Journal of Analytical Atomic Spectrometry最新文献

{"title":"Elemental detection of jades with reduced sample damage by target-enhanced orthogonal double-pulse LIBS using surface micro-structured copper target","authors":"Yufeng Li, Zenghui Wang, Xueqin Huang, Runhua Li and Yuqi Chen","doi":"10.1039/D5JA00235D","DOIUrl":"https://doi.org/10.1039/D5JA00235D","url":null,"abstract":"<p >Reduced sample damage is necessary when sensitive elemental analysis is carried out on precious samples. High analytical sensitivity and reduced sample damage are contradictory in the conventional laser-induced breakdown spectroscopy (LIBS) analysis. To solve this problem, target-enhanced orthogonal double-pulse LIBS (TEODP-LIBS) in a reheating regime was developed in this work. A copper plate fabricated with periodic micro-structures on its surface using electroplating was used as the signal enhancement target. The presence of periodic micro-structures on the copper surface changes the laser–target and laser–plasma interactions, increasing both temperature and electron density of the plasma, thus being able to introduce about 2-folds secondary signal enhancement for the sample elements compared with the flat surface copper target. Xiuyan jade samples were analyzed experimentally. For minor element detection, the same level of signal intensity was detected <em>via</em> reheating TEODP-LIBS as that <em>via</em> single-pulse LIBS, but due to the selection of different pulse energies, a 19.6-fold reduction in sample damage was observed. This work demonstrated the possibility of using a surface micro-structured solid plate as the signal enhancement target in TEODP-LIBS to facilitate more sensitive elemental detection in solid samples. This technique is especially useful for the elemental analysis of precious samples, when reduced sample damage is required.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 10","pages":" 2737-2744"},"PeriodicalIF":3.1,"publicationDate":"2025-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145196067","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}

{"title":"Correction: Quantification of ferric iron content in minerals via the STEM-EELS-mapping method","authors":"Shan Li, Ke Wen, Yiping Yang, Xiaoju Lin, Yonghua Cao, Yao Xiao, Haiyang Xian, Jianxi Zhu and Hongping He","doi":"10.1039/D5JA90036K","DOIUrl":"https://doi.org/10.1039/D5JA90036K","url":null,"abstract":"<p >Correction for ‘Quantification of ferric iron content in minerals <em>via</em> the STEM-EELS-mapping method’ by Shan Li <em>et al.</em>, <em>J. Anal. At. Spectrom.</em>, 2025, https://doi.org/10.1039/D5JA00002E.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 9","pages":" 2608-2608"},"PeriodicalIF":3.1,"publicationDate":"2025-08-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ja/d5ja90036k?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144909587","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}

{"title":"A novel approach to achieve Os isotope equilibration under ambient conditions for negative thermal ionization mass spectrometry (N-TIMS) analysis","authors":"Jin-Hua Liu, Xiao-Dong Deng, Jian-Wei Li, Lan-Ping Feng and Thomas J. Algeo","doi":"10.1039/D5JA00151J","DOIUrl":"https://doi.org/10.1039/D5JA00151J","url":null,"abstract":"<p >The rhenium–osmium (Re–Os) isotopic system has emerged as a widely utilized tool in cosmochemistry and high-temperature geochemical studies. A critical prerequisite for high-precision Os isotope analysis <em>via</em> Negative Thermal Ionization Mass Spectrometry (N-TIMS) involves achieving complete isotopic equilibrium between the sample and spike through the isotope dilution technique. In this study, we present an innovative technique to address valence state disparities in Os species within mixed solutions, thereby enabling effective isotopic equilibration through a chemical reducing reaction with a strong reductant under ambient conditions. Experimental results demonstrate that a solution containing 0.05 mol L<small>⁻¹</small> hydroxylamine hydrochloride (NH<small>₂</small>OH·HCl) coupled with 0.01 mol L<small>⁻¹</small> HBr effectively stabilizes a nanogram-level Os mass. Systematic optimization of reductant concentration and sample-to-reductant ratio yielded a mean <small>¹⁹⁰</small>Os/<small>¹⁸⁸</small>Os value of 1.2280 ± 0.0006 (2<em>s</em>, <em>n</em> = 18) for a mixed Os spike solution, closely aligned with the recommended value of 1.2278 ± 0.0003 (2<em>s</em>, <em>n</em> = 12) obtained through the conventional Carius tube method. Controlled comparative experiments revealed critical considerations for method implementation: (1) a freshly prepared reductant must be employed immediately to ensure reagent efficacy, and (2) precise absolute volume control of the reductant solution is essential to mitigate potential losses of volatile OsO<small>₄</small> linked to extended decomposition times. This novel approach successfully achieves isotopic equilibration between sample–spike and inter-spike components under ambient conditions, offering significant analytical advantages over traditional methods. The validity of the proposed approach was demonstrated by analyzing reference material WMS-1a yielding a <small>¹⁸⁷</small>Os/<small>¹⁸⁸</small>Os value of 0.1665 ± 0.0006 (2<em>s</em>, <em>n</em> = 5), which agrees within uncertainty with the established value of 0.1664 ± 0.0003 (2<em>s</em>, <em>n</em> = 5) obtained <em>via</em> the Carius tube method. The protocol enhances operational efficiency by reducing equilibration time and explosive risk, and decreases procedural Os blanks <em>via</em> reducing material and reagent consumption. The combined improvements in precision, cost-effectiveness, and methodological flexibility position this technique as a valuable advancement in Os isotope geochemistry.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 10","pages":" 2641-2648"},"PeriodicalIF":3.1,"publicationDate":"2025-08-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145196074","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}

