Journal of Analytical Atomic Spectrometry最新文献

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Needle tip-enhanced laser-induced breakdown spectroscopy for nebulized aqueous solution analysis
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-28 DOI: 10.1039/D4JA00381K
Yiwei Xiong, Weihua Huang, Jihua Yang, Junfei Nie and Lianbo Guo
{"title":"Needle tip-enhanced laser-induced breakdown spectroscopy for nebulized aqueous solution analysis","authors":"Yiwei Xiong, Weihua Huang, Jihua Yang, Junfei Nie and Lianbo Guo","doi":"10.1039/D4JA00381K","DOIUrl":"https://doi.org/10.1039/D4JA00381K","url":null,"abstract":"<p >In the detection of aqueous solutions through Laser-induced Breakdown Spectroscopy (LIBS), the implementation of nebulization is instrumental in mitigating liquid splashing and preventing plasma quenching. However, gas dilution during nebulization would greatly undermine the detection limits. This study proposes a needle tip-enhancement method that excites the metal tip to produce a high-temperature plasma before ablating the nebulized solution. The optimization results for needle tip materials reveal that among the seven materials Zn, Ag, Cu, Mo, Ni, Ti, and W, Zn, Ag, and Cu exhibit minimal interference with the target elements Mn and Cr, with Zn showing the highest spectral enhancement effect. The average Pearson correlation between the enhancement effect and the melting and boiling points of the materials exceeds 0.90. Further optimization of the needle tip diameter revealed that a diameter that is too thin can cause material deformation, while a diameter that is too thick would lead to liquid adsorption and deep pit formation. Therefore, a diameter of 0.5 mm was chosen as the optimal under experimental conditions. Additionally, the optimization results of the relative position between the aerosol plume and the needle tip indicate that the best enhancement effect occurs when the aerosol plume passes through the core of the plasma. Using a needle tip-enhancement method, we detected Cu, Mn, and Cr in water samples, applying machine learning for quantitative analysis. The Gaussian Process Regression (GPR) model yielded the highest accuracy at 0.99. The spectral intensities of Cu, Mn, and Cr were enhanced by 7.20, 8.57, and 11.49 times, respectively. Detection limits of Cu, Mn, and Cr with needle tip-enhancement reached 42.80 mg L<small><sup>−1</sup></small>, 51.25 mg L<small><sup>−1</sup></small>, and 58.40 mg L<small><sup>−1</sup></small>. This study has the potential to facilitate real-time online monitoring of water solutions.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 2","pages":" 503-512"},"PeriodicalIF":3.1,"publicationDate":"2024-12-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143184587","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 dual-stage purge–trap protocol to separate species-specific mercury from marine biota for precise isotopic analysis†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-26 DOI: 10.1039/D4JA00341A
Songjing Li, Ruoyu Sun, Xiaowei Chen, Wei Zhang, Mei Meng, Yi Liu, Wang Zheng and Jiubin Chen
{"title":"A dual-stage purge–trap protocol to separate species-specific mercury from marine biota for precise isotopic analysis†","authors":"Songjing Li, Ruoyu Sun, Xiaowei Chen, Wei Zhang, Mei Meng, Yi Liu, Wang Zheng and Jiubin Chen","doi":"10.1039/D4JA00341A","DOIUrl":"https://doi.org/10.1039/D4JA00341A","url":null,"abstract":"<p >The application of mercury (Hg) isotopes in marine food webs has greatly advanced our understanding of the sources and transformation of marine Hg. However, previous studies mainly focused on the total Hg (THg) isotope composition. While species-specific Hg isotope compositions are more informative, the separation of individual species remains a technological hurdle. Here, we optimized a dual-stage purge–trap protocol to separate inorganic Hg (IHg) and methylmercury (MeHg) from marine biota to facilitate high-precision isotopic analysis. First, the homogenized biological samples are dissolved in hydrochloric acid (HCl) and reduced by stannous chloride (SnCl<small><sub>2</sub></small>) to convert IHg to Hg(0) vapor that is subsequently purged and trapped in the downstream trapping solution. Then, the sample residue is treated with potassium permanganate (KMnO<small><sub>4</sub></small>) and potassium persulfate (K<small><sub>2</sub></small>S<small><sub>2</sub></small>O<small><sub>8</sub></small>) to fully demethylate MeHg into IHg, which undergoes a second stage of SnCl<small><sub>2</sub></small> reduction and Hg(0) purging and trapping. The intermediate precision of this protocol was verified by monitoring Hg recoveries and isotopic compositions of both certified reference materials and natural samples. Our protocol provides the advantages of simultaneously separating IHg and MeHg from a single sample aliquot, featuring a rapid processing time of ∼3.5 h, a minimal procedural blank of ∼0.03 ng mL<small><sup>−1</sup></small>, high recoveries (IHg: 96.2 ± 5.8% and MeHg: 96.8 ± 5.6%), and the capability to handle large volumes of samples.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 727-737"},"PeriodicalIF":3.1,"publicationDate":"2024-12-26","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553601","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
Automated on-line monitoring of a lithium hydroxide production process using micro-discharge OES†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-17 DOI: 10.1039/D4JA00330F
Bastian Wiggershaus, Miisamari Jeskanen, Aappo Roos, Toni Laurila and Carla Vogt
{"title":"Automated on-line monitoring of a lithium hydroxide production process using micro-discharge OES†","authors":"Bastian Wiggershaus, Miisamari Jeskanen, Aappo Roos, Toni Laurila and Carla Vogt","doi":"10.1039/D4JA00330F","DOIUrl":"https://doi.org/10.1039/D4JA00330F","url":null,"abstract":"<p >The fast, precise and continuous on-line analysis of highly saline process solutions is challenging for conventional laboratory techniques like ICP-OES or ICP-MS due to the necessity of high plasma gas flow rates (Ar and He), a high power consumption and the limited resistance of the sensitive spectrometer technique to harsh on-site conditions like dust, vibrations or temperature fluctuations. Therefore, an on-site and on-line method with comparable performance despite such conditions would be preferable. In this study we used the Micro-Discharge Optical Emission Spectroscopy (μDOES) for the given challenge of monitoring fully automated on-site and on-line production of lithium hydroxide, which is an essential precursor for the battery industry. The technology is based on creating a micro-plasma directly inside the aqueous sample without any carrier gas by using electrodes and high voltage pulses and thus enabling optical emission spectroscopy on-site. After optimisation of several parameters like sample conductivity, signal integration settings or selection of emission lines, measurements were carried out at an industrial pilot plant. The entire process chain was monitored, starting with the leaching of the calcined lithium-containing ore, through several intermediate products to the end product lithium hydroxide monohydrate of battery grade. The individual process steps were measured continuously (10–20 h), simplifying the monitoring of the process and allowing trends in the concentrations of the elements Li, Na, K, Ca, Mg and Rb to be identified. Reference measurements were performed using laboratory ICP-OES and/or ion chromatography to verify the results. Micro-discharge OES proved to be useful for a fast and precise on-site and on-line analysis of saline solutions with good long-term stability and a high agreement with the used reference methods, resulting in deviations below 10% for the most important components Li, Na and K.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 2","pages":" 338-345"},"PeriodicalIF":3.1,"publicationDate":"2024-12-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ja/d4ja00330f?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143184580","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
Highly selective cloud point extraction of thorium(iv) ions in environmental samples for their ultra-trace level determination by total reflection X-ray fluorescence spectrometry†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-13 DOI: 10.1039/D4JA00348A
Abhijit Saha, Kaushik Sanyal, Khushboo Kumari, Sadhan Bijoy Deb and Manoj Kumar Saxena
