Journal of Analytical Atomic Spectrometry最新文献

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Analytical-performance enhancement of laser-induced breakdown spectroscopy using an annular laser beam
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-02-04 DOI: 10.1039/D4JA00445K
Bo Dai, Jingge Wang, Mianyun Ye, Yonghao Han and Hehe Li
{"title":"Analytical-performance enhancement of laser-induced breakdown spectroscopy using an annular laser beam","authors":"Bo Dai, Jingge Wang, Mianyun Ye, Yonghao Han and Hehe Li","doi":"10.1039/D4JA00445K","DOIUrl":"https://doi.org/10.1039/D4JA00445K","url":null,"abstract":"<p >In this paper, an axicon and a spherical lens were used to convert a circular Gaussian beam into an annular beam. Plasma was produced by a Q-switched Nd:YAG laser from an alloy steel sample with the annular beam. The spectral characteristics and analytical performance of trace elements using annular and Gaussian beam laser-induced breakdown spectroscopy (LIBS) were compared. The annular beam produced a larger stable plasma region with a flat spatial distribution. A 2–3 times enhancement in spectral stability was observed, while detection sensitivity increased by 2.1 times and the limit of detection (LoD) was reduced by 38.5%. The results of this study demonstrated that the plasma induced by an annular laser beam provides a new method to improve the analytical performance of LIBS.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 879-887"},"PeriodicalIF":3.1,"publicationDate":"2025-02-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553634","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
High intermediate precision rhenium isotopic measurements in geological samples
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-02-03 DOI: 10.1039/D4JA00267A
Jinhua Liu, Lian Zhou, Xiang Wang, Jianwei Li, Thomas J. Algeo and Xiaodong Deng
{"title":"High intermediate precision rhenium isotopic measurements in geological samples","authors":"Jinhua Liu, Lian Zhou, Xiang Wang, Jianwei Li, Thomas J. Algeo and Xiaodong Deng","doi":"10.1039/D4JA00267A","DOIUrl":"https://doi.org/10.1039/D4JA00267A","url":null,"abstract":"<p >Stable rhenium (Re) isotopes are important tracers for geological processes related to melting and differentiation of planetary interiors, ore mineralization and paleoenvironmental redox conditions. However, methods for the precise determination of Re isotope ratios have received limited investigation to date due to the extremely low Re mass fractions of most geological materials. In this study, we present a new protocol for increased intermediate precision in the measurement results of Re isotope ratios in geological materials using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). Preconcentration of Re is an essential first step, involving digestion of 1–2 g of sample powder by concentrated NH<small><sub>3</sub></small> solution, followed by coprecipitation of matrix ions other than Re, Mn and Mo. Subsequent purification and extraction of Re from the residual matrix was performed on TEVA resin. This approach provided an efficient purification with a low blank (&lt;0.2 pg) and high yield of Re (93.2 ± 2.4%, 2s, <em>n</em> = 5) for reference materials BCR-2 and TDB-1. Instrumental mass bias was monitored and corrected through a combination of standard-sample bracketing (SSB) and internal normalization of Ir as a calibration standard. This approach yielded about a two-fold improvement in the intermediate precision relative to SSB alone. In addition, a further two-fold improvement in precision was obtained by the use of a membrane desolvation system which can increase the intensity of Re isotopic signals by an order of magnitude. This protocol improved the intermediate precision of measured δ<small><sup>187</sup></small>Re<small><sub>SRM3143</sub></small> for a 1 ng g<small><sup>−1</sup></small> Re analyte solution to 0.048‰. The δ<small><sup>187</sup></small>Re<small><sub>SRM3143</sub></small> of USGS basalt reference materials were measured using this measurement procedure, yielding δ<small><sup>187</sup></small>Re<small><sub>SRM3143</sub></small> of −0.31 ± 0.04‰ (2s, <em>n</em> = 6), −0.33 ± 