Alban Petitjean, Olivier Musset, Pierre Sansjofre, Christophe Thomazo
{"title":"A Laser-Laser Method for In Situ C and O Isotope Measurements in Carbonate Materials","authors":"Alban Petitjean, Olivier Musset, Pierre Sansjofre, Christophe Thomazo","doi":"10.1111/ggr.70023","DOIUrl":"https://doi.org/10.1111/ggr.70023","url":null,"abstract":"<p>A portable device was developed to produce CO<sub>2</sub> through laser-induced calcination of carbonates that can be paired with a commercial field-deployable isotope ratio mass spectrometer. This new set-up allows for direct measurements of carbon (δ<sup>13</sup>C) and oxygen (δ<sup>18</sup>O) isotope ratios of carbonates under field conditions. The set-up was designed with a pistol-form handset and backpack for ease of handling by a single operator in the field. We demonstrate how the sampling prototype circumvents the steps of sample collection, grinding, drying and acid digestion by directly producing CO<sub>2</sub> from a raw rock sample in conditions that are representative of fieldwork. The CO<sub>2</sub> evolved using our new device was isotopically measured off-site, using an isotope-ratio infrared spectrometer and the results were compared with those from a classical preparation that used acid digestion. Different ways to achieve the necessary threshold of CO<sub>2</sub> concentration for subsequent isotope measurements are discussed. Overall, we demonstrate that this laser portable calcination device allows for isotope measurements after a minimal conversion of 32 mg of carbonate material with an uncertainty at 1<i>s</i> of 0.41 and 0.68‰ for δ<sup>13</sup>C and δ<sup>18</sup>O, respectively. The comparison with measurements performed after acid digestion shows that the uncertainty in the preparation technique is 0.01 and 0.03‰ for δ<sup>13</sup>C and δ<sup>18</sup>O, respectively. Overall, the laser-induced calcination portable device offers an avenue for fast, accurate and remote measurements of carbonate isotope ratios, but field specific challenges such as the water content of samples also need to be considered.</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"97-113"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147567682","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"地球科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Marco Silva, Cristiano Lana, Ricardo Scholz, Ian Buick, Sandra Kamo, Nick M.W. Roberts, Axel Gerdes, Michael Wiedenbeck, Blair Schoene, Francisco E. Apen, Sean P. Gaynor
{"title":"RioM-1: A New Calcite Reference Material for U-Pb LA-ICP-MS Geochronology","authors":"Marco Silva, Cristiano Lana, Ricardo Scholz, Ian Buick, Sandra Kamo, Nick M.W. Roberts, Axel Gerdes, Michael Wiedenbeck, Blair Schoene, Francisco E. Apen, Sean P. Gaynor","doi":"10.1111/ggr.70018","DOIUrl":"https://doi.org/10.1111/ggr.70018","url":null,"abstract":"<p>Determining absolute ages of carbonate diagenesis, faulting, fossil formation, speleothem growth, carbonate-hosted hydrocarbon deposits, vein mineralisation and hydrothermal alteration has become increasingly accessible through LA-ICP-MS U-Pb dating of calcite, complementing traditional isotope dilution methods still applicable to certain materials (e.g., speleothems via micro-drilling). However, well-calibrated reference materials for LA-ICP-MS calcite geochronology remain scarce. Here, we characterise the Rio Maior calcite, designated ‘RioM-1’, as a potential reference material for U-Pb dating by LA-ICP-MS. Fragments (0.1 to 1 cm<sup>3</sup>) from a single scalenohedral crystal were analysed by ID-TIMS (U-Pb), LA-ICP-MS (U-Pb and <sup>87</sup>Sr/<sup>86</sup>Sr), and SIMS (O isotopes). RioM-1 displays high U mass fraction and low, though variable, proportions of common Pb. Combined ID-TIMS analyses from two independent laboratories yielded a Tera-Wasserburg lower intercept date of 63.93 ± 0.11 Ma (2<i>s</i>, MSWD = 1.3, <i>n</i> = 16). LA-ICP-MS U-Pb data from three independent laboratories are concordant with the TIMS age, producing a pooled date of 64.10 ± 0.12/1.2 Ma (2<i>s</i>, MSWD = 7.7, <i>n</i> = 708) and an initial <sup>207</sup>Pb/<sup>206</sup>Pb ratio of 0.85 ± 0.01. Other calcite reference materials, when normalised to RioM-1, yielded dates within uncertainty of their published values. SIMS measurements returned a mean <sup>18</sup>O/<sup>16</sup>O of 0.002044450 ± 181 (1<i>s</i>) and δ<sup>18</sup>O<sub>SMOW</sub> of 19.57 ± 0.92‰ (1<i>s</i>), while LA-ICP-MS strontium isotope measurement yielded a mean <sup>87</sup>Sr/<sup>86</sup>Sr of 0.708177 ± 9 (2<i>s</i>).