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Overcoming Polyatomic Interferences in Sulfur Isotope Measurement Using MC-ICP-MS MC-ICP-MS测定硫同位素中多原子干扰的克服
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2025-10-06 DOI: 10.1111/ggr.70019
Yang Yu, Patrick Sugden, Robert C. J. Steele, Mohammad Nuruzzama, Andrea Burke
{"title":"Overcoming Polyatomic Interferences in Sulfur Isotope Measurement Using MC-ICP-MS","authors":"Yang Yu,&nbsp;Patrick Sugden,&nbsp;Robert C. J. Steele,&nbsp;Mohammad Nuruzzama,&nbsp;Andrea Burke","doi":"10.1111/ggr.70019","DOIUrl":"https://doi.org/10.1111/ggr.70019","url":null,"abstract":"<p>Accurate and precise sulfur isotope (<sup>32</sup>S, <sup>33</sup>S and <sup>34</sup>S) measurement using multi-collector inductively coupled plasma-mass spectrometry (MC-ICP-MS) is often challenged by the formation of polyatomic ions, leading to isobaric interferences that overlap with sulfur isotopes of interest. Traditionally, high-resolution mode is required to resolve sulfur isotopes from these interferences, but achieving high resolving power typically comes with a substantial reduction in analyte sensitivity. In this study, we address the challenge of spectral interferences by adjusting plasma operating conditions (quantified using the Normalised Argon Index, NAI), thereby significantly mitigating the formation of polyatomic ions. As a result, δ<sup>34</sup>S and δ<sup>33</sup>S can be accurately measured at the peak centre in low-resolution mode. The use of low-resolution mode leads to an approximately threefold increase in sensitivity compared with conventional high-resolution measurement. This sensitivity improvement is particularly advantageous for analysing samples with low sulfur mass fractions, or where sample material is limited such as ice cores. In addition, the optimised plasma condition provides a predictable pattern of instrumental mass fractionation, which is essential for accurate mass bias correction using the standard-sample bracketing technique. Overall, our new approach simplifies the analytical workflow and minimises instrument wear, offering a sensitive, user-friendly, and high-throughput method for sulfur isotope measurement with MC-ICP-MS.</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"85-95"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1111/ggr.70019","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147563676","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}
引用次数: 0
GGR Handbook of Rock and Mineral Analysis Chapter 2 (Part 2) Analysis of Geological Materials – 2: Pre-Concentration and Separation Procedures 岩石和矿物分析GGR手册第2章(第2部分)地质材料分析- 2:预富集和分离程序
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2026-02-22 DOI: 10.1111/ggr.70038
Philip Robinson
{"title":"GGR Handbook of Rock and Mineral Analysis Chapter 2 (Part 2) Analysis of Geological Materials – 2: Pre-Concentration and Separation Procedures","authors":"Philip Robinson","doi":"10.1111/ggr.70038","DOIUrl":"https://doi.org/10.1111/ggr.70038","url":null,"abstract":"<p>This chapter (Analysis of Geological Materials – 2: Pre-Concentration and Separation Procedures) is a contribution to the <i>Geostandards and Geoanalytical Research Handbook of Rock and Mineral Analysis</i> – an online textbook that is a fully revised and updated edition of <i>A Handbook of Silicate Rock Analysis</i> (P. J. Potts, 1987, Blackie, Glasgow).</p><p>In Chapter 2, Part 2 (from Section 1 of the handbook dealing with fundamentals of measurement and instrument design) the principles and procedures of ion exchange chromatographic techniques and processes are first examined followed by a review of their application to isotope measurement by TIMS and MC-ICP-MS for radiogenic and stable isotope systems. Determination of platinum-group and rare earth elements by ICP-MS is also covered. Following this, liquid-liquid (solvent) extraction and extraction chromatography are examined, including a review of EXC resins in the analysis of silicate materials. Part 2 Chapter 2 concludes with a treatment of coprecipitation and vapour generation (for hydrides, mercury and osmium).</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"5-64"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147567537","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}