0.05‰ (2s, <em>n</em> = 3), −0.35 ± 0.05‰ (2s, <em>n</em> = 3) for BCR-2, BHVO-2, BIR-1a, respectively, in agreement with values obtained in previous studies. Other reference materials were analyzed, yielding δ<small><sup>187</sup></small>Re<small><sub>SRM3143</sub></small> of −0.35 ± 0.05‰ (2s, <em>n</em> = 2), −0.36 ± 0.04‰ (2s, <em>n</em> = 3) and −0.31 ± 0.03‰ (2s, <em>n</em> = 3) for diabase (TDB-1), komatikic basalt (OKUM), and andesite (AGV-2), respectively. The developed procedure was successfully applied to measurement of samples with low Re mass fractions, extending the range of geological materials for which Re isotopic values can be determined.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 868-878"},"PeriodicalIF":3.1,"publicationDate":"2025-02-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553633","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
High-precision measurement of Eu isotopes enabled by Nd internal normalization†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-01-31 DOI: 10.1039/D4JA00420E
Hao Wu, Jiang-Hao Bai, Xi-Rong Liang, Xi-Bin Lu, Yong-Ying Li, Yi-Nan Deng, Ye Zhao and Gang-Jian Wei
{"title":"High-precision measurement of Eu isotopes enabled by Nd internal normalization†","authors":"Hao Wu, Jiang-Hao Bai, Xi-Rong Liang, Xi-Bin Lu, Yong-Ying Li, Yi-Nan Deng, Ye Zhao and Gang-Jian Wei","doi":"10.1039/D4JA00420E","DOIUrl":"https://doi.org/10.1039/D4JA00420E","url":null,"abstract":"<p >Eu isotopes are recognized as potential indicators for understanding continental crust evolution, ocean circulation, and rare earth element mineralization. However, methods for achieving high-precision Eu isotopic analysis remain underdeveloped. This study pioneers a comprehensive application of the Nd internal normalization technique in Eu isotope analysis, facilitating high-precision measurements of Eu isotope compositions in geological reference materials. It assesses the correction effectiveness of various Nd isotopic ratios (<small><sup>146</sup></small>Nd/<small><sup>144</sup></small>Nd, <small><sup>146</sup></small>Nd/<small><sup>145</sup></small>Nd, and <small><sup>150</sup></small>Nd/<small><sup>148</sup></small>Nd) on Eu isotopic measurements and investigates the fractionation behavior of Eu–Nd in mass spectrometers. These findings demonstrate that the <small><sup>146</sup></small>Nd/<small><sup>145</sup></small>Nd ratio significantly enhances the stability and reproducibility of Eu isotope measurements, achieving a long-term external precision of <em>δ</em><small><sup>153/151</sup></small>Eu at 0.04‰ (2SD). Additionally, the study reveals that the fractionation behavior of Eu–Nd in mass spectrometry theoretically aligns more closely with the power law rather than the traditionally assumed exponential law. However, in practical tests, no significant difference in results is observed whether employing the power law or the exponential law. These insights advance Eu isotope geochemistry and provide a valuable reference for the high-precision analysis of other rare earth elements.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 860-867"},"PeriodicalIF":3.1,"publicationDate":"2025-01-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553632","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Second version of the open-source software GSA for gamma-ray spectrum analysis
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-01-29 DOI: 10.1039/D4JA00398E
Lahcen El Amri, Hamid Amsil, Omar El Bounagui, Abdelouahed Chetaine, Brahim Elmokhtari, Hamid Bounouira and Abdessamad Didi
