Journal of Analytical Atomic Spectrometry最新文献

{"title":"High-precision MC-ICP-MS measurements of Cd isotopes using a novel double spike method without Sn isobaric interference†","authors":"Jin Li, Suo-han Tang, Xiangkun Zhu, Jian-xiong Ma, Zhiyong Zhu and Bin Yan","doi":"10.1039/D4JA00357H","DOIUrl":"https://doi.org/10.1039/D4JA00357H","url":null,"abstract":"<p >Previous studies have reported that even low concentrations of Sn can lead to biased Cd isotopic measurements using MC-ICP-MS. In this paper, we propose a novel method of Cd isotopic analysis involving use of a <small>¹⁰⁶</small>Cd–<small>¹¹¹</small>Cd double spike. To eliminate isobaric interference from <small>¹¹⁴</small>Sn, we use <small>¹¹³</small>Cd together with <small>¹⁰⁶</small>Cd, <small>¹¹⁰</small>Cd, and <small>¹¹¹</small>Cd to obtain <em>δ</em><small>^113/110</small>Cd, and then calculate <em>δ</em><small>^114/110</small>Cd as 1.33 × <em>δ</em><small>^113/110</small>Cd. We find that when Sn/Cd is ≤2.5 in sample solutions, <em>δ</em><small>^114/110</small>Cd values are not affected by Sn, which behaves as a matrix element rather than causing isobaric interference. Cd isotopic measurements are not sensitive to the molarities of diluted HNO<small>₃</small> or the Cd concentration. Additionally, when Mo/Cd, Ni/Cd, and Se/Cd are ≤1 in sample solutions, Cd isotopic measurements are not significantly affected. Instead, when Zn/Cd is &gt;0.1, In/Cd &gt; 0.05, and Pd/Cd &gt; 5 × 10<small>⁻³</small>, the measured <em>δ</em><small>^114/110</small>Cd values deviate significantly from zero. However, Zn and In can be eliminated completely, and Pd was not detected in any Cd eluents. The <em>δ</em><small>^114/110</small>Cd values of three standard solutions (Spex-CUGB, BAM I012, and Münster) and four geochemical reference materials (SGR-1b, BCR-2, GSD-7a, and NIST 2711a) were measured and found to be in close agreement with published results (with 2SD and ranges for all data of less than 0.090 and 0.120, respectively). This indicates that the data obtained by our double spike method are precise and reliable. Additionally, our new technique can help to simplify separation procedures, thus saving time and reducing the quantities of acid required.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 3106-3115"},"PeriodicalIF":3.1,"publicationDate":"2024-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714077","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":"Laser-induced breakdown spectroscopy (LIBS): calibration challenges, combination with other techniques, and spectral analysis using data science","authors":"Dennis Silva Ferreira, Diego Victor Babos, Mauro Henrique Lima-Filho, Heloisa Froehlick Castello, Alejandro C. Olivieri, Fabiola Manhas Verbi Pereira and Edenir Rodrigues Pereira-Filho","doi":"10.1039/D4JA00250D","DOIUrl":"https://doi.org/10.1039/D4JA00250D","url":null,"abstract":"<p >Laser-Induced Breakdown Spectroscopy (LIBS) is a versatile and powerful analytical technique widely used for rapid, <em>in situ</em> elemental analysis across various fields, from industrial quality control to planetary exploration. This review addresses the critical aspects and emerging trends in LIBS, focusing on calibration challenges, integrating complementary techniques (data fusion), and applying data science for spectral analysis. Calibration is a fundamental challenge in LIBS due to matrix effects, signal drift, and variations in experimental conditions. Recent advancements aim to develop matrix-independent calibration models and employ machine learning algorithms to improve calibration accuracy and robustness. LIBS has also proven invaluable in space exploration, particularly on Mars. Instruments like ChemCam and SuperCam have successfully utilized LIBS to perform real-time chemical analysis of the Martian surface, providing critical insights into its composition and history. The review further explores the advancements in multivariate calibration techniques for handling complex and multi-component systems. Techniques such as Partial Least Squares (PLS) regression and Principal Component Analysis (PCA) are increasingly employed to address the high dimensionality of LIBS data, enhancing the precision and reliability of the analysis. In addition, combining LIBS with other instrumental analytical techniques expands its analytical capabilities. Data fusion strategies integrating LIBS with techniques like Raman spectroscopy, X-ray fluorescence (XRF), and hyperspectral imaging provide a more comprehensive understanding of material composition. These integrated systems, supported by sophisticated data fusion algorithms, offer unprecedented insights and accuracy. Finally, applying data science in LIBS transforms spectral inspection and analysis. Machine learning and deep learning methods are being adopted to automate and enhance the processing and interpretation of LIBS spectra, uncovering complex patterns and improving analysis accuracy. The future lies in leveraging big data analytics and real-time processing to address more complex analytical challenges. In conclusion, LIBS is evolving rapidly, driven by advancements in calibration methods, techniques integration, and data science. This review highlights the potential of LIBS to continue pushing the boundaries of material analysis and its significant contributions to diverse scientific and industrial fields.