引用次数: 0
Exploration of a Combined LIBS and LA-ICP-MS Approach for Apatite Characterisation 结合LIBS和LA-ICP-MS方法用于磷灰石表征的探索
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2025-10-15 DOI: 10.1111/ggr.70021
C. Derrick Quarles Jr., Benjamin T. Manard, N. Alex Zirakparvar, Joe Petrus, Bence Paul, David Douglas, Andy Gleadow, Barry Kohn, Samuel Boone, Ling Chung, Malcolm McMillan, Gokce K. Ustunisik, Francis M. McCubbin
{"title":"Exploration of a Combined LIBS and LA-ICP-MS Approach for Apatite Characterisation","authors":"C. Derrick Quarles Jr.,&nbsp;Benjamin T. Manard,&nbsp;N. Alex Zirakparvar,&nbsp;Joe Petrus,&nbsp;Bence Paul,&nbsp;David Douglas,&nbsp;Andy Gleadow,&nbsp;Barry Kohn,&nbsp;Samuel Boone,&nbsp;Ling Chung,&nbsp;Malcolm McMillan,&nbsp;Gokce K. Ustunisik,&nbsp;Francis M. McCubbin","doi":"10.1111/ggr.70021","DOIUrl":"https://doi.org/10.1111/ggr.70021","url":null,"abstract":"<p>A combined laser-induced breakdown spectroscopy (LIBS) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) method is demonstrated for comprehensive apatite analysis. These measurements provide elemental imaging that can be used as a screening technique for chemical selection of grains for subsequent analysis (e.g., U-Pb geochronology) or can be used to understand elemental distributions within a single grain that would have direct textural-chemical implications (e.g., zoning patterns). Adding LIBS as a simultaneous measurement, to LA-ICP-MS U-Pb geochronology, allowed for the direct determination of F (H and O show promise for future applications) in addition to major and trace elements of interest. The quantitative measurements were validated against a series of apatites with known values and used to characterise a wide range of samples. Fluorine detection limits were determined to be as low as 70 μg g<sup>-1</sup> F (broadband CMOS detector) and 4.2 μg g<sup>-1</sup> F (ICCD detector). U-Pb age dating was simultaneously collected by LA-ICP-MS with the quantitative elemental data from LIBS, providing a comprehensive method for geochronology.</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"67-83"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147565931","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}
引用次数: 0
Six Ca-Mg-Fe Carbonate Reference Materials for In Situ Measurement of Oxygen and Carbon Isotope Ratios 六种Ca-Mg-Fe碳酸盐基准物质原位测量氧和碳同位素比值
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2025-12-22 DOI: 10.1111/ggr.70031
Maria Rosa Scicchitano, Chris Harris, Julie Luyt, Andreas Pack, Tommaso di Rocco, Torsten Vennemann, Franziska D.H. Wilke, Anja M. Schleicher, Johannes Glodny, Kimberly T. Tait, Simon Philippo
{"title":"Six Ca-Mg-Fe Carbonate Reference Materials for In Situ Measurement of Oxygen and Carbon Isotope Ratios","authors":"Maria Rosa Scicchitano,&nbsp;Chris Harris,&nbsp;Julie Luyt,&nbsp;Andreas Pack,&nbsp;Tommaso di Rocco,&nbsp;Torsten Vennemann,&nbsp;Franziska D.H. Wilke,&nbsp;Anja M. Schleicher,&nbsp;Johannes Glodny,&nbsp;Kimberly T. Tait,&nbsp;Simon Philippo","doi":"10.1111/ggr.70031","DOIUrl":"https://doi.org/10.1111/ggr.70031","url":null,"abstract":"<p>Six potential Ca-Mg-Fe carbonate reference materials were assessed for oxygen and carbon isotope ratios homogeneity by secondary ion mass spectrometry (SIMS). This new suite includes three dolomites (Tucka-22, M9548.2, Eugui) and one ankerite (WPA-177-2) with Fe# ranging from 0.0004 to 0.3429, one magnesite (M21350.2) with Fe# = 0.0099 and one siderite (Vizille-1) with Fe# = 0.6152. The six materials were split into 128 to 2048 metrologically identical aliquots, each containing roughly 100 mg of sample. In this study, we report a detailed characterisation of the split materials for their major and minor chemical element compositions using electron probe microanalysis (EPMA), mineralogical compositions using X-ray diffraction (XRD), oxygen and carbon isotope values determined in three independent gas-source isotope ratio mass spectrometry (GS-IRMS) laboratories. The repeatability of our SIMS measurements varied from ± 0.15 to ± 0.31‰ (1 standard deviation, 1<i>s</i>) for δ<sup>18</sup>O and from ± 0.29 to ± 0.71‰ (1<i>s</i>) for δ<sup>13</sup>C. These six