Atomic Spectroscopy

The Atomic Spectroscopy (ISSN: 0195-5373, JCR Q2) is a peer-reviewed journal dedicated to the rapid publication of innovative research on fundamentals, instrumentation, methodologies and applications across all areas of atomic spectroscopy and inorganic mass spectrometry. All published articles are freely available online and no article processing charges (APC) are required for publication.

Editor-in-Chief: Prof. Xian-Hua Li
Executive Editor: Prof. Wei Guo
Associate Editors: Prof. Michael Dürr, Prof. Wei Hang, Prof. Zhaochu Hu

Call for papers:

1. Special issue: 14th LIBS 2026

Aim: This collection features contributions from "The 14th International Conference on Laser-Induced Breakdown Spectroscopy (LIBS 2026)"
Guest editors: Meirong Dong and Shunchun Yao
Submission deadline: 01 July 2026
Please select: 14th LIBS 2026 Special Issue upon submission.

2. Special issue: 2027 Early Career Analyst

Aim: To amplify emerging voices, foster academic exchange, and support the professional development of early-career researchers. AS welcomes original articles across all atomic spectroscopy and inorganic mass spectrometry fields
Guest editors: Jorge Pisonero Castro, Willis B. Jones, Yanbei Zhu, Anika Retzmann, and John Thomas Caulfield
Submission deadline: 15 October 2026
Please select: 2027 Early Career Analyst Special Issue upon submission.

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New Olivine Reference Materials for In Situ Oxygen Isotopic Determination

Juan Li, Shui-Jiong Wang*, Li-Guang Wu, Feng-Kun Li, Xian-Hua Li

DOI: 10.46770/AS.2026.0001

[Abstract] (3) [PDF 2.34 M] (20) [Supporting Information]

Abstract:
Olivine is a key mineral of mafic-ultramafic and metamorphic rocks. Oxygen isotopic composition of olivine has been widely used to decipher mantle processes, igneous differentiation, and fluid-rock interaction in metamorphic systems. Accurate in situ oxygen isotopic analysis of olivine by secondary ion mass spectrometry (SIMS) requires matrix-matched reference materials to correct instrumental mass fractionation and monitor the stability of instrument. In this study, we report two natural olivine reference materials, AOL (Fo: 91-97) and POL (Fo: 94-97), for in situ oxygen isotopic analysis. These samples exhibit homogeneous oxygen isotopic compositions, with a two-standard deviation of 0.33‰ (N = 105) and 0.37‰ (N = 105), respectively. The recommended δ1?O values, determined by laser fluorination isotope ratio mass spectrometry, are 5.52 ± 0.25‰ for AOL and 5.64 ± 0.13‰ for POL (all ± 2SD, N = 5). Combined with previously reported olivine standards, our results confirm that no significant matrix effects were observed within the forsterite (Fo) content range of Fo?? to Fo??, supporting the wide use of AOL and POL as reference materials for high?precision oxygen isotopic microanalysis.

Enhancing the Discriminative Power of LIBS for Uranium Slag Classification via Multi-Source Weighted Feature Fusion Strategy

Mengjia Zhang, Xiaoliang Liu*, Min Zhang, Chunyan Zou, Rong Hua, Xinglei Zhang, Debo Wu, Shaohua Sun, Zuoye Liu

DOI: 10.46770/AS.2026.029

[Abstract] (4) [PDF 10.65 M] (21)

Abstract:
Feature engineering is a critical step in addressing the “curse of dimensionality” and high noise levels inherent in laser-induced breakdown spectroscopy (LIBS) data to enable rapid and accurate classification. However, for complex matrices like uranium (U) slag, individual feature selection methods often struggle to capture the full spectrum of discriminative information, leading to suboptimal model robustness. To address this, a weighted feature fusion (WFF) strategy is proposed for the first time to achieve high-precision classification of U slag. This strategy generates a comprehensive importance metric by performing a weighted linear fusion of normalized scores derived from random forest (RF), least absolute shrinkage and selection operator (LASSO), and mutual information (MI). The influence of diverse weight configurations on support vector machine (SVM), linear discriminant analysis (LDA), and k-nearest neighbors (KNN) models was systematically investigated using LIBS spectra from 23 U slag samples. The results demonstrate that the WFF strategy effectively reconciles the complementary strengths of the baseline methods—leveraging the dominant discriminative power of RF, the sparse linear features of LASSO, and the nonlinear associations from MI. Under the optimal weight configuration (RF: LASSO: MI = 0.5: 0.2: 0.3), the LDA model achieved a peak F1-score of 97.09%, significantly outperforming the best single-method approach (RF-LDA, 94.15%). The proposed strategy exhibits superior generalization and successfully mitigates the adaptation limitations typically observed when specific models are paired with individual selection methods. This study provides a novel, flexible, and interpretable feature engineering solution, offering critical methodological support for the field-deployable monitoring and resource utilization of nuclear-related solid waste.