{"title":"Evaluation of different types of paper as solid substrates and their effects on LIBS emission signals","authors":"Adriana L. Sales, Nilvan A. Silva and Ivo M. Raimundo","doi":"10.1039/D5JA00194C","DOIUrl":"https://doi.org/10.1039/D5JA00194C","url":null,"abstract":"<p >In the present work, different types of paper were evaluated as a solid substrate for LIBS measurements, aimed at verifying their effects on the emission signals, taking into account their grammage, thickness and metal ions naturally present (minor components/impurities). Cu(<small>II</small>) and Mn(<small>II</small>) ions were used in the present study. The emission signals for Cu <small>I</small> and Mn <small>I</small> significantly varied depending on the paper type, whose intensities decreased after rinsing with nitric acid solution. No correlation was found between signal intensity and paper grammage or paper thickness, whose effect could be hidden by the metal ions present in the paper, as signals significantly decreased after their removal. In addition, after washing with nitric acid solution, the wettability of the paper (measured as the contact angle with water) increased, allowing a more effective absorption of the metal ion solution by the paper, a fact that can also contribute to decreasing the signal intensity. The addition of Na(<small>I</small>) and Ca(<small>II</small>) ions in the paper sheet previously rinsed with nitric acid solution caused an increase in the signal emission of Cu <small>I</small> and Mn <small>I</small>, as these ions can contribute to the electron density of the plasma, increasing its temperature. However, the addition of Fe(<small>II</small>) ions and other transition metal ions in the paper also provided an increase in the emission of Cu <small>I</small> and Mn <small>I</small> and signal intensities can be recovered by adding a mix of these metal ions on the paper. The sensitivity of the measurements (taken as the slope of the calibration curve) provided by using office paper as a substrate was around 14 and 2.7 times higher than those obtained with quantitative filter paper for Cu and Mn, respectively. Therefore, depending on the analyte to be determined, ordinary paper can be used to improve the sensitivity of the desired LIBS method.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 10","pages":" 2682-2691"},"PeriodicalIF":3.1,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145196078","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}