</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"181-199"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1111/ggr.70018","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147563630","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"地球科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Combined Stable and Radiogenic Nd Isotope Characterisation of Sedimentary and Iron Formation Reference Materials by Double Spike MC-ICP-MS","authors":"Anne K.C. Kaufmann, Alex J. McCoy-West","doi":"10.1111/ggr.70020","DOIUrl":"https://doi.org/10.1111/ggr.70020","url":null,"abstract":"<p>This study presents combined stable (<sup>146</sup>Nd/<sup>144</sup>Nd, <sup>148</sup>Nd/<sup>144</sup>Nd) and radiogenic (<sup>143</sup>Nd/<sup>144</sup>Nd) Nd isotope ratios obtained by double spike (DS) MC-ICP-MS for twenty-five geological reference materials (RMs), focusing particularly on the initial characterisation of sedimentary, phosphate and iron formation (IF) RMs. Pure Nd solutions and previously characterised igneous RMs of basaltic to rhyolitic composition were utilised to validate the DS MC-ICP-MS method. The (combined) expanded uncertainty (95% c.i.) on JNdi-1 normalised δ<sup>146/144</sup>Nd measurement results was improved by <i>ca</i>. 4 ppm when data collection was increased from 50 to 100 cycles, which translates into a shift from ±0.016 to ±0.012‰. Intermediate measurement precision (over nearly 3 years) of δ<sup>146/144</sup>Nd determined from Nd solutions (<i>n</i> = 4) and igneous, sedimentary and iron formation RMs with multiple digestions (<i>n</i> = 17) is on average ±0.016‰ 2<i>s</i>. Our obtained results agree well with published stable δ<sup>146/144</sup>Nd and radiogenic <sup>143</sup>Nd/<sup>144</sup>Nd values for all igneous RMs analysed herein, attesting to the accuracy of the DS MC-ICP-MS approach. Sedimentary RMs are overall isotopically light with δ<sup>146/144</sup>Nd signatures between -0.057 and -0.006‰, overlapping closely with igneous RMs (-0.038 to +0.010‰ δ<sup>146</sup>Nd) and the bulk silicate Earth. The two phosphate RMs with δ<sup>146/144</sup>Nd of +0.040 and +0.090‰, are significantly heavier in comparison. In contrast, global IF RMs exhibit a large range in δ<sup>146/144</sup>Nd from -0.057 to +0.261‰ and include the heaviest (so far) recorded Nd stable isotope signature in a terrestrial geological material. Correlations of heavy δ<sup>146/144</sup>Nd with seawater proxies (e.g., Y/Ho) and light δ<sup>146/144</sup>Nd with tracers for continental contamination (e.g., Zr) suggest a strong potential for the application of stable Nd isotopes in sediments and IF for palaeo-reconstruction purposes.</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"221-240"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147566664","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"地球科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"A Novel Analytical Method Utilising an In-House PTFE Digester Using NH4HF2 and Dilute HCl for Total Dissolution of Pegmatite-Type Lithium Ores (α-Spodumene, Petalite and Lepidolite)","authors":"Venkata Balarama Krishna Mullapudi, Chandrasekaran Krishnan, Sukumar Anandkrishnan Arcot, Dash Kulamani","doi":"10.1111/ggr.70022","DOIUrl":"https://doi.org/10.1111/ggr.70022","url":null,"abstract":"<p>A novel and highly efficient hot plate digestion method was developed utilising an in-house PTFE digester using a mixture of ammonium bi-fluoride (NH<sub>4</sub>HF<sub>2</sub>) and dilute HCl (1, 1) for the total dissolution of pegmatite-type lithium ore samples (spodumene, petalite and lepidolite) for the quantitative determination of Li, Nb, Ti, Rb, Cs and Be and other co-existing elements (Fe, Al, Mn, Na, K, Ca and Mg) by inductively coupled plasma-atomic emission spectrometry. The proposed method was carried out in three analytical steps for total dissolution of Li ore matrix. The first step involved complete decomposition of the sample matrix (using a 1:4 sample to NH<sub>4</sub>HF<sub>2</sub> ratio), while evaporation of the silica matrix was carried out in the second step. The third step involved <i>aqua regia</i> treatment for conversion of insoluble fluorides to corresponding soluble forms to obtain particle-free and clear sample solutions. Critical analytical parameters related to hot plate digestion processes were optimised by a univariate approach to obtain quantitative recoveries (> 95%) for all of the selected analytes. The solid residues obtained at each step of sample preparation were characterised by XRD and EDS analysis. The method was validated through the analysis of three NBS reference materials (spodumene 181, petalite 182 and lepidolite) certified for Li mass fraction only. The other mass fractions listed are approximate/information values. The developed method was subsequently applied to multiple ore samples of different geological origins.</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"137-153"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147563778","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"地球科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Qishuai Huang, Yali Sun, Shouqian Zhao, Thomas C. Meisel