{"title":"Highly selective cloud point extraction of thorium(iv) ions in environmental samples for their ultra-trace level determination by total reflection X-ray fluorescence spectrometry†","authors":"Abhijit Saha, Kaushik Sanyal, Khushboo Kumari, Sadhan Bijoy Deb and Manoj Kumar Saxena","doi":"10.1039/D4JA00348A","DOIUrl":"https://doi.org/10.1039/D4JA00348A","url":null,"abstract":"<p >The toxicological effects of thorium on human health are twofold due to its chemical as well as radiological toxicity. The mining of natural thorium resources and anthropogenic uses of thorium contribute to its increased human exposure. Thorium compounds are known as potential occupational carcinogens. The low solubility of thorium compounds in natural water systems requires ultra-trace level detection of Th(<small>IV</small>) ions. This calls for the selective preconcentration of Th(<small>IV</small>) in the presence of ubiquitously present uranium and lanthanides along with naturally abundant alkali, alkaline earth, and transition metals. In this work, the bis(phosphoramidate) ligand was examined for selective cloud point extraction (CPE) of the Th(<small>IV</small>) ion. The CPE parameters were optimized for quantitative recovery of Th(<small>IV</small>). It was found that at pH 4 the ligand and sodium dodecyl sulfate in the micelle medium made a supramolecular complex with Th(<small>IV</small>) <em>via</em> a cation exchange mechanism. The CPE procedure was found to have an extraction efficiency and recovery of (98.9 ± 0.2)% and 99% respectively. The preconcentration factor of the method was 91. All these parameters resulted in quantitative preconcentration of Th(<small>IV</small>) in the surfactant rich phase (SRP) which was then directly analyzed by total reflection X-ray fluorescence (TXRF) spectrometry. The small sample volume requirement of the TXRF technique makes it an excellent candidate for microlitre volume SRP analysis without compromising on the preconcentration factor. Oxidative pyrolysis of the SRP before TXRF analysis improved the thorium detection limit from 0.9 to 0.1 μg L<small><sup>−1</sup></small>. The proposed analytical methodology was validated by analyzing certified reference materials (CRMs) and real samples <em>via</em> spike addition. The overall process had a maximum precision of 2% on the reported results.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 2","pages":" 447-456"},"PeriodicalIF":3.1,"publicationDate":"2024-12-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143184593","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
Enhanced emission spectra from flame-assisted LIBS for high-sensitivity detection of Pb in water 用于高灵敏度检测水中铅的火焰辅助 LIBS 增强发射光谱
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-13 DOI: 10.1039/D4JA00294F
Xiangtong Wan, Xin Yu, Yutong Chen, Ying Wang, Anmin Chen and Mingxing Jin
{"title":"Enhanced emission spectra from flame-assisted LIBS for high-sensitivity detection of Pb in water","authors":"Xiangtong Wan, Xin Yu, Yutong Chen, Ying Wang, Anmin Chen and Mingxing Jin","doi":"10.1039/D4JA00294F","DOIUrl":"https://doi.org/10.1039/D4JA00294F","url":null,"abstract":"<p >Laser-induced breakdown spectroscopy (LIBS) is a powerful technique for detecting and analyzing material elements through plasma emission generated by high-power laser pulses. In this study, the enhancement of Cu plasma emission spectra using flame-assisted LIBS was investigated. The plasma temperature and electron number density were calculated to understand the enhancement mechanism. Additionally, the dry droplet pretreatment method was combined with flame-assisted LIBS to quantitatively analyze trace amounts of heavy metal Pb in aqueous solutions. A calibration curve for Pb was established, and the limits of detection (LOD) for Pb with and without flame assistance were determined. The LOD without flame was 15.120 ng mL<small><sup>−1</sup></small>, while the LOD with flame assistance was significantly lower at 0.741 ng mL<small><sup>−1</sup></small>, demonstrating a 20-fold improvement. The <em>R</em><small><sup>2</sup></small> values of the calibration curves with and without flame assistance were 0.987 and 0.999, respectively. These results confirm that the flame-assisted method significantly enhances LIBS signal intensity, and the combination with dry droplet pretreatment improves the sensitivity for analyzing trace metal elements in water.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 2","pages":" 365-373"},"PeriodicalIF":3.1,"publicationDate":"2024-12-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143184582","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