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 2949-2973"},"PeriodicalIF":3.1,"publicationDate":"2024-11-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714062","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":"Sensitive and rapid determination of the iodine/calcium ratio in carbonate rock samples by ICP-MS based on solution cathode glow discharge sampling†","authors":"Xuan Wang, Xing Liu, Lanlan Jin, Zhenli Zhu, Junhang Dong, Pengju Xing, Linjie Chen, Yuanhui Geng, Jingwen Zhang, Hao Tong, Hongtao Zheng, Min Zhang and Shenghong Hu","doi":"10.1039/D4JA00264D","DOIUrl":"https://doi.org/10.1039/D4JA00264D","url":null,"abstract":"<p >The iodine-to-calcium ratio (I/Ca) in carbonate rocks has been extensively used to indicate marine oxidation states. However, the low-iodine and high-calcium characteristics of carbonate samples pose challenges in achieving rapid and accurate determination of I/Ca. In this study, we have developed a solution cathode glow discharge (SCGD) sampling technique coupled with inductively coupled plasma mass spectrometry (ICP-MS) for highly sensitive and accurate determination of I/Ca in low-iodine carbonate samples. The proposed method takes full advantage of the high-efficiency vapor generation of iodine and the inefficient introduction of calcium by SCGD, thereby significantly enhancing the sensitivity for iodine measurement and reducing matrix interference. In addition, it enables the simultaneous determination of I and Ca even in high-calcium samples. Compared to conventional pneumatic nebulization sampling, the SCGD sampling method demonstrated a 100-fold sensitivity improvement for iodine determination, while Ca sensitivity was reduced by a factor of 70. The effect of operating parameters and reaction conditions on the signal intensities was investigated. Under optimized conditions, the iodine detection limit was as low as 0.9 pg g<small>⁻¹</small> for carbonate samples. Finally, the validity of the method was verified through the analysis of standard reference samples, actual carbonate rocks, and simulated samples. The results conclusively demonstrate that our developed method offers a simple, sensitive, and rapid approach for accurately measuring the I/Ca ratio in carbonate rocks, thereby facilitating broader application of the I/Ca indicator.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 3198-3206"},"PeriodicalIF":3.1,"publicationDate":"2024-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714072","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":"Magneto-electrical fusion enhancement of LIBS signals: a case of Al and Fe emission lines' characteristic analysis in soil","authors":"Zihan Yang, Mengyu Pang, Jincheng Ma, Yanru Zhao, Keqiang Yu and Yong He","doi":"10.1039/D4JA00223G","DOIUrl":"https://doi.org/10.1039/D4JA00223G","url":null,"abstract":"<p >Soil is a vital resource for human survival. In particular, aluminum (Al) and iron (Fe) metal elements in soil play significant roles in stabilizing soil organic matter. Therefore, the rapid and effective detection of Al and Fe elements in soil is imperative. Compared with conventional elemental detection techniques, laser-induced breakdown spectroscopy (LIBS) has emerged as a pivotal method for soil detection because of the advantages of simultaneous detection of multiple elements, rapidity and environmental friendliness. However, the LIBS signal of trace metal elements remains to be enhanced due to some influencing factors like the soil matrix effect. Hence, this study introduces a magneto-electrical fusion soil LIBS signal enhancement device, through an investigation into the impacts of magnetic field strength, energization, and magneto-electric fusion on the LIBS signals of Al and Fe in soil. Examining the single-factor effects of magnetic field strength and energization on soil LIBS signals, enhancements were observed in the spectral intensity (SI), signal to background ratio (SBR), plasma electronic temperature (PET), and plasma electronic density (PED) for soil Al and Fe elements compared to those observed with the unenhanced LIBS technique. According to the results of two-factor analysis of variance (ANOVA), the cost of the study and the safety of use, the appropriate magnetic field strength