Infrared-heated Sample Introduction System to Enhance Transport Efficiency for Yeast Cell Analysis by Single Cell Inductively Coupled Plasma Mass Spectrometry

Zichao Zhou, Mirah J. Burgener, John Burgener, Diane Beauchemin*

DOI: 10.46770/AS.2026.071

[Abstract] (4) [PDF 718.59 K] (25) [Supporting Information]

Abstract:
Single cell inductively coupled plasma mass spectrometry (scICPMS) enables quantitative analysis of individual cells, providing access to cellular heterogeneity that is obscured in bulk analyses. However, its analytical performance is strongly constrained by sample introduction efficiency, particularly for biological cells whose transport behaviour differs from those of standard solutions and nanoparticles. In this work, an infrared (IR)–heated pneumatic sample introduction system based on a modified cyclonic spray chamber, where the aerosol is pre-evaporated without solvent removal prior to entering the plasma, was employed for scICPMS analysis of a Se-enriched Saccharomyces cerevisiae (yeast) certified reference material (SELM-1) while monitoring the number of detected cell events. Multivariate optimization of IR-heating temperature, nebulizer gas flow rate, sample uptake rate, and sampling position was conducted. At 150 °C and 5 μL min?1 uptake rate, the IR-heated system achieved a cell transport efficiency of 47 ± 6%, representing a substantial improvement compared with a conventional cyclonic spray chamber (1.1 ± 0.4%) and exceeding that of a commercial single cell introduction system (30 ± 3%). Detection limits of 100–120 ag per cell were obtained for both ??Se and ?2Se. The Se mass per cell determined by scICPMS (65–68 fg cell?1) is consistent with independent estimates derived from certified total Se concentration and bulk digestion measurements, confirming analytical accuracy. Cell lysis occurred at IR-heating temperatures above 220 °C, emphasizing the necessity of optimization using cell-based matrices. Overall, this study demonstrates that controlled IR-heated sample introduction significantly enhances transport efficiency and enables reliable Se quantification in cells without requiring independent transport efficiency calibration.

A Review of Tandem Quadrupole ICP-MS/MS for the Determination of Radionuclides in Environmental, Biological, and Nuclear Waste Samples

Feng Zhang, Chenyang Peng, Shan Xing*, Jing Lin, Hao Wang, Jie Chen, Xinyu Du, Yiman Lu, Jiang Sun, Haomiao Ma, Cancan Chen, Weichao Zhang*

DOI: 10.46770/AS.2025.286

[Abstract] (22) [PDF 5.57 M] (310)

Abstract:
Long half-life natural and artificial radionuclides have been paid great attention in the environment, geochronology, nuclear accidents, as well as the operation of nuclear facilities for over a decade. However, the rapid and accurate quantification of these ultra-trace level (fg or mBq) radionuclides has become a formidable challenge nowadays. A triple-quadrupole inductively coupled plasma mass spectrometry (ICP-MS) equipped with a collision reaction cell (CRC), namely ICP-MS/MS, is a valuable technique for rapid and sensitive analysis of ultra-trace level radionuclides in various kinds of samples. This article provides a comprehensive review and critical comparison of published analytical methods for ultra-trace level radionuclides in environmental, biological and nuclear waste samples. The methods of sample pre-treatment, valence state adjustment, chemical separation of radionuclides, and ICP-MS/MS measurement are systematically described and discussed. Importantly, the advantages and limitations of the collision reaction cell (CRC) technology on the removal of interferences and the radionuclide measurement are comprehensively summarized. In addition, the article also explores advancements in automated separation and measurement methodologies for radionuclides.

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Editorial

Minchao Cui Honored with Atomic Spectroscopy 2026 Best Paper Award

Ming Li, Wei Guo*

2026,47(2),175-178,

DOI: 10.46770/AS.2026.007

[Abstract] (18) [PDF 1.43 M] (220)

Abstract:

Article

A Correlative Microanalytical Protocol Integrating FIB-SEM, TOF-SIMS, AFM-IR, and NanoSIMS for Mars-analog Basalt

Jingbo Nan*, Jun-Heng Wang, Yilin Wang, Zongjun Yin*

2026,47(2),179-186,

DOI: 10.46770/AS.2025.203

[Abstract] (32) [PDF 9.14 M] (441) [Supporting Information]

Abstract:
The search for carbonaceous matter in Martian rocks is the key to evaluating their potential biosignatures. Studying carbonaceous matter preserved within Earth’s basaltic analogs provides critical insights into the mineral–organic interactions that may also occur on Mars. To characterize molecular-level chemical information of carbonaceous matter, correlative surface-sensitive approaches such as Focused Ion Beam Scanning Electron Microscopy (FIB-SEM), Secondary Ion Mass Spectrometry (SIMS), and Atomic Force Microscopy Infrared Spectroscopy (AFM-IR) are employed. In this study, we developed a correlative microanalytical protocol starting with the ex-situ FIB-SEM lift-out, in which lamellae from a Mars-analog basalt were transferred onto a clean silicon substrate using a glass-needle nanomanipulator. The lamellae were then analyzed sequentially by Time-of-Flight SIMS (TOF-SIMS), AFM-IR, and Nano-scale Secondary Ion Mass Spectrometry (NanoSIMS). Specifically, spatially and chemically co-registered TOF-SIMS, AFM-IR, and NanoSIMS analyses provided complementary insights into the same region, correlating organic distribution, molecular vibrations, and isotopic compositions within mineral matrices. Together, these results demonstrate that the established correlative microanalytical protocol in this study effectively integrates sample preparation and multi-modal surface analyses, providing a framework for investigating planetary materials and future Mars samples.