{"title":"A Simplified Method for the Determination of Re and PGE Mass Fractions, and Os Isotope Ratios in Ultramafic Rocks Combined with Se-SnCl2 Co-Precipitation","authors":"Qishuai Huang, Yali Sun, Shouqian Zhao, Thomas C. Meisel","doi":"10.1111/ggr.70030","DOIUrl":"https://doi.org/10.1111/ggr.70030","url":null,"abstract":"<p>A new measurement procedure was developed for determining Re, PGE mass fractions and Os isotope ratios in geological samples using ICP-MS and N-TIMS. Two sample decomposition techniques, including Carius tube digestion and NaOH-Na<sub>2</sub>O<sub>2</sub> fusion, were used to compare digestion efficiency. Osmium was separated from the sample matrix by distillation, while Re and other PGE were separated by Se-SnCl<sub>2</sub> co-precipitation and further purified using chelating resin. Rhenium and PGE mass fractions in WPR-1, WMG-1 and GPt-6 demonstrate good precision (RSD), with values under 5% for acid digestion and 10% for alkaline fusion. Relatively poor precision was obtained for the results of TDB-1, WGB-1, GPt-3, GPt-4 and CHR-Bkg, due to sample heterogeneity at a test portion size of 1 g. Furthermore, a more significant variance of PGE data was observed in DZ∑-1, DZ∑-2, GPt-5, GAN Pt-1 and HHH. From the point of view of sample digestion, refractory minerals (e.g., laurite, PGE alloys) can be completely decomposed by the NaOH-Na<sub>2</sub>O<sub>2</sub> fusion process, resulting in much higher PGE mass fraction yields and thereby making the heterogeneity of mantle rocks and chromitites visible. Consequently, the proposed method could significantly simplify the chemical procedure and yield more accurate data when measuring <sup>187</sup>Re-<sup>187</sup>Os-PGE in samples with very refractory minerals.</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"115-135"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147564637","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"地球科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Bin Qin, Yong Xu, Jie Li, Yao Sun, Ruohan Gao, Yujian Wang, Zhuyin Chu, Jingao Liu
{"title":"Enhanced High-Precision Os Isotope Measurements Testified by a New Os Reference Material – CUGB","authors":"Bin Qin, Yong Xu, Jie Li, Yao Sun, Ruohan Gao, Yujian Wang, Zhuyin Chu, Jingao Liu","doi":"10.1111/ggr.70032","DOIUrl":"https://doi.org/10.1111/ggr.70032","url":null,"abstract":"<p>The <sup>190</sup>Pt-<sup>186</sup>Os isotope system has unique potential in tracing planetary and geological processes. Elaborate efforts have been made to improve the accuracy and precision of <sup>190</sup>Pt-<sup>186</sup>Os isotope measurements over the past decades, which include investigating Pt-W-Re oxides and oxygen isotope interferences in Os isotope measurements and employing amplifiers with higher resistance to achieve higher signal voltages. However, several problems still limit the accuracy and precision of <sup>186</sup>Os/<sup>188</sup>Os ratios. We examine key factors that may affect Os isotope measurement results. Baseline drift during measurement contributes to deviations in isotopic ratios, resulting in a bias from the reference value. While it is debated whether W oxide interferences are present, our findings show that potential real W oxide interferences may exist, which can significantly disturb results. In addition, incorporating oxygen isotope monitoring before and after each measurement lowers the measurement uncertainty. Under the influence of W oxide interferences and baseline drift, significant residual correlations between <sup>186</sup>Os/<sup>188</sup>Os and <sup>184</sup>Os/<sup>188</sup>Os are observed. We advocate a residual correction approach to correct these residual correlations, which can effectively reduce the uncertainty of <sup>186</sup>Os/<sup>188</sup>Os ratios. Corrected isotope ratios for the same reference materials show slight discrepancies from published values, which may be ascribed to differences in Faraday cup efficiency. Hence, we recommend a standardising procedure to regulate Os isotope ratio results across reference materials, enabling direct comparison of data from different laboratories and different time periods. At least two reference materials should be used to monitor the consistency of instrument and the reliability of measurement results. Based on this enhanced method, we present high-precision Os isotope ratios for our newly prepared reference material CUGB: <sup>184</sup>Os/<sup>188</sup>Os = 0.0013036 ± 0.0000007, <sup>186</sup>Os/<sup>188</sup>Os = 0.1199711 ± 0.0000060, <sup>187</sup>Os/<sup>188</sup>Os = 0.1739252 ± 0.0000141, <sup>189</sup>Os/<sup>188</sup>Os = 1.219709 ± 0.000010, <sup>190</sup>Os/<sup>188</sup>Os = 1.983793 ± 0.000011 (2<i>s</i>).</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"201-220"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147569825","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"地球科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}