and energizing voltage were selected, respectively, to be 110 mT and 12 V. The magneto-electrical fusion LIBS signal enhancement device was designed based on the above results of the study in terms of operational reliability, ease of operation, safety and economy. It mainly included a base module, a support module and an enhancement module. For the designed device performance, validation was carried out in terms of parameters and applications, respectively. For parameter validation, the fusion enhancement device realized the enhancement of soil LIBS signals in 4 different areas. For application validation, the soils originating from 4 different regions were subjected to discriminant analysis. Comparative analysis with the original LIBS technique revealed significant enhancement in the performance of the soil origin discrimination model facilitated by the fusion enhancement device. This study provides support for the development of efficient techniques and equipment for soil element detection in farmland, as well as a theoretical basis for high-quality agricultural production.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 3094-3105"},"PeriodicalIF":3.1,"publicationDate":"2024-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714051","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":"A Gaussian spot overlap ablation model for prediction of aluminium alloy spectral peak intensity in high pulse repetition frequency LIBS","authors":"Dongming Qu, Bohao Su, Zhongshu Bai, Biye Liu, Xueying Jin, Guanyu Chen, Yuting Fu, Tingwen Gu, Guang Yang and Qingkai Li","doi":"10.1039/D4JA00298A","DOIUrl":"https://doi.org/10.1039/D4JA00298A","url":null,"abstract":"<p >The use of microjoule high pulse repetition frequency (PRF) lasers as excitation sources is an important direction in the miniaturisation of laser-induced breakdown spectroscopy (LIBS) instruments. However, high PRF LIBS is sensitive to experimental parameters, and the relationship between the experimental parameters and the spectral intensity of high PRF LIBS is less studied. In this work, we present a model based on Gaussian spot overlapping ablation with aluminium alloys as samples. After the index values have been collected in the non-motion state, the model derivation formula can be used to calculate the intensity of the spectral peaks under any proposed experimental parameters in the motion state. The experimental results show that the mean relative error (MRE) between the measured and predicted values of spectral peak intensity is ≤0.15 under different experimental parameters, and this result proves the validity of the model in predicting the spectral peak intensity. Meanwhile, we used 5 standard aluminium alloy samples to construct the standard curves of measured and predicted values under different experimental parameters. The experimental results show that the MRE between the measured and predicted values is ≤0.15, and the two standard curves fitted with the measured and predicted values have a high similarity with an average <em>R</em><small>²</small> ≥ 0.85. This study is expected to provide a universally applicable and efficient method for the quantitative analysis of high PRF LIBS in different application scenarios.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 1","pages":" 162-172"},"PeriodicalIF":3.1,"publicationDate":"2024-11-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142912589","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":"Investigation of direct simultaneous uranium isotopic determination and age dating of micrometer-sized uranium particles by laser ablation – multi-collector ICPMS†","authors":"Anne-Claire Humbert, Fabien Pointurier and Amélie Hubert","doi":"10.1039/D4JA00280F","DOIUrl":"https://doi.org/10.1039/D4JA00280F","url":null,"abstract":"<p >In this study, we demonstrate that it is possible to simultaneously determine accurate uranium <small>²³⁴</small>U and <small>²³⁵</small>U abundances and the date of purification (or “age”) of uranium oxide materials at the particle scale using laser ablation – multi-collector ICPMS coupling. The method was successfully applied to microparticles of uranium materials enriched at 5%, 85% and 90% and purified 70 years ago. The deviations from the reference age are, at most, respectively 6 years, 2 years and 1 month which is comparable to what can be obtained using the reference technique LG-SIMS. The precision of <small>²³⁵</small>U abundances and <small>²³⁴</small>U abundances, at the particle scale, was respectively between 0.11% and 1.95% and between 0.4% and 5% which is equivalent to or better than what was previously published for the analyses of depleted to moderately enriched materials by LA-ICPMS, showing that adding <small>²³⁰</small>Th determination doesn't degrade the determination of <small>²³⁴</small>U and <small>²³⁵</small>U abundances. Due to the small amount of material introduced into the ICPMS, μm-sized particle analysis by LA-ICPMS has the advantage of being less subject to laser-induced fractionation than bulk material analyses by LA-ICPMS. In contrast to the latter, a correction for uranium <em>versus</em> thorium fractionation can be applied based on the measurement of their relative sensitivities in standard solutions.