Multielement Analysis of Petroleum Products Using the Promising Technique of Optical Emission Spectrometry with Two-Jet Plasma

N. A. Orlov, A. V. Volzhenin, N. S. Medvedev *

2026,47(2),187-194,

DOI: 10.46770/AS.2025.235

[Abstract] (23) [PDF 1.55 M] (221) [Supporting Information]

Abstract:
The main analytical challenges during multi-element analysis of petroleum product are related to the difficulties of sample introduction into the excitation and ionization sources and significant spectral matrix effects. The method of analysis of samples of the petroleum products by two-jet plasma optical emission spectrometry (TJP-OES) is proposed. The innovation lies primarily in application of TJP-OES for viscous organic samples (motor oil and heavy fuel oil), associated sample preparation strategy, optimized drying protocol and the demonstration of performance for a wide range of elements in challenging matrices. The proposed approach to sample preparation and measurement is dilution of the samples by organic solvent (kerosene) with subsequent drying on the graphite powder under IR lamp and TJP-OES analysis of mixture of graphite powder and the analyzed sample. This approach allows perform analysis of the petroleum products without the use of non-standard sample injection systems into atomization sources or labor-intensive sample preparation procedures. The limits of detection (LODs) of the analytes ranged from 10-6 to 10-3 % wt for 29 trace elements are achieved. Recovery values were from 70 to 130 % are obtained during ?spike? experiment. Accuracy of proposed method was confirmed by comparison the results of analysis of the petroleum products by TJP-OES and optical emission spectrometry with inductively coupled plasma (ICP-OES). Thus, the applicability of the TJP-OES method for multi-element analysis of samples of the petroleum product is demonstrated.

Research on the Evolutionary Law of LIBS Spectra Under Asymmetric Spatial Effects

Jiangfei Yang, Xiaomei Lin*, Jingjun Lin*, Yutao Huang, Jiahan Li

2026,47(2),195-205,

DOI: 10.46770/AS.2026.002

[Abstract] (17) [PDF 8.26 M] (201)

Abstract:
Studying the asymmetric spatial effects of LIBS is crucial for enhancing defect spectral detection accuracy in metal additive manufacturing (AM). A parallel wall cavity was used to simulate asymmetric conditions of crack defects, with the distance between the ablation point and the left wall (DAPLW) systematically varied. Experimental conditions were established for both symmetric (DAPLW = 7 mm) and asymmetric (DAPLW = 1-6 mm) configurations to study the spatiotemporal distribution of plasma under different spatial effects. Results revealed that asymmetric spatial effects significantly influenced the spatiotemporal distribution of plasma, causing more complex fluctuations in spectral intensity and changes in plasma morphology. Under asymmetric spatial effects, plasma showed enhanced spectral intensity at various acquisition delay times (e.g., 7 μs and 13 μs at DAPLW = 4 mm). However, spectral intensity fluctuations also increased, indicated by a higher relative standard deviation (RSD). Additionally, the study examined the impact of various point-wall distance constraints on the plasma’s time evolution and observed a significant shift in the core position of plasma (CPP) (10-22 μs). During this process, the near roundness ratio of plasma (NRRP) value exhibited significant changes (10-13 μs), particularly when the DAPLW was 1 mm. It decreased from a stable value of 0.8 to below 0.1, reflecting notable morphological changes. In contrast, the symmetric space effect and unconstrained plasma behavior remained stable, with spectral intensity changes showing clear regularity and only relatively small alterations in plasma morphology. This indicated that the delay time of the acquisition system is crucial for using LIBS technology to detect defects in metal AM components with asymmetric cavities. Therefore, understanding asymmetric cavity effects enhances plasma behavior knowledge and provides new guidance for improving defect detection accuracy.

Using Integrated Single-Particle ICP-MS and XANES to Reveal in Situ Speciation Transformation of Silver Nanoparticles in Cellular Environments

Yuyuan Peng#, Meng Wang#, Tingfeng Zhang, Yuchi Yao, Hao Fang, Jinke Liu, Xu Wang, Lingna Zheng, Xueqing Xing, Meng Wang, Xuesong Feng*, Bing Wang*, Weiyue Feng

2026,47(2),206-214,

DOI: 10.46770/AS.2026.005

[Abstract] (32) [PDF 3.16 M] (235)

Abstract:
Despite significant advances in analytical techniques, quantitative in situ characterization of silver nanoparticles (AgNPs) in biological systems—particularly regarding the dynamic balance between ionic and particulate silver—remains a major challenge. This study reveals that the dissolution behavior of AgNPs strongly depends on particle size and the surrounding biological medium. For example, 50?nm PVP-coated AgNPs exhibited significantly greater dissolution than 75?nm particles in both aqueous solution and DMEM medium. In aqueous environments, over 95% of silver from 50?nm NPs existed as ionic silver, compared to only about 38% from 75?nm NPs. In DMEM, a dynamic equilibrium was established, characterized by the concurrent dissolution of primary particles and the formation of new particulate species, leading to continuous fluctuations in particle number and ionic silver concentration over time. After 48?h of incubation, the released ionic silver accounted for approximately 38.4% from 50?nm particles and 26.2% from 75?nm particles. Chemical speciation analysis via synchrotron radiation-based X-ray absorption near edge structure (XANES)spectroscopy further demonstrated that intracellular silver underwent progressive transformation from the original AgNPs into Ag?S nanoparticles, reaching a conversion ratio of 61.9% at 12?h, along with minor formation of AgCl. This transformation was closely linked to the acidic intracellular milieu and interactions with biological ligands. Although no marked cytotoxicity was observed within the first 24?h of exposure, the gradual intracellular accumulation of transformation products, particularly Ag?S nanoparticles, eventually led tomild cytotoxic effects. These findings collectively underscore that the biological impact of AgNPs is fundamentally governed by their intracellular chemical transformation dynamics.