Atomic spectrometry update – a review of advances in environmental analysis 原子光谱法的最新进展——环境分析的进展综述
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-11 DOI: 10.1039/D4JA90056A
Warren R. L. Cairns, Owen T. Butler, Olga Cavoura, Christine M. Davidson, José-Luis Todolí-Torró and Marcus von der Au
{"title":"Atomic spectrometry update – a review of advances in environmental analysis","authors":"Warren R. L. Cairns, Owen T. Butler, Olga Cavoura, Christine M. Davidson, José-Luis Todolí-Torró and Marcus von der Au","doi":"10.1039/D4JA90056A","DOIUrl":"https://doi.org/10.1039/D4JA90056A","url":null,"abstract":"&lt;p &gt;Highlights in the field of air analysis included: a new focus on measuring micro- and nanoplastic particles in air, the development of hyphenated ICP-MS systems for &lt;em&gt;in situ&lt;/em&gt; sampling and measurement of airborne metallic particles and the reported use of wearable black carbon sensors for measuring exposure to diesel fumes within the workplace. Significant advancements in the analysis of waters have been made in developing novel resin materials and new protocols for existing commercially available resins, aimed at the determination and speciation of trace levels of metals and metalloids in water matrices. These developments have been validated for sample purification and pre-concentration. In addition to traditional column chemistry, on-line hyphenated techniques were employed to enhance speciation analysis, with optimized methods enabling faster analysis and facilitating a more holistic approach by allowing the simultaneous detection of multiple species or elements in a single run. Efforts have also been directed towards detecting particles in the micro- and nanometer range, broadening the analytical scope beyond the ionic fraction. This year, the focus shifted from natural and engineered nanoparticles towards the critical field of plastic pollution, with several innovative methodologies introduced. Furthermore, to achieve better precision and lower detection limits in the field of MS/MS, numerous studies explored the behaviour of gases and reactions within reaction cells, contributing to the refinement of these techniques. In the analysis of soils and plants, methods aimed at improving the efficiency of green solvents were again prominent. Developments in AES were largely driven by the desire to create small, low-cost, low-power-consumption instrumentation suitable for field deployment. The study of NPs in soil and plant systems continued to be a focus for sp-ICP-MS. The past year has again seen a large volume of publications featuring LIBS, with particular interest in methods to enhance signal intensity and thereby improve limits of detection. Of interest in XRF was the development of in-house spectrometers for underwater mercury screening and &lt;em&gt;in vivo&lt;/em&gt; plant analysis. Developments in geological analysis include new homogeneous natural and synthetic materials that have been developed as reference materials (RMs) in the analysis of geological samples by microanalytical techniques, such as LA-ICP-MS, LIBS and SIMS. Additional information on already existing RMs has been obtained for &lt;em&gt;in situ&lt;/em&gt; isotope ratio determinations. Attention has been paid to sample preparation and purification methods able to shorten the analysis time and to improve the accuracy. Much attention has been paid to the use of LA-ICP-MS/MS as a means for removing spectral interferences in the case of &lt;em&gt;in situ&lt;/em&gt; localized isotopic analysis and dating of geological materials. The development of new chemometric models as well as software has continue","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 1","pages":" 11-69"},"PeriodicalIF":3.1,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142912688","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
In situ carbon isotope analysis of diamonds using LA-MC-ICP-MS inspired by the distribution of ions and isotope ratios in ICP†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-11 DOI: 10.1039/D4JA00354C