carbonate samples span a wide range in oxygen (δ<sup>18</sup>O<sub>VSMOW</sub> from 12.98 ± 0.09‰ to 26.92 ± 0.11‰, 1 standard error of the mean, 1SE) and carbon (δ<sup>13</sup>C<sub>VPDB</sub> from -11.74 ± 0.20‰ to 2.43 ± 0.06‰, 1SE) isotope ratios. Significant SIMS compositional matrix effects of +6.7‰ (for δ<sup>18</sup>O) and -3.2‰ (for δ<sup>13</sup>C) were observed along the dolomite-ankerite solid-solution series in the compositional range Fe# = 0.0004 to 0.3429. Similarly, large compositional matrix effects of +4.2‰ and -9.5‰ were observed for δ<sup>18</sup>O and δ<sup>13</sup>C, respectively, along the magnesite-siderite solid-solution series. This confirms the need for multiple matrix-matched reference materials spanning across a wide range in chemical compositions in order to get accurate SIMS isotope ratios in carbonate minerals that form solid-solutions. The Ca-Mg-Fe carbonate reference materials described in this study were produced in sufficient amounts to be available to the global geochemical community for years to come.</p>","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":"155-179"},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1111/ggr.70031","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147567522","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}
引用次数: 0
A Laser-Laser Method for In Situ C and O Isotope Measurements in Carbonate Materials 碳酸盐材料中C、O同位素原位测量的激光-激光方法
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2025-10-20 DOI: 10.1111/ggr.70023
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,&nbsp;Olivier Musset,&nbsp;Pierre Sansjofre,&nbsp;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}
引用次数: 0
RioM-1: A New Calcite Reference Material for U-Pb LA-ICP-MS Geochronology RioM-1:一种新的U-Pb LA-ICP-MS年代学方解石基准物质
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2025-10-06 DOI: 10.1111/ggr.70018
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,&nbsp;Cristiano Lana,&nbsp;Ricardo Scholz,&nbsp;Ian Buick,&nbsp;Sandra Kamo,&nbsp;Nick M.W. Roberts,&nbsp;Axel Gerdes,&nbsp;Michael Wiedenbeck,&nbsp;Blair Schoene,&nbsp;Francisco E. Apen,&nbsp;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}
引用次数: 0
IAG Membership Information IAG会员信息
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 DOI: 10.1111/ggr.70042
{"title":"IAG Membership Information","authors":"","doi":"10.1111/ggr.70042","DOIUrl":"https://doi.org/10.1111/ggr.70042","url":null,"abstract":"","PeriodicalId":12631,"journal":{"name":"Geostandards and Geoanalytical Research","volume":"50 1","pages":""},"PeriodicalIF":3.4,"publicationDate":"2026-03-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://onlinelibrary.wiley.com/doi/epdf/10.1111/ggr.70042","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147564306","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}
引用次数: 0
Combined Stable and Radiogenic Nd Isotope Characterisation of Sedimentary and Iron Formation Reference Materials by Double Spike MC-ICP-MS 用双尖峰MC-ICP-MS联合表征沉积和铁组参考物质的稳定和放射成因Nd同位素
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2025-10-17 DOI: 10.1111/ggr.70020
Anne K.C. Kaufmann, Alex J. McCoy-West
{"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,&nbsp;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}
引用次数: 0
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) 利用室内聚四氟乙烯蒸馏池用NH4HF2和稀HCl分析伟晶岩型锂矿石(α-锂辉石、Petalite和Lepidolite)总溶解的新方法
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2025-11-06 DOI: 10.1111/ggr.70022
Venkata Balarama Krishna Mullapudi, Chandrasekaran Krishnan, Sukumar Anandkrishnan Arcot, Dash Kulamani
{"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,&nbsp;Chandrasekaran Krishnan,&nbsp;Sukumar Anandkrishnan Arcot,&nbsp;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 (&gt; 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}
引用次数: 0
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 硒- sncl2共沉淀法测定超镁铁质岩石中稀土、稀土质量分数及Os同位素比值的简化方法
IF 3.4 2区 地球科学
Geostandards and Geoanalytical Research Pub Date : 2026-03-09 Epub Date: 2025-12-10 DOI: 10.1111/ggr.70030
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,&nbsp;Yali Sun,&nbsp;Shouqian Zhao,&nbsp;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}
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