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 3180-3189"},"PeriodicalIF":3.1,"publicationDate":"2024-11-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714070","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":"Applying standard addition to determine antimony isotopes in low-Sb samples using HG-MC-ICP-MS†","authors":"Honggang Zhu, Jian-Ming Zhu, Decan Tan, Zhuo Lu, Hongfei Liao and Yiwei Ma","doi":"10.1039/D4JA00333K","DOIUrl":"https://doi.org/10.1039/D4JA00333K","url":null,"abstract":"<p >The standard addition (SA) method has been successfully employed in measuring metal-stable isotopes in recent years. Here, utilizing hydride generator (HG)-multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS, Nu Plasma II and Neptune Plus), we evaluated the method's robustness through achieving high-precision <em>δ</em><small>¹²³</small>Sb(antimony) values (relative to NIST 3102a) in samples with more complex matrices and low-Sb concentrations. By using element doping (<small>^113/111</small>cadmium) coupled with sample-standard bracketing (SSB), a mass discrimination correction model was presented. The Sb isotope ratios of 30 geological reference materials (GRMs) were reported, in which the values of selected GRMs agreed well with previously published values. The SA method was then used to determine four of these with low-Sb samples. The analytical precision (2 standard deviations: 2SD) was found to mainly depend on the sample fraction (<em>f</em><small>_spl</small>) in the mixture, with the ideal mixing range recommended to be <em>f</em><small>_spl</small> ≥ 0.50 for single- and ≥ 0.45 for double SA when expected precision is ≤0.09‰ (2SD). The <em>δ</em><small>¹²³</small>Sb ratio calculated for basalt BCR-2 (Sb = 0.30 μg g<small>⁻¹</small>) was 0.28 ± 0.09‰, and together with the other four GRMs, it confirmed that accurate and precise Sb isotopes can be analyzed for samples with low-Sb using SA. Validating the measurement of Sb isotope composition in low-Sb samples with complex matrices by SA will expand the application of Sb isotopes in environmental, agricultural, life, Earth, and planetary sciences.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 3082-3093"},"PeriodicalIF":3.1,"publicationDate":"2024-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714050","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":"Automated detection of element-specific features in LIBS spectra","authors":"Zuzana Gajarska, Anna Faruzelová, Erik Képeš, David Prochazka, Pavel Pořízka, Jozef Kaiser, Hans Lohninger and Andreas Limbeck","doi":"10.1039/D4JA00247D","DOIUrl":"https://doi.org/10.1039/D4JA00247D","url":null,"abstract":"<p >This work introduces a novel semi-automatic approach to identify elemental lines in spectra obtained <em>via</em> laser-induced breakdown spectroscopy (LIBS). The algorithm is based on unique spectral fingerprints of individual elements that are configured into comb-like filters. The element-specific filters are then correlated with measured spectra for semi-supervised qualitative analysis of samples. Spectral variations are accommodated by adjusting the micro-parameters of the comb filter. This step ensures accurate results despite minor deviations from the instrument's ideal calibration due to instrumental fluctuations, <em>e.g.</em>, drift in spectral calibration or line broadening. Additionally, the algorithm can autonomously detect spectral interference regions, aiding the analyst in verifying spectral lines where such interference may occur. The paper presents a comprehensive overview of the algorithm and discusses the main concepts, parameters, optimization steps, and limitations using Echelle spectra of two standard reference materials with different complexity: borosilicate glass (NIST 1411) and low-alloyed steel (SUS1R). Furthermore, the transferability of the approach to different scenarios and real-life applications is demonstrated using a single-channel Czerny–Turner spectrum of an amalgam filling extracted from a hyperspectral image of a human tooth. A demo of the algorithm is publicly available for non-commercial purposes.