{"title":"Second version of the open-source software GSA for gamma-ray spectrum analysis","authors":"Lahcen El Amri, Hamid Amsil, Omar El Bounagui, Abdelouahed Chetaine, Brahim Elmokhtari, Hamid Bounouira and Abdessamad Didi","doi":"10.1039/D4JA00398E","DOIUrl":"https://doi.org/10.1039/D4JA00398E","url":null,"abstract":"<p >The collaboration among the PRESN team, LaMCScI laboratory and CNESTEN center made it possible to implement the first version of the GSA software. Its first version is already available to the public; it is not only free but also an open source, demonstrating the developers' commitment to promoting the open sharing of scientific knowledge. This first version is characterized by its flexibility and non-commerciality, and it is available without any conditions on the following website: https://www.github.com/LAHCEN-EL-AMRI/Gamma-Spectra-Analysis, allowing users to add personal options, making it a particularly adaptable tool to the different requirements of scientific research. This article deals with the second version of GSA, which focuses on a core and complementary feature: the calculation of isotope activity. In order to accomplish this goal, instead of implementing a single efficiency formula, as is often the case in most software, four formulas were integrated. The users can therefore select the one they want to implement. To ensure the accuracy and reliability of this new feature, a validation was performed on GSA. The results obtained with GSA v2 were carefully studied by comparing them to those obtained with the renowned Genie 2000 software. Owing to this comparison step, it was possible to verify and confirm the accuracy of the results of GSA version 2. This second version of GSA is available as a free and open source software on the following site: https://www.github.com/LAHCEN-EL-AMRI/GSA-v2/tree/master.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 738-746"},"PeriodicalIF":3.1,"publicationDate":"2025-01-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553602","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A ray tracing survey of asymmetric operation of the X-ray Rowland circle using spherically bent crystal analyzers
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-01-28 DOI: 10.1039/D4JA00339J
Yeu Chen, Anthony J. Gironda, Yaxin Shen, André D. Taylor and Gerald T. Seidler
{"title":"A ray tracing survey of asymmetric operation of the X-ray Rowland circle using spherically bent crystal analyzers","authors":"Yeu Chen, Anthony J. Gironda, Yaxin Shen, André D. Taylor and Gerald T. Seidler","doi":"10.1039/D4JA00339J","DOIUrl":"https://doi.org/10.1039/D4JA00339J","url":null,"abstract":"<p >The Spherically Bent Crystal Analyzer (SBCA) is a widely adopted hard X-ray optic, renowned for its good energy resolution and large collection solid angle. It is frequently employed in synchrotron-based techniques like Resonant Inelastic X-ray Scattering (RIXS) and X-ray Emission Spectroscopy (XES), as well as in the rebirth of laboratory-based X-ray Absorption Fine Structure (XAFS) and XES, and its predominant use has been in ‘symmetric’ operation on the Rowland circle. The recent study of Gironda <em>et al.</em> (<em>J. Anal. At. Spectrom.</em>, 2024, <strong>39</strong>, 1375) emphasizes the benefits of ‘asymmetric’ SBCA operation, demonstrating the use of multiple crystal reflections from a single SBCA to broaden its accessible energy range. Furthermore, Gironda <em>et al.</em> demonstrate that asymmetric operation frequently mitigates energy broadening intrinsic to Johann optics and propose that under a specific Rowland circle configuration, designated here the Johann Normal Alignment (JNA), such broadening is eradicated altogether. We report extensive ray tracing simulations and new experimental results to scrutinize the impact of asymmetric configurations on energy broadening and detector plane defocusing. We find that the performance of asymmetric SBCA operation generally exceeds its symmetric counterpart in energy resolution when no analyzer masking is used and, with strategic detector placement, the decrease in detection efficiency due to defocusing can be minimized. Spectroscopic imaging is adversely affected by the detector plane blurring, but rejection of scattering from special environment windows in X-ray Raman imaging is still feasible and high imaging quality can be recovered by Johann-like analyzer edge masking. These results help inform future, more common implementation of asymmetric reflections with SBCA in several synchrotron applications and in laboratory-based XAFS and XES.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 836-847"},"PeriodicalIF":3.1,"publicationDate":"2025-01-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553631","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