Yi-Ming Huo, Zhi-Yong Zhu, Chang-Fu Fan, Yu-Wei She, Jia-Long Hao and Xiang-Kun Zhu
{"title":"In situ carbon isotope analysis of diamonds using LA-MC-ICP-MS inspired by the distribution of ions and isotope ratios in ICP†","authors":"Yi-Ming Huo, Zhi-Yong Zhu, Chang-Fu Fan, Yu-Wei She, Jia-Long Hao and Xiang-Kun Zhu","doi":"10.1039/D4JA00354C","DOIUrl":"https://doi.org/10.1039/D4JA00354C","url":null,"abstract":"<p >Carbon-stable isotopes of diamonds provide clues regarding their growth processes. Thus, an accurate, efficient, and affordable method to determine the carbon isotope ratio is extremely urgent. Accurate and precise determination of the carbon isotope ratio with LA-MC-ICP-MS is limited by the high background intensity of <small><sup>12</sup></small>C<small><sup>+</sup></small> and instrumental settings. Hence, laser parameters were gradient-changed to investigate their influences on carbon isotope analysis. Besides, high-resolution spatial distributions of <small><sup>12</sup></small>C<small><sup>+</sup></small> and <small><sup>40</sup></small>Ar<small><sup>3+</sup></small> intensities coupled with the <small><sup>13</sup></small>C/<small><sup>12</sup></small>C value in the ICP were investigated in detail to elucidate the ionization kinetics of <small><sup>40</sup></small>Ar<small><sup>3+</sup></small> and to determine the most stable zone for carbon isotope analysis in the ICP. Finally, two types of diamonds (a natural diamond (D-N-1) and synthetic diamond (D-HTHP)) were measured to verify their homogeneity and flexibility for <em>in situ</em> analysis of the carbon isotope on diamonds with LA-MC-ICP-MS. The signal-to-noise ratio (SINR) greatly affects precision, which could be significantly improved by optimizing laser parameters. The internal precision of <em>in situ</em> C isotope analysis is better than 0.2‰ (2SE) when the SINR is more than 4. The ionization efficiency of <small><sup>40</sup></small>Ar<small><sup>3+</sup></small> was found to be controlled by the catalysis of C ions and the thermodynamic parameters of the ICP. The most stable zone for carbon isotope analysis in the ICP was found to be located at ≈1.4 mm ahead of the <small><sup>12</sup></small>C<small><sup>+</sup></small> signal-maximum point. Hence, the precision of <small><sup>13</sup></small>C/<small><sup>12</sup></small>C could be improved when the torch was retreated ≈1.4 mm from the maximum <small><sup>12</sup></small>C<small><sup>+</sup></small> intensity point axially. The natural and synthetic diamonds exhibited similar down-hole fractionation behaviors of the C isotope during laser ablation, indicating that they can be used to correct each other with LA-MC-ICP-MS. The accuracy of the carbon isotope was validated by comparing the data with those of nano-scale secondary ion mass spectrometry (NanoSIMS) and laser ablation-isotope ratio mass spectrometry (LA-IRMS). This study suggested that <em>in situ</em> LA-MC-ICP-MS is a rapid, precise and accurate way to measure the carbon isotope of diamonds. The interactive influence of the ionization process of nuclides leads to elemental and isotopic fractionations, which is one of the mechanisms of the matrix effect.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 3","pages":" 700-714"},"PeriodicalIF":3.1,"publicationDate":"2024-12-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143553599","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
Rapid determination of iodide ion content in chloride molten salt by ascorbic acid reduction
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-10 DOI: 10.1039/D4JA00242C
Ming Cheng, Junxia Geng, Haixia Cong, Qiang Dou and Haiying Fu
{"title":"Rapid determination of iodide ion content in chloride molten salt by ascorbic acid reduction","authors":"Ming Cheng, Junxia Geng, Haixia Cong, Qiang Dou and Haiying Fu","doi":"10.1039/D4JA00242C","DOIUrl":"https://doi.org/10.1039/D4JA00242C","url":null,"abstract":"<p >This study aimed to establish an alternative method for assessing the efficacy of removing fission product iodine from molten salt spent nuclear fuel under acidic conditions. In the pretreatment stage, ascorbic acid with a mass fraction of 0.5 wt% was used instead of dilute nitric acid with a volume fraction less than 2 vol%. The iodide content of molten salt samples