Robust Modeling and Feature Visualization for Small-Sample Soil LIBS Quantitative Analysis Using CNN

Weinan Zheng, Xun Gao*, Hailong Yu, Yinping Dou, Qiuyun Wang*

2026,47(2),215-227,

DOI: 10.46770/AS.2026.008

[Abstract] (22) [PDF 6.17 M] (181) [Supporting Information]

Abstract:
Rapid and precise determination of elemental content in soil is significant for precision agriculture and saline-alkali land remediation. Although Laser-Induced Breakdown Spectroscopy (LIBS) offers advantages of rapid, multi-element simultaneous detection, it is prone to issues of insufficient quantitative accuracy and model overfitting under conditions of complex soil matrix interference and small sample modeling, thereby limiting the model's generalization capability. To overcome these limitations, this study developed a quantitative regression model based on a 1-Dimensional Convolutional Neural Network (1D-CNN). This model directly utilises raw LIBS spectra as input, automatically extracting multi-scale spectral features to predict the contents of Ca, Mg, and Na in soil. 10-fold cross-validation results demonstrate that the CNN model performs exceptionally well across both high and low concentration ranges. For high-concentration samples, R2 ≥ 0.972, while for low-concentration samples, R2 ≥ 0.98. This confirms the model's high accuracy and strong generalization capability in quantitative LIBS analysis of small samples. Its overall performance significantly outperforms comparison models such as Random Forest (RF) and Backpropagation Neural Network (BPNN). Further integration with Gradient-weighted Class Activation Mapping (Grad-CAM) enables feature visualisation, confirming that the model's focus regions align with element-specific spectral lines, indicating physical plausibility. This study provides a high-precision, interpretable modeling approach for quantitative LIBS analysis of small-sample native soils.

Assessing Apatite Reference Materials and Common Pb Correction for In Situ U–Pb Geochronology

Fen Xiao, Yueheng Yang*, Lei Xu, Shitou Wu, Chao Huang, Hao Wang, Liewen Xie, Jinhui Yang, Fuyuan Wu

2026,47(2),228-242,

DOI: 10.46770/AS.2026.026

[Abstract] (29) [PDF 10.38 M] (193) [Supporting Information]

Abstract:
Apatite is a common accessory mineral in U–Pb geochronology and provides valuable constraints on magmatic evolution, orogenic processes, and basin thermal histories. However, its generally low U concentrations and high common Pb contents have limited its broader application. The long-term stability of matrix-matched reference materials and the reliability of common Pb correction are critical factors controlling data quality. Here, we present in situ U–Pb data obtained by LA–SF–ICP–MS for a suite of widely used apatite reference materials, including NW-1, McClure Mountain, Emerald, Durango, Otter Lake, MAD, AP1 and AP2, covering an age range from ~1157 to 32 Ma. Their long-term stability and homogeneity are evaluated based on analytical results over the past five years. Using real reference materials with contrasting common Pb contents, we further assess the influence of common Pb correction using anchored initial Pb compositions with propagated uncertainties. The results show that U–Pb ages for most reference materials are consistent with ID–TIMS certified values or previously published data, with deviations ≤2%, demonstrating their long-term analytical stability. NW-1, characterized by high U concentrations and the lowest common Pb, is recommended as primary reference material, whereas AP1 and AP2 are better suited as secondary reference materials. This study confirms the robustness of the established analytical protocol, clarifies the appropriate application of different apatite reference materials, and provides a practical framework for matrix matching and multi–reference material cross-calibration in in situ apatite U–Pb geochronology.

Infrared and Raman Spectroscopy of Chang'e-5 Samples Reveal Lunar Magmatic Evolution

Xuesen Xu*, Tangying Tong, Shoulong Huang, Xizhu Wang, Helen L. Grant, Hailin Wang, Rong Shu*

2026,47(2),243-252,

DOI: 10.46770/AS.2026.010

[Abstract] (19) [PDF 6.84 M] (188)

Abstract:
The Fo content of olivine is a key parameter for understanding the processes of lunar magmatic evolution. However, limited by detection methods, obtaining the Fo content of olivine on the lunar surface has long been confronted with numerous challenges. Traditional methods such as Electron Probe Microanalysis (EPMA) require polishing and sample preparation, making them unsuitable for future in-situ exploration missions. This study employed microscopic infrared spectroscopy, microscopic Raman spectroscopy, and Energy Dispersive Spectroscopy (EDS) to conduct compositional analysis on olivine grains in Chang'e-5 (CE-5) lunar soil samples. We verified the reliability of the infrared spectroscopy Reststrahlen Band (RB) characteristic peak position method and the Raman spectroscopy main peak shift method for the quantitative inversion of olivine Fo content by comparative analysis. Furthermore, the Fo contents derived from the three analytical techniques exhibit systematic deviations, reflecting differences in their respective technical principles and information depths. The low Fo contents suggest that the basalts at the CE-5 landing site have undergone intense crystallization differentiation, while the coexistence of olivines with distinct compositions may stem from magma mixing events. Not only does this study deepen the understanding of the magmatic history of CE-5 samples, but the spectroscopic methods validated herein also enable the systematic acquisition of olivine Fo contents on the lunar surface during the future Chang'e-7 mission, through a combination of orbiter-based infrared surveys and lander-based high-precision Raman detection, thereby providing a novel approach for in-depth studies of lunar magmatic evolution.