: a selection tool for asymmetric reflections of spherically bent crystal analyzers for high resolution X-ray spectroscopy
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-01-28 DOI: 10.1039/D4JA00340C
Jared E. Abramson, Yeu Chen and Gerald T. Seidler
{"title":": a selection tool for asymmetric reflections of spherically bent crystal analyzers for high resolution X-ray spectroscopy","authors":"Jared E. Abramson, Yeu Chen and Gerald T. Seidler","doi":"10.1039/D4JA00340C","DOIUrl":"https://doi.org/10.1039/D4JA00340C","url":null,"abstract":"<p >High resolution, hard X-ray spectroscopy at synchrotron X-ray light sources commonly uses spherically bent crystal analyzers (SBCAs) formed by shaping a single crystal wafer to a spherical backing. These Rowland circle optics are almost always used in ‘symmetric’ (or nearly symmetric) configurations wherein the reciprocal lattice vector used for energy selectivity <em>via</em> diffraction is coincident with the normal vector to the curved wafer surface. However, Gironda, <em>et al.</em>, <em>J. Anal. At. Spectrom.</em>, 2024, <strong>39</strong>, 1375–1387 recently proposed that asymmetric operation of SBCAs, wherein the reciprocal lattice vector is no longer normal to the wafer surface, has significant operational benefits and has been an underutilized opportunity. First, those authors find improved energy resolution through decreased Johann error, or equivalently find increased solid angle at a chosen experimental tolerance for energy broadening. Second, they find productive, high-resolution use of a large number of reciprocal lattice vectors from a single SBCA, thus enabling operation over a wide energy range without need to exchange SBCA upon making large changes in desired photon energy. These observations hold the potential to improve performance, increase flexibility and decrease cost for both laboratory and synchrotron applications. Given these motivations, we report an open-source software package, <img>, that enables exploration of the complex space of analyzer wafer choice, experimental energy range or ranges, and desired suppression of Johann error. This package can guide both the design and the day-to-day operations of Rowland spectrometers enabled for asymmetric use.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 817-824"},"PeriodicalIF":3.1,"publicationDate":"2025-01-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553615","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Novel calibration approach for particle size analysis of microplastics by laser ablation single particle-ICP-MS†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-01-27 DOI: 10.1039/D4JA00351A
Lukas Brunnbauer, Laura Kronlachner, Elias Foisner and Andreas Limbeck
{"title":"Novel calibration approach for particle size analysis of microplastics by laser ablation single particle-ICP-MS†","authors":"Lukas Brunnbauer, Laura Kronlachner, Elias Foisner and Andreas Limbeck","doi":"10.1039/D4JA00351A","DOIUrl":"10.1039/D4JA00351A","url":null,"abstract":"<p >The need to analyze and characterize microplastics (MPs) is ever-increasing to monitor and understand their environmental impact. In this work, a developed calibration approach that utilizes an in-house-created polystyrene (PS) thin film for the sizing of MPs is presented, circumventing the need for certified particulate standard material. LA was used for sampling and transporting intact MPs of different sizes and polymer types to the ICP-MS. For the calibration, defined amounts of carbon were introduced into the ICP-MS by quantitatively ablating a polymer thin film with different laser spot sizes. With this approach, a LOD of 4.85 pg carbon was obtained, which translates to a size of 2.12 μm for spheric PS particles. The calibration using PS thin film was successfully applied to sampled PS MPs and allowed accurate sizing of 2 μm, 3 μm, and 4.5 μm particles. When using the PS calibration for determining polyvinyl chloride (PVC) and poly(methyl methacrylate) (PMMA) particle sizes, a good estimate of the size could be achieved despite the different compositions of the polymers. This indicates the universal applicability of the presented approach. The investigation of the transport efficiency showed that it is mainly influenced by particle size, and factors such as the polymer type and length of the transport line and carrier gas. Under optimum conditions, up to 95% of the sampled particles were detected.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 753-761"},"PeriodicalIF":3.1,"publicationDate":"2025-01-27","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC11783204/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143078014","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