dissolved in various ratios of Cl<small><sup>−</sup></small> to I<small><sup>−</sup></small> was determined and compared by inductively coupled plasma mass spectrometry (ICP-MS) and ion chromatography (IC). The iodide ions in simulated chloride salts containing LiI were tested after pretreatment. It was found that at 1.0 mg L<small><sup>−1</sup></small> chloride ion concentration, the detection limit of this method was 0.255 μg L<small><sup>−1</sup></small>, with a spike-and-recovery experience between 103.3% and 102.8% and a relative standard deviation of less than 3% (<em>n</em> = 6). The average spike-and-recovery experience was 104.3%, and the limit of detection was 0.472 μg L<small><sup>−1</sup></small> at a concentration of 100.0 mg L<small><sup>−1</sup></small> with RSD of less than 5%. When the concentration ratio of Cl<small><sup>−</sup></small>/I<small><sup>−</sup></small> in the molten salt was less than two orders of magnitude, the analytical value of this technique was comparable to the measurement result by IC. Furthermore, the accuracy of ICP-MS was superior to that of IC when the concentration ratio of Cl<small><sup>−</sup></small>/I<small><sup>−</sup></small> was higher than two orders of magnitude. The results indicate that the improved pretreatment method with ascorbic acid can eliminate inaccuracies caused by the iodide memory effect. The method has been verified to determine iodide content in high chloride molten salt under acidic conditions and will be used in the treatment of spent fuel from molten salt reactors.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 2","pages":" 429-436"},"PeriodicalIF":3.1,"publicationDate":"2024-12-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143184591","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
Three new natural secondary reference materials for in situ andradite U–Pb geochronology†
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-06 DOI: 10.1039/D4JA00290C
Yueheng Yang, Shitou Wu, Hao Wang, Sandra L. Kamo, Qian Ma, Ting Liang, Lei Xu, Liewen Xie, Chao Huang, Bo Wan, Jinhui Yang and Fuyuan Wu
{"title":"Three new natural secondary reference materials for in situ andradite U–Pb geochronology†","authors":"Yueheng Yang, Shitou Wu, Hao Wang, Sandra L. Kamo, Qian Ma, Ting Liang, Lei Xu, Liewen Xie, Chao Huang, Bo Wan, Jinhui Yang and Fuyuan Wu","doi":"10.1039/D4JA00290C","DOIUrl":"https://doi.org/10.1039/D4JA00290C","url":null,"abstract":"<p >Andradite-rich garnet is a common mineral found in various rock types, such as alkaline igneous rocks and skarns, and often exhibits high U/Pb ratios, making it suitable for <em>in situ</em> U–Pb dating. However, the limited availability of well-characterised andradite reference materials has impeded their broader application in microanalysis. In this study, three natural andradite samples (MKWB, DGS, and Stanley) have been characterised and assessed as potential secondary reference materials for <em>in situ</em> U–Pb geochronology. U–Pb isotopic analyses were conducted across four different laboratories using isotope dilution – TIMS, SIMS, and laser ablation (SF, Q)-ICP-MS, to examine the homogeneity of the euhedral andradite crystals. We report ID-TIMS <small><sup>206</sup></small>Pb/<small><sup>238</sup></small>U ages of 264.9 ± 5.8 Ma (2 s, <em>n</em> = 6, MSWD = 3.4), 139.42 ± 0.36 Ma (2 s, <em>n</em> = 5, MSWD = 1.9), and 23.28 ± 0.38 Ma (2 s, <em>n</em> = 3, MSWD = 1.9) for MKWB, DGS, and Stanley, respectively. These three newly characterised natural secondary reference materials should significantly contribute to the advancement of <em>in situ</em> U–Pb andradite-rich garnet geochronology.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 2","pages":" 326-337"},"PeriodicalIF":3.1,"publicationDate":"2024-12-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143184578","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
Comparison of nanosecond and femtosecond laser-induced breakdown spectroscopy for determination of U and Th in tantalum–niobium ores
IF 3.1 2区 化学
Journal of Analytical Atomic Spectrometry Pub Date : 2024-12-06 DOI: 10.1039/D4JA00268G
Xiaoliang Liu, Shichao Ren, Ming Zhang, Lingling Peng, Ye Zhang, Xiangting Meng, Shujia Wu, Yuhong Li, Lin Liu and Shaohua Sun
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