Potential Stibnite Reference Materials for in situ S and Sb Isotope measurement by LA-MC-ICP-MS

Jiaxin Zhang, Kejun Hou*, Ran Wang, Yutian He, Tao Yang, Xiaowei Gao, Mengqi Zhang

2026,47(2),253-262,

DOI: 10.46770/AS.2026.027

[Abstract] (20) [PDF 1.63 M] (162) [Supporting Information]

Abstract:
Stibnite is the principal sulfide mineral and the most important ore mineral in antimony deposits worldwide. In situ S and Sb isotope analyses of stibnite are crucial for investigating the genesis of antimony deposits and for deciphering detailed mineralization processes. To obtain reliable in-situ isotopic data, matrix-matched reference materials are essential for correcting instrumental mass fractionation. In this study, two natural stibnite samples (WX34-80 and KKY) were characterized on the basis of their elemental and isotopic compositions. The results demonstrate that both samples are homogeneous in terms of S and Sb contents, as well as their isotopic signatures, and exhibit significantly distinct sulfur isotopic compositions, rendering them highly suitable reference standards for in situ Sb and S isotope analyse using LA-MC-ICP-MS. Based on IRMS measurements, the recommended δ3?SV-CDT values are ?2.17 ± 0.29‰ (2SD, n = 18) for WX34-80 and 10.63 ± 0.38‰ (2SD, n = 18) for KKY. Correspondingly, SN-MC-ICP-MS analyses yield recommended δ123Sbspex values of ?0.33 ± 0.07‰ (2SD, n = 8) for WX34-80 and ?0.29 ± 0.05‰ (2SD, n = 8) for KKY.

Classification of Healthy and Diseased Bangla Betel Leaves (Piper betel L.) using Laser-Induced Breakdown Spectroscopy and k-Nearest Neighbors Modeling

Madhumita Patel, Neha Sharma*, Sandeep Kumar*, Yonghoon Lee, V. K. Singh, R. K. Singh, S. B. Singh, S. V. Dwived, A. C. Mishra, Piyush K. Rai, Vivek K. Singh*

2026,47(2),263-273,

DOI: 10.46770/AS.2026.009

[Abstract] (83) [PDF 5.91 M] (223)

Abstract:
Betel leaf (Piper betel L.) is highly susceptible to severe fungal and bacterial diseases such as leaf rot, collar rot, anthracnose (leaf spot), and bacterial leaf spot, which cause significant yield losses through rotting, spotting, and wilting. Its rich phytochemistry underpins various medicinal properties, while its production supports rural economies in Asia. However, diseases and perishability pose serious challenges to yield and profitability, necessitating improved agronomic practices, disease management, and post-harvest handling to sustain and enhance its global economic contribution. Effective disease management therefore requires early integration of cultural practices along with fungicidal and bactericidal treatments. In the present study, laser-induced breakdown spectroscopy (LIBS) coupled with k-nearest neighbors (KNN) modeling was employed to discriminate between healthy and diseased betel leaves. The discriminative potential of nineteen LIBS emission peaks was evaluated using an interclass distance approach. Among these, the Mg II (279 nm) and Na I (588 nm) emission peaks were identified as the most effective variables for classification. One-dimensional KNN models developed using the spectral intensities of Mg II and Na I achieved classification accuracies of 92% and 96%, respectively. This approach demonstrates a cost-effective and time-efficient alternative to conventional elemental analysis techniques, enabling rapid, field-deployable analysis with minimal sample preparation.

Natural Garnet Reference Materials for the Electron Microprobe Flank Method to Determine the Fe3+/ΣFe of Unknown Garnets

Wen-Tan Xu Di-Cheng Zhu*, Qing Wang, Liang-Liang Zhang, Jin-Cheng Xie, Ze Liu, Si-Hua Yuan

2026,47(2),274-283,

DOI: 10.46770/AS.2026.028

[Abstract] (11) [PDF 2.28 M] (115) [Supporting Information]

Extending Sequential Leaching Approaches to Stable Sr Isotopes in Carbonate Reference Materials

Jena Jeong*, Seung-Gu Lee, Youngsook Huh*

2026,47(2),284-294,

DOI: 10.46770/AS.2026.012

[Abstract] (19) [PDF 2.05 M] (132) [Supporting Information]

Abstract:
Reliable Sr isotope analysis of carbonate rocks requires effective separation of non-carbonate phases that can bias both radiogenic (R(87Sr/86Sr)) and stable (δ88Sr/86SrSRM987) isotope measurements. While sequential leaching has been evaluated using the R(87Sr/86Sr), the behavior of δ88Sr/86SrSRM987 during this process remains poorly constrained. Here, we systematically investigate the evolution of both radiogenic and stable Sr isotopes across sequential leaching steps in three carbonate reference materials, JLs-1, JDo-1, and NIST SRM 1d. This study reports new δ88Sr/86SrSRM987 data for individual leaching fractions of carbonate reference materials and provides the first sequential leaching–based Sr isotope dataset for NIST SRM 1d, for which both radiogenic and stable Sr isotope data have previously been limited. Early leaching fractions are dominated by surface-adsorbed and exchangeable Sr, whereas later fractions reflect contributions from clay minerals, both of which produce isotopic signatures distinct from primary carbonate phases. Only intermediate fractions yield reproducible Sr isotope compositions representative of primary carbonate minerals. The R(87Sr/86Sr) values obtained from bulk leaching differ from those of the intermediate fractions by more than analytical precision, whereas smaller but detectable effects (~0.03‰) are observed for δ88Sr/86SrSRM987, especially in clay-rich samples. Applying the carbonate-dominated leaching range, representative values of carbonate reference materials are obtained with R(87Sr/86Sr) of 0.707783±0.000028, 0.707386±0.000028, and 0.708008±0.000028, and δ88Sr/86SrSRM987 of 0.252±0.035‰, 0.256±0.035‰, and 0.325±0.035‰ for JLs-1, JDo-1 and SRM 1d, respectively (2SD). These results demonstrate that not only R(87Sr/86Sr) but also δ88Sr/86SrSRM987 are sensitive to phase-specific Sr released during leaching and highlight the necessity of accurate pretreatment for Sr isotope analysis. The dataset and analytical framework presented here expand the application of sequential leaching from Sr isotopes and improve the utility of carbonate reference materials for high-precision isotope studies.