An emergency radiobioassay method for Pu, Am and Cm isotopes in urine samples using tandem quadrupole ICP-MS†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-01-24 DOI: 10.1039/D4JA00279B
Yang Wu, Xiongxin Dai, Maoyi Luo, Hongmei Guo, Ni Yuan, Yonggang Yang, Jingjing He and Yuanyuan Guo
{"title":"An emergency radiobioassay method for Pu, Am and Cm isotopes in urine samples using tandem quadrupole ICP-MS†","authors":"Yang Wu, Xiongxin Dai, Maoyi Luo, Hongmei Guo, Ni Yuan, Yonggang Yang, Jingjing He and Yuanyuan Guo","doi":"10.1039/D4JA00279B","DOIUrl":"https://doi.org/10.1039/D4JA00279B","url":null,"abstract":"<p >The rapid bioassay method for measuring actinides in human urine samples is the most appropriate way for the assessment of internal exposure doses during radiological and nuclear emergencies. A rapid simultaneous analysis method for <small><sup>239</sup></small>Pu, <small><sup>240</sup></small>Pu, <small><sup>241</sup></small>Am and <small><sup>244</sup></small>Cm in 100 mL urine samples was established by using tandem quadrupole ICP-MS (ICP-MS/MS), combined with a hydrous titanium oxide (HTiO) co-precipitation step and a tandem small size resin column (TEVA + DGA) purification step for shortening the sample processing time. The ICP-MS/MS measurements of Pu isotopes, <small><sup>241</sup></small>Am and <small><sup>244</sup></small>Cm were optimized in Q3 only mode and MS/MS mode, respectively, and the interferents from the urine matrix were appropriately suppressed by applying Axial Field Voltage (AFT). The measurement sensitivities of Pu and Am isotopes were improved by employing NH<small><sub>3</sub></small> or He as collision/reaction cell gases, and an interesting finding is that pure NH<small><sub>3</sub></small> significantly improved the Pu measurement sensitivity. The detection limits for the method were estimated to be 1.12 fg (2.57 × 10<small><sup>−3</sup></small> mBq) for <small><sup>239</sup></small>Pu, 0.97 fg (8.14 × 10<small><sup>−3</sup></small> mBq) for <small><sup>240</sup></small>Pu, 1.46 fg (0.19 mBq) for <small><sup>241</sup></small>Am and 0.74 fg (2.16 mBq) for <small><sup>244</sup></small>Cm in 100 mL urine, meeting the sensitivity requirements for emergency urine bioassay methods.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 2","pages":" 513-519"},"PeriodicalIF":3.1,"publicationDate":"2025-01-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143184588","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Determination of Ru and Os with enhanced sensitivity and Rh, Pd, Pt and Ir at sub ng g−1 levels in geological samples by ICP-MS†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-01-23 DOI: 10.1039/D4JA00383G
Qishuai Huang, Yali Sun and Shouqian Zhao
{"title":"Determination of Ru and Os with enhanced sensitivity and Rh, Pd, Pt and Ir at sub ng g−1 levels in geological samples by ICP-MS†","authors":"Qishuai Huang, Yali Sun and Shouqian Zhao","doi":"10.1039/D4JA00383G","DOIUrl":"https://doi.org/10.1039/D4JA00383G","url":null,"abstract":"<p >The precise and accurate determination of platinum group elements (PGEs) at low abundance levels remains challenging. Here, an improved method was developed for the determination of ruthenium (Ru) and osmium (Os) with high sensitivity, as well as other platinum group elements (Ir, Rh, Pt and Pd) in geological samples, by isotope dilution-inductively coupled plasma-mass spectrometry (ID-ICP-MS). Following the decomposition of the samples with NaOH–Na<small><sub>2</sub></small>O<small><sub>2</sub></small> fusion and subsequent acidification with HNO<small><sub>3</sub></small>, Ru