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 3151-3161"},"PeriodicalIF":3.1,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://pubs.rsc.org/en/content/articlepdf/2024/ja/d4ja00247d?page=search","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714081","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":"Determination of boron isotopic compositions in five fractions of soil boron: traces of the environmental behavior of boron in soil†","authors":"Xuejun Chen, Qingcai Xu, Li Yan, Xiaodong Hao, Xiaochen Guan, Xiaopeng Han, Aide Sun, Zhiqun Chen, Lihua Liu and Zihao Zhu","doi":"10.1039/D4JA00286E","DOIUrl":"https://doi.org/10.1039/D4JA00286E","url":null,"abstract":"<p >Boron in soil can be divided into five fractions: readily soluble, carbonate-adsorbed, organically bound, adsorbed-bound and residual boron. Regarding differences in physicochemical properties, the fractions of soil boron affect the distribution and processes of boron and its isotopes in soil. A stepwise extraction for five fractions of soil boron was successfully established to reveal the isotopic behavior of boron in soils, which was performed to eliminate the isotope interference of neighboring forms in soil boron as much as possible. Ten soil samples were used to evaluate the proposed method. A large difference of 57‰ (−31.9‰ to +25.8‰) in the <em>δ</em><small>¹¹</small>B values occurred among the five fractions of soil boron. Residual boron had the highest content, which was hundreds of times greater than that in the other forms, and the lowest <em>δ</em><small>¹¹</small>B values, ranging from −31.9‰ to −24.5‰. Among the other four fractions, readily soluble boron had a relatively low content and the most positive <em>δ</em><small>¹¹</small>B values, adsorbed-bound boron had a relatively high content and less negative <em>δ</em><small>¹¹</small>B values, and carbonate-adsorbed boron had the lowest content. The relationship between the content and <em>δ</em><small>¹¹</small>B values revealed the scope of each fraction of soil boron, which may have resulted from the different processes of adsorption, transportation and weathering and the input of various provenances in the open soil medium. Further studies on the different types of soil influenced by different climates are expected to make important contributions to further knowledge of boron recycling in plant–soil systems with the proposed extraction method.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 3162-3170"},"PeriodicalIF":3.1,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714064","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":"A single-stage purification method for the precise determination of zirconium isotopic composition in geological samples by double spike MC-ICP-MS†","authors":"Lanping Feng, Chen Wang, Yan Han, Wen Zhang, Jing-Liang Guo, Lian Zhou and Zhaochu Hu","doi":"10.1039/D4JA00332B","DOIUrl":"https://doi.org/10.1039/D4JA00332B","url":null,"abstract":"<p >Interest in studying zirconium (Zr) stable isotopic fractionation in both low and high-temperature environments has increased significantly in recent years. Multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) is the preferred technique for stable Zr isotope analysis due to its low sample consumption and high precision. However, the multi-column separation steps required to remove interferences and meet the stringent matrix requirements for Zr isotopes during MC-ICP-MS testing typically make the sample preparation process time-consuming. Here, we present a new, simple, and efficient single-pass chromatographic exchange technique for the chemical isolation of Zr from complex sample matrices. This new separation protocol is based on DGA resin and consists of only three elution steps and two types of acid eluents (15 mL 7 mol L<small>⁻¹</small> HNO<small>₃</small> and 5 mL 3 mol L<small>⁻¹</small> HNO<small>₃</small> + 0.1 mol L<small>⁻¹</small> HF), which afford straightforward separation of Zr with high yield, good purity, and low blank levels. Zr isotope ratios were measured using Neptune Plus MC-ICP-MS with the <small>⁹¹</small>Zr–<small>⁹⁶</small>Zr double spike in combination with standard–sample bracketing for mass bias correction. The validity of the proposed method is demonstrated by analyzing eight geological reference materials (including BCR-2, which has an extremely high Mo content of ∼248 μg g<small>⁻¹</small>) with satisfactory results that are in good agreement with published values. Based on repeated analyses of pure standard solutions and geological reference materials, the long-term measurement reproducibility is better than ±0.048‰ for <em>δ</em><small>⁹⁴</small>Zr. Therefore, the proposed method can be used for the rapid and efficient determination of stable Zr isotope ratios in geological samples.</p>","PeriodicalId":81,"journal":{"name":"Journal of Analytical Atomic Spectrometry","volume":" 12","pages":" 3035-3047"},"PeriodicalIF":3.1,"publicationDate":"2024-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142714103","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}