Ultra-sensitive Detection of Chlorine in Air by Using a Miniaturized Optical Emission Spectrometer with Absorption-Headspace Sampling

Peng Zhao, Meng Zhang, Kai Li*, Xiandeng Hou, Hui Yin, Peng Wu, Xiaoming Jiang*

2026,47(2),295-302,

DOI: 10.46770/AS.2026.030

[Abstract] (14) [PDF 5.81 M] (111) [Supporting Information]

Abstract:
Chlorine is a highly toxic and hazardous gas, which poses severe risks to environmental safety and occupational health even at low concentrations. Thus, highly sensitive and rapid detection of chlorine at trace levels is essential for air quality monitoring in laboratories, factories, and emergency sites, etc. Herein, a miniaturized optical emission spectrometer was constructed for ultra-sensitive detection of chlorine in air, with absorption-headspace injection. Chlorine gas was first absorbed in a potassium hydroxide solution and subsequently released as molecular Cl2 by a redox reaction with acidic potassium permanganate. The liberated chlorine was accumulated in the sealed headspace vial, and then rapidly transported to the discharge microplasma for subsequent excitation, in which characteristic optical emission of Cl at 837.59 nm was observed and recorded for quantification. Under the selected experimental conditions, a limit of detection of 0.01 ppm (0.03 mg/m3) was achieved, with a relative standard deviation of 3.8% (1 ppm, 2.95 mg/m3, n = 9), meeting the requirements for chlorine gas detection specified in a China’s national standard GB 11984–2024. It was successfully applied for analysis of certified reference materials and real air samples, confirming its accuracy and applicability. Owing to the advantages of high sensitivity, wide linear range, simple operation, and compact design, the proposed method and instrument would be promising for potential on-site detection and monitoring of chlorine in various chlorine operation related scenarios.

Reduction of Matrix Effect and Volatilization Loss for Iodine Detection in Marine Carbonates by NH4HF2 digestion ICP-MS

Mingying Liu, Weipeng Yao, Yan Wu, Tao Luo, Zhaochu Hu, Lanlan Jin, Shenghong Hu, Wei Guo*

2026,47(2),303-308,

DOI: 10.46770/AS.2026.006

[Abstract] (6) [PDF 623.85 K] (87) [Supporting Information]

Abstract:
As a valid seawater oxygen proxies, trace iodine in marine carbonates is crucial for reconstructing the redox conditions of the paleoceanography. Although highly sensitive inductively coupled plasma-mass spectrometry (ICP-MS) is often used for the determination of iodine, the accurately determining trace iodine of marine carbonates remains challenging due to its high volatility loss during the sample digestion and the matrix effect of coexisting high-calcium (Ca) in ICP-MS analysis. In this study, an ammonium bifluoride (NH4HF2) sample digestion ICP-MS method was evaluated for analyzing sub-μg/g levels of I in marine carbonate rocks. Results show that more than 97% of the target iodine can be well retained in the digestion solution, while simultaneously achieving the removal of the coexisting calcium matrix (over 86% of the calcium remains in the residue). The limit of detection (LOD, 3 sigma) the established method is 0.024 μg g-1 (taken into 250-fold dilution) with the relative standard deviation (RSD, N=5) ranging from 3.1 % to 8.0 %. The proposed method was applied to determination of I in a series of carbonate rock reference materials (RMs) and the satisfactory results (recovery, 87-104%) indicate that it has great potential for the determination of trace level I in various marine carbonate rocks.

Determination of Trace Copper in Biological Samples by On-line Chemical Vapor Generation-Atomic Fluorescence Spectrometry

Liang He, Xiaofan Zhu, Li Wu, Xiandeng Hou*

, DOI: 10.46770/AS.2008.03.004

[Abstract] (523) [PDF 146.88 K] (3855)

Abstract:
On-line chemical vapor generation atomic fluorescence spectrometry (CVG-AFS) was, for the first time, used to determine trace copper in biological samples by merging acidified sample solution with potassium tetrahydroborate aqueous solution in the presence of micro-amounts of 1,10-phenanthroline. Nitric acid, for both sample digestion and chemical vapor generation, was used as the acid medium. CVG conditions and instrumental parameters were optimized for the best CVG efficiency, good gas/liquid separation, and efficient atomization/excitation. Under the optimized conditions, a limit of detection of 4 ng mL(-1) was obtained for copper, with a linear dynamic range of over three orders of magnitude. The proposed method was successfully applied to the determination of copper in biological certified reference materials.