{"title":"SI-traceable total analysis of nitrate and nitrite by isotope dilution optical spectroscopy and its application to Berlin surface waters","authors":"Carlos Abad, Dennis Jegielka, Allen Aloysius and Sebastian Recknagel","doi":"10.1039/D5JA00252D","DOIUrl":"https://doi.org/10.1039/D5JA00252D","url":null,"abstract":"<p >Accurate nitrate and nitrite data support water-quality regulation, yet routine methods rely on external calibration and rarely achieve SI traceability. We report a calibration-free determination of nitrate and nitrite by combining isotope dilution with high-resolution continuum-source graphite furnace molecular absorption spectrometry (ID-HR-CS-GF-MAS). A <small>¹⁵</small>N-enriched nitrate spike (its concentration verified by reverse isotope dilution against the standard reference material NIST 3185) provides the SI link, and it is gravimetrically added to samples; nitrate and residual nitrite are converted in situ to nitric oxide (NO), whose 215 nm band is recorded at a pixel resolution of <em>λ</em>/Δ<em>λ</em> ≈ 140 000. The 0.2127 nm shift between <small>¹⁴</small>NO and <small>¹⁵</small>NO electronic spectra is resolved, and a three-latent-variable partial least squares regression model yields the <small>¹⁵</small>N/<small>¹⁴</small>N ratio with 0.3% precision. Instrumental LoD values of 4.8 ng (<small>¹⁴</small>N) and 3.2 ng (<small>¹⁵</small>N) translate to a method LoD of 4.8 ng of nitrogen (equivalent to 1.05 mg L<small>⁻¹</small> NO<small>₃</small><small>⁻</small> for a 20 μL aliquot). The furnace program allows for successive drying/pyrolysis loops, so additional 20 μL aliquots can be layered onto the graphite platform. Alternatively, a 10 mL anion-exchange solid-phase extraction step concentrates nitrate and nitrite fivefold, allowing for the analysis of even lower sample concentrations. Results for four certified reference materials (2.9 to 1000 mg L<small>⁻¹</small> NO<small>₃</small><small>⁻</small>) agreed with certified values, giving relative expanded uncertainties of 2 to 4%. Analysis of twenty Berlin surface-water samples revealed concentrations ranging from 0.10 to 7.3 mg L<small>⁻¹</small> NO<small>₃</small><small>⁻</small>, indicating that the Panke River and Teltow Canal are the primary sources of nitrogen. ID-HR-CS-GF-MAS thus delivers ID-MS-level accuracy in a few minutes per run with bench-top optics, and, with optional on-platform or SPE pre-concentration, extends SI-traceable nitrate/nitrite monitoring into the low-ng regime.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 10","pages":" 2692-2701"},"PeriodicalIF":3.1,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ja/d5ja00252d?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145196083","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}

{"title":"Single particle inductively coupled plasma mass spectrometry for the characterization of colloidal particles in soils, sediments and sludges: comparative study of sector field and time-of-flight instruments","authors":"Zhizhong Li, Madjid Hadioui and Kevin J. Wilkinson","doi":"10.1039/D5JA00181A","DOIUrl":"https://doi.org/10.1039/D5JA00181A","url":null,"abstract":"<p >Colloids and nanoparticles in solid phase environmental matrices (soils, sediments, sludges) are widely heterogenous and polydisperse, which complicates their sampling and characterization by bulk analysis techniques. Indeed, techniques based upon single particle measurements are better equipped for identifying important, but low frequency, properties or characteristics which are needed to understand the function of environmental colloids. In this study, a continuous flow extraction assisted by ultrasound was used to sample colloidal particles from several solid matrices. The high sensitivity of a sector field ICP-MS and the quasi-instantaneous, multi-isotope measurements of a time-of-flight ICP-MS were combined to enable the characterization of colloidal particles extracted from soils, sediments and sludges. Single particle (SP) analysis of the particle leachates using the sector field instrument (SP-ICP-SF-MS) led to the detection of larger numbers (up to 6800×) of Mg-, Al-, Si-, Ca-, Ti-, Fe-, and Ba-containing particles than measured by single particle time-of-flight ICP-MS (SP-ICP-ToF-MS), largely due to the different size detection limits of the techniques, <em>i.e. ca.</em> 16 nm by SP-ICP-SF-MS and 76 nm by SP-ICP-ToF-MS, when measuring aluminosilicates. Despite the limitation of SP-ICP-ToF-MS in detecting smaller particles, the technique was successfully used to identify mineral phases of illite, vermiculite, and smectite based on elemental ratios in the individual particles. The multi-isotope capability of the SP-ICP-ToF-MS was also used for the determination of isotopic ratios in both individual particles and bulk digested leachates. Mean <small>²⁰⁶</small>Pb/<small>²⁰⁷</small>Pb ratios in the particles extracted from the solid phase samples deviated from measurements obtained from bulk digestions by 1.2–5.9%, indicating the potential of the SP-ICP-ToF-MS to perform such measurements. SP-ICP-SF-MS and SP-ICP-ToF-MS were complementary for obtaining insight into the composition and particle size distributions of the colloids and nanoparticles. Specifically, neither technique gave the complete particle size distribution due to their complementary size detection windows.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 9","pages":" 2487-2497"},"PeriodicalIF":3.1,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ja/d5ja00181a?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144909593","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}