and Os were distilled in the form of volatile RuO<small><sub>4</sub></small> and OsO<small><sub>4</sub></small>, respectively, using an oxidant, K<small><sub>2</sub></small>S<small><sub>2</sub></small>O<small><sub>8</sub></small>. The RuO<small><sub>4</sub></small> and OsO<small><sub>4</sub></small> were simultaneously absorbed with H<small><sub>2</sub></small>O with yields of 84.3 and 92.9%, respectively, resulting in a higher sensitivity of 60-fold for Ru and 11-fold for Os relative to their low valences by ICP-MS analysis. After distillation, HF was added to the remaining sample to remove silica, and dissolved in 3 mol l<small><sup>−1</sup></small> HCl. Then Pd, Rh, Ir and Pt were co-precipitated with tellurium (Te), dissolved in 0.24 mol l<small><sup>−1</sup></small> HCl, and analyzed directly by ICP-MS. The entire procedural blank of this method was evaluated and found to range from 11 pg for Rh to 300 pg for Pd. The proposed method was validated with nine geological reference materials, including GBW07289 (GPt-2), TDB-1, and WGB-1, with very low PGE contents. Given the sample heterogeneity and digestion efficiency of different methods, our results are comparable to those previously reported. The newly developed method can be applied to the PGE analysis of low-abundance samples (<em>e.g.</em>, basaltic rocks and sediments).</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 795-807"},"PeriodicalIF":3.1,"publicationDate":"2025-01-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553608","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Spatio-temporal evolution of laser ablation W plasma under low-pressure Ar gas and Ar plasma ambients†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2025-01-22 DOI: 10.1039/D4JA00326H
Boliang Men, Cong Li, Qi He, Hongmin Qu, Shiming Liu, Longfei Li, Huace Wu, Zhonglin He, Jielin Shi, Ding Wu, Ran Hai, Xingwei Wu and Hongbin Ding
{"title":"Spatio-temporal evolution of laser ablation W plasma under low-pressure Ar gas and Ar plasma ambients†","authors":"Boliang Men, Cong Li, Qi He, Hongmin Qu, Shiming Liu, Longfei Li, Huace Wu, Zhonglin He, Jielin Shi, Ding Wu, Ran Hai, Xingwei Wu and Hongbin Ding","doi":"10.1039/D4JA00326H","DOIUrl":"https://doi.org/10.1039/D4JA00326H","url":null,"abstract":"<p >Understanding the spatio-temporal evolution of laser ablation plasma under low-pressure ambients is a crucial area of study in the field of laser-induced breakdown spectroscopy (LIBS). In this work, LIBS combined with plasma imaging was employed to diagnose the spatio-temporal evolution of laser ablation W plasma under Ar gas ambient and continuous Ar plasma ambient with low-pressure conditions. Results revealed that laser ablation W plasma under Ar plasma ambient exhibited high radiative recombination loss and radiative thermal bremsstrahlung loss in the early stages of spatio-temporal evolution. This led to an increased continuous radiation background and W II signal intensity. It was found that the electron temperature initially exhibited a brief decline, followed by an increase, and then decreased gradually. This resulted in a temporary temperature drop caused by the inertia of plasma expansion, which was quickly compensated by the recompression of the shockwave layer. Plasma imaging results revealed plume splitting, plume sharpening, and plume turbulence in laser ablation W plasma under Ar gas ambient. The front position and area of the plasma plume under Ar gas ambient and Ar plasma ambient were compared. In the later stages of temporal evolution, the plume area of the plasma could be described using a drag model. Thus, this study provides new insights into the physical mechanisms of laser ablation W plasma under different background ambients, which is important for the real-time diagnostics of wall materials by LIBS during tokamak discharges.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 762-774"},"PeriodicalIF":3.1,"publicationDate":"2025-01-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ja/d4ja00326h?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553604","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
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