Rapid Determination of Chemical Oxygen Demand by Flame AAS Based on Flow Injection On-line Ultrasound- assisted Digestion and Manganese Speciation Separation

Zhi-Qi Zhang*, Hong-Tao Yan, Lin Yue

, DOI: 10.46770/AS.2004.04.006

[Abstract] (481) [PDF 86.02 K] (3720)

Abstract:
A rapid, sensitive, and cost-effective method was developed for the determination of trace mercury in water samples by on-line coupling of flow injection (FI) sorption preconcentration with oxidative elution to cold vapor atomic fluorescence spectrometry (CV-AFS). race Hg(II) in aqueous solution was preconcentrated by on-line formation of mercury diethyldithiocarbamate complex (Hg-DDTC) and adsorption of the resulting neutral complex on the inner walls of a PTFE knotted reactor (KR). A mixture of 16% (v/v) HCl and 10% (v/v) H2O2 was used as the eluent to remove the adsorbed Hg-DDTC from the KR, then convert on-line the Hg-DDTC into Hg(II) prior to its reduction to elemental mercury by KBH4 for subsequent on-line CV-AFS detection. The tolerable concentrations of Cd(II) As(Ill) Se(IV) Fe(III), Co(II), Ni(II), and Cu(II) and Cu(II) for the determination of 0.1 mug L-I Hg(II) were 0.1, 10, 0.1, 0.1, 0.7, 1, 0.3, and 0.2 mg L-1, respectively. With a sample loading flow rate of 3.1 mL, min(-1) for a 60-s preconcentration, a detection limit (3sigma) of 4.4 ng L-I was achieved at a sample throughput of 36 samples h(-1). The precision (RSD, n = 11) was 1.7% at the 1 0, 1-mug L-1 Hg (11) level. The method was successfully applied to the determination of mercury in a certified reference material, GBW(E) 080392, and a number of local natural water samples.

Determination of Cadmium at the Nanogram per Liter Level in Seawater by Graphite Furnace AAS Using Cloud Point Extraction

Chun-gang Yuan, Gui-bin Jiang*, Ya-qi Cai, Bin He, Jing-fu Liu

, DOI: 10.46770/AS.2004.04.003

[Abstract] (470) [PDF 99.16 K] (4042)

Abstract:
A method based on?cloud?point?extraction?was developed to determine?cadmium?at?the?nanogram?per?liter?level?in?sea-water?by?graphite?furnace?atomic absorption spectrometry. Diethyldithiocarbamate (DDTC) was used as?the?chelating reagent to form Cd-DDTC complex; Triton X-114 was added as?the?surfactant.?The?parameters affecting sensitivity and?extraction?efficiency (i.e., pH?of?the?solution, concentration?of?DDTC and Triton X-114, equilibration temperature, and centrifugation time) were evaluated and optimized. Under?the?optimum conditions, a preconcentration factor?of?51.6 was obtained for a 20-ml, water sample.?The?detection limit was as low as 2.0 ng L-1 and?the?analytical curve was linear?in?the?10.0-200.0 ng L-1 range with satisfactory precision (RSD < 4.7%).?The?proposed method was successfully applied to?the?trace?determination?of?cadmium?in?seawater.

Development and Validation Method for the Determination of Rare Earth Impurities in High Purity Neodymium Oxide by ICP-MS

Man He, Bin Hu*, Zucheng Jiang, Yan Zeng

, DOI: 10.46770/AS.2004.01.002

[Abstract] (499) [PDF 154.90 K] (3899)

Abstract:
The analytical procedure for the determination of trace rare earth impurities in high purity neodymium oxide (Nd2O3) by ICP-MS is described. The effect of ICP-MS operating parameters on the REO(H)(+)/RE+ production ratio was studied in detail, and the optimal ICP operating conditions were established. In this context, the relationship between REO(H)(+)/RE+ production ratio and the bond strength of the rare earth oxides is also discussed briefly. For the correction of the spectral interference induced by the matrix (neodymium), a simple correction equation was used for correcting the interferences of the polyatomic ions NdO+ and NdOH+ with Tb-159 and Ho-165. The proposed method was applied to the determination of trace rare earth impurities in high purity Nd2O3\, and the analytical results were in good agreement with the recommended reference values.

Multielement Analysis of Alkaline-Resistant Glass and Basalt Glass Fibers Using Laser Ablation ICP-MS: A Useful Tool in Technical Textile Quality Control

J. Su. Becker, C. Pickhardt, N. Hoffmann, H. H?cker, J. Sa. Becker*

, DOI: 10.46770/AS.2002.01.001

[Abstract] (613) [PDF 135.56 K] (4308)

Abstract:
A powerful multielement analytical technique using laser ablation Inductively coupled plasma source mass spectrometry (LA-ICP-MS) for the sensitive determination of trace impurities in thin glass filaments, used as reinforcing material in the construction industry, was developed. The trace analysis was carried out directly on very thin solid strands (without any sample preparation steps) by LA-ICP-MS whereby a bundle of thin glass fibers (with a filament diameter of about 10 - 20 mum) was fixed on a thin, special tape of a target holder. The fibers were ablated in the ablation chamber with the aid of a commercial laser ablation system using a Nd-YAG laser at a wavelength of 266 nm). In order to verify the trace analytical data, the ablated T-glass fibers were analyzed using a quadrupole (LA-ICP-QMS) and double-focusing sector field mass spectrometer (LA-ICP-SFMS). The detection limits of the trace elements in glass fibers using the LA-ICP-MS with a quadrupole analyzer were in the sub mug g(-1) range, whereas using a sector,field mass spectrometer (LA-ICP-SFMS) the detection limits could be Improved by 3-4 orders of magnitude down to the low and sub ng g(-1) range. The multielement trace analytical method, developed for high-purity glass fibers, was applied to the determination of chemical composition on thin alkati-resistant glass and basalt fibers with finishing additives used in fine concrete for the building industry. The analytical results were quantified using standard reference materials (SRMs) of glass matrix, such as the NIST 612 glass SRM and the basalt geological reference glasses, KL-2G and ML3B-G, for the trace analysis of basalt glass fibers. The experimentally determined relative sensitivity coefficients (RSC) in LA-ICP-MS for both SRMs varied between 0.2 and 3 for most of the elements. An increase of the relative sensitivity coefficients was observed with increasing mass. The relative standard deviation (RSD) of most elements (N = 3) was T between 2 and 10%. The results of the trace element concentrations by LA-ICP-MS using different instrumentation are in good agreement.