{"title":"Influence of sample matrix and filter fixation on LIBS signal in analysis of algae on filter","authors":"Aleš Hrdlička, Jana Horská, Jitka Hegrová, Martina Bucková, David Prochazka, Jakub Buday, Pavel Pořízka, Viktor Kanický and Jozef Kaiser","doi":"10.1039/D5JA00236B","DOIUrl":"https://doi.org/10.1039/D5JA00236B","url":null,"abstract":"<p >This study first reveals the matrix effect mechanism of filter fixation on laser-induced breakdown spectroscopy (LIBS) quantitative analysis of algae, providing a methodological reference for <em>in situ</em> environmental detection. A collinear 1064 nm double pulse LIBS was used for analysis of green algae on a cellulose filter. Intensities of the contaminant elements Zn, Ni and those of some matrix lines of C I, Ca I, II, K I, Mg I, II, Mn I, II, Na I, H I, O I were measured and compared for various numbers of tape layers used for the filter fixation onto a microscope glass slide. This arrangement simulated surface modifications which can substantially lower the measured intensities. Maximum intensities were measured for 1 or 2 tape layers and lowest intensities for 6 layers for filters with contaminated algae; however, this intuitive result was not yielded for non-contaminated algae. It might indicate substantial changes of the filter properties and interaction with the laser beam at minimal changes of the analyte. This is crucial for quantitative analysis influenced not only by the sample fixation and surface quality but also by the composition of the filtered algae. The results were, to some extent, supported by principal component analysis, a shadowgraphic study of a single pulse microplasma shockwave, crater size and by simplified geometric and thermodynamic models. These were based on a spherical shape and full validity of the Boltzmann distribution respectively. The relatively small changes of the abovementioned parameters are in contrast to important changes of the lines intensities measured from the microplasma on the contaminated samples.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 9","pages":" 2426-2437"},"PeriodicalIF":3.1,"publicationDate":"2025-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ja/d5ja00236b?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144909574","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}

{"title":"Self-organizing maps for the detection and classification of natural nanoparticles, nanoparticle systems and engineered nanoparticles characterized using single particle ICP-time-of-flight-MS","authors":"C. W. Cuss, M. F. Benedetti, Carla Costamanga, Lucas Mesnard and M. Tharaud","doi":"10.1039/D5JA00179J","DOIUrl":"https://doi.org/10.1039/D5JA00179J","url":null,"abstract":"<p >The development of single-particle inductively coupled plasma time-of-flight mass spectrometry (spICP-ToF-MS) heralds a breakthrough in our ability to measure the multi-elemental composition of natural nanoparticles and colloids (NPs), and to characterize the dynamics, responses, and impacts of systems of natural NPs (NNPs). However, further developments and associated comparisons across studies and research groups are hindered by the lack of a consistent, reliable and comparable approach for detecting and differentiating NPs and NNPs. Self-organizing maps (SOM, aka Kohonen networks) are single-layer artificial neural networks that are widely used for pattern recognition and classification in the natural sciences and beyond. The SOM is a nonparametric statistical method which adapts to data structures and is robust to noise, outliers, and sparse data, making it especially suitable for peak detection and particle classification using raw spICP-ToF-MS time-series. This article provides a brief review of SOM and their outputs before demonstrating their ability to detect particles in spICP-ToF-MS time-series, and to characterize and compare NNPs. Additional considerations and research directions for the application of SOM to spICP-ToF-MS and particle data are then discussed. The raw data and algorithms used in this study are provided in the SI to facilitate the testing of SOM across research groups, and for comparing their performance with other methods.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 9","pages":" 2471-2486"},"PeriodicalIF":3.1,"publicationDate":"2025-07-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ja/d5ja00179j?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144909592","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}

