. The method is based on the deconvolution of the isotope patterns found in the sample into four molar contribution factors: natural xenon (Xe nat), natural barium (Ba nat), Ba135, and Ba137. The ratio of molar contributions between Ba137 and Ba135 is constant and independent of the contribution of natural barium in the sample. This procedure was tested in brown trout ( Salmo trutta ) kept in captivity. Trout were injected with three different Ba137/Ba135 isotopic signatures ca. 7 months and 7 days before spawning to compare the efficiency of the marking procedure at long and short term, respectively. The barium isotopic profiles were measured in the offspring by means of inductively coupled plasma mass spectrometry. Each of the three different isotopic signatures was unequivocally identified in the offspring in both whole eggs and larvae. For 9 month old offspring, the characteristic barium isotope signatures could also be detected in the otoliths even in the presence of a high and variable amount of barium of natural isotope abundance. In conclusion, it can be stated that the proposed dual-isotope marking is inheritable and can be detected after both long-term and short-term marking. Furthermore, the dual-isotope marking can be made individual-specific, so that it allows identification of offspring from a single individual or a group of individuals within a given fish group.
The present study evaluates the use of an individual-specific transgenerational barium dual-isotope procedure and its application to salmon specimens from the Sella River (Asturias, Spain). For such a purpose, the use of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) in combination with multiple linear regression for the determination of the isotopic mark in the otoliths of the specimens is presented. In this sense, a solution in which two barium-enriched isotopes ((137)Ba and (135)Ba) were mixed at a molar ratio of ca. 1:3 (N Ba137/N Ba135) was administered to eight returning females caught during the spawning period. After injection, these females, as well as their offspring, were reared in a governmental hatchery located in the council of Cangas de Onís (Asturias, Spain). For comparison purposes, as well as for a time-monitoring control, egg and larva data obtained by solution analysis ICP-MS are also given. Otoliths (9-month-old juveniles) of marked offspring were analysed by LA-ICP-MS demonstrating a 100 % marking efficacy of this methodology. The capabilities of the molar fraction approach for 2D imaging of fish otoliths are also addressed.
This study is focused on the El Milagro mine (Asturias, Spain) and is part of a large‐scale effort on the measurement of the lead isotopic composition of Spanish copper ores from prehistoric mines in the provinces of Asturias and León, from which no data were available until recently. Lead isotopic values are compared to the published lead data from the El Aramo mine in the same region. The results show that both mines have a very similar lead isotopic composition, apart from some highly radiogenic samples in the El Milagro mine, which are clearly different from those previously reported for the Iberian Peninsula.
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