On-line Ion Exchange Preconcentration in a Sequential Injection Lab-on-valve Microsystem Incorporating a Renewable Column With ETAAS for the Trace Level Determination of Bismuth in Urine and River Sediment

Jianhua Wang, Elo Harald Hansen*

, DOI: 10.46770/AS.2001.03.003

[Abstract] (400) [PDF 167.98 K] (3583)

Abstract:
A?sequential?injection?system?for?on-line?ion exchange separation and?preconcentration?of trace level amounts of metal ions with ensuing detection by electrothermal atomic absorption spectrometry (ETAAS) is described. Based on the use of?a?renewable microcolumn incorporated within an integrated lab-on-valve microsystem, the?column?is initially loaded with?a?defined volume of beads of an SP Sephadex C-25 cation exchange resin. After having been exposed to?a?metered amount of sample solution, the loaded bead suspension is precisely manipulated within the valve to allow reproducible elution of the retained analyte by 30 muL nitric acid (1: 16,v/v) which, via air segmentation, are then transported into the graphite tube for quantification. The content of the used?column?is afterwards discarded and new?column?material is aspirated for the next run. The ETAAS determination is performed in parallel with the?preconcentration?process of the ensuing sample. The performance of the?system?is demonstrated for the determination of bismuth. With 2.4-mL sample loading, an enrichment factor of 33.4,?a?detection limit of 27 ng 1:1, along with?a?sampling frequency of 10 h(-1) was obtained. The relative standard deviation was 2.3% for the determination of 2.0 mg 1:1 Bi (n = 7). The procedure was validated by determination of bismuth in?a?certified reference material CRM 320 (river sediment) and by bismuth spike recoveries in two human urine samples.

A Sequential Injection On-Line Column Preconcentration System for Electrothermal AAS Determination of Thallium in Geochemical Samples

Zhang-Run Xu, Shu-Kun Xu, Zhao-Lun Fang*

, DOI: 10.46770/AS.2000.01.004

[Abstract] (392) [PDF 116.38 K] (3477)

Abstract:
A?sequential?injection?system?for?on-line?sorbent extraction?preconcentration?in electrothermal atomic absorption spectroscopy was developed for the determination of trace thallium in geochemical samples. The TlBr4-1 complex was adsorbed on?a?20-mu L micro-column?(located at the tip of the furnace sampling probe) packed with XAD-8 resin. After sequentially aspirating separate zones of acetone, rinsing acid, and sample (pretreated with bromine) into?a?2.5-m long, 1-mm i.d. holding coil, the flow was reversed and directed to the?column. Sample loading, analyte adsorption,?column?rinsing and analyte elution were achieved within?a?single reversed syringe stroke. The adsorbed analyte was eluted into the furnace with 50 mu L acetone. Mutual mixing between sample, rinsing acid, and eluent were prevented by separating the zones with small air segments during metering. Tightening of?column?packing was avoided by?a?slight back-suction through the?column?after each operational cycle. With 1-mL sample loading, an enrichment factor of 15 was obtained with?a?detection limit of 18 ng/L thallium (3 sigma).?A?precision of 2.4% RSD (n=11, 4 μ g/L) and?a?sampling frequency of 11/hour were achieved. The method was applied to the analysis of geochemical samples. The results were in good agreement with the certified values of standard reference geochemical materials.

Trace Metals in Traditional Chinese Medicine: A Preliminary Study Using ICP-MS for Metal Determination and As Speciation

Xiaoru Wang, Zhixia Zhuang, Dahai Sun, Jiangxing Hong, Xihong Wu

, DOI: 10.46770/AS.1999.03.002

[Abstract] (558) [PDF 283.26 K] (3954)

Abstract:
The metal content in several TCM drugs was determined by ICP-MS. The efficiencies of different sample digestion methods were compared. Since one of the products studied is known to contain arsenic sulfides as a main ingredient, a solvent fractionation scheme was developed and applied to speciate As in the product. The metal content in the same TCM drug produced by different manufacturers was compared. The concentration of some metals such as Pb and Cd differs widely with different manufacturers, suggesting that their origin is primarily from external contamination. The high sensitivity and precision of the ICP-MS technique offers considerable advantages over conventional ICP-OES techniques for the analysis of complex samples such as TCM materials. Standardized analytic protocols based on ICP-MS are being developed fur the determination and characterization of metals and trace elements in TCM materials for product quality assessment.

Theory, design, and operation of a dynamic reaction cell for ICP-MS

Tanner S.D.* Baranov V.I.

, DOI: 10.46770/AS.1999.02.001

[Abstract] (470) [PDF 0.00 Byte] (0)

Abstract:
Theory, design, and operation of a dynamic reaction cell for ICP-MS

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