{"title":"High-precision quantification and low detection limits of chlorine and fluorine in coal via laser-induced breakdown spectroscopy","authors":"Yazi Wang, Xiaoning Yang, Wen Yi, Xiaodong Liu, Haohan Sun, Xinyu Zhang, Shuoyu Yang, Yongyi Du, Jiaqi Zhao, Yue Lv, Caihao Ding, Lixiang Zhong and Ruibin Liu","doi":"10.1039/D5JA00199D","DOIUrl":"https://doi.org/10.1039/D5JA00199D","url":null,"abstract":"<p >Chlorine (Cl) and fluorine (F), as halogen elements, hold significant detection value across numerous fields (<em>e.g.</em>, Mars exploration, industrial production, and environmental protection). Conventional detection methods are not only intricate and time-consuming but also fail to facilitate real-time analysis. In contrast, laser-induced breakdown spectroscopy (LIBS) offers simplicity, rapidity, and the capability for simultaneous multi-element detection. However, detecting Cl and F in coal using LIBS presents substantial challenges, primarily due to coal's complex matrix effects and the difficulty of exciting halogens to generate high-intensity atomic peaks. To overcome these obstacles, this study investigated the correlation between F and Cl content and characteristic peaks using statistical methods. It was found that Ca emission lines exhibit a high correlation (&gt;0.9) with Cl and F. The unification of high correlation and low Gibbs free energy laws elucidates the influence of underlying chemical reaction pathways from thermodynamic and statistical perspectives, offering a promising solution for detecting low – content elements in complex matrices. Ultimately, principal component analysis combined with partial least squares (PCA–PLS) modeling was applied to analyze preprocessed spectra. This approach effectively mitigated the matrix effects in coal and enhanced the model's robustness. The root mean square error (RMSE) for F and Cl prediction results in the out-of-model set were 0.0447 wt% and 0.0809 wt%, respectively. This study achieved highly accurate simultaneous quantitative analysis of F and Cl at low detection limits. Specifically, the limits of detection (LOD) are 0.04 wt% for F and 0.06 wt% for Cl, respectively. Compared to the traditional LIBS atomic line method, these LODs are lower, and the detection accuracies are higher. In this study, for the first time, LIBS technology has achieved synchronous low LOD detection of F and Cl in coal, and it is capable of meeting the detection requirements for practical applications. This provides a novel approach for the rapid, efficient, and simultaneous detection of hazardous elements in coal, contributing to reduced environmental pollution.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 9","pages":" 2462-2470"},"PeriodicalIF":3.1,"publicationDate":"2025-07-30","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144909561","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}

{"title":"Operando laboratory XAS on battery materials using the DANOISE cell in a von Hámos spectrometer","authors":"Sebastian Praetz, Morten Johansen, Delf Kober, Marko Tesic, Christopher Schlesiger, Dorthe Bomholdt Ravnsbæk and Birgit Kanngießer","doi":"10.1039/D5JA00155B","DOIUrl":"https://doi.org/10.1039/D5JA00155B","url":null,"abstract":"<p >This work presents laboratory-based <em>operando</em> X-ray absorption spectroscopy (XAS) measurements on electrodes for rechargeable batteries. Using the “Developed in Aarhus: New <em>Operando</em> In-house Scattering Electrochemical” (DANOISE) cell, <em>operando</em> XAS measurements were performed with two von Hámos spectrometers, optimized for X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). Selected battery electrodes, including commercial LiFePO<small>₄</small> (LFP) for Li-ion batteries and layered transition metal oxides, Na<small>_<em>x</em></small>TMO<small>₂</small> (TM = Fe, Mn), electrodes for Na-ion batteries, were measured to present a proof of principal for the applicability of these spectrometers in battery research. The von Hámos spectrometers used in this study offer a high efficiency and the ability to measure a large spectral bandwidth (up to 1500 eV beyond the edge). Fe K-edge XANES measurements of LFP with an acquisition time of 15 minutes per spectrum successfully captured the transition of Fe species to FePO<small>₄</small> during cycling. Additionally, Mn K-edge XANES measurements on Na-ion battery materials highlight the challenges associated with Na-ion batteries, particularly due to their higher absorption compared to Li-ion counterparts. Nevertheless, the Mn K-edge was successfully measured, allowing for oxidation state determination in the material. Fe K-edge EXAFS measurements on Na-ion battery materials revealed the transition of Fe species during charging, within an acquisition time of 15 to 25 minutes.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 9","pages":" 2447-2461"},"PeriodicalIF":3.1,"publicationDate":"2025-07-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2025/ja/d5ja00155b?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"144909575","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}