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: 10 August, 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: 31 December, 2026
Please select: 2027 Early Career Analyst Special Issue upon submission.

Recent Issues

Vol.47,2026,NO.4
Pages: 486-614

Full Issue

Cover

Vol.47,2026,NO.3
Pages: 309-485

Full Issue

Cover

Vol.47,2026,NO.2
Pages: 175-308

Full Issue

Cover

Vol.47,2026,NO.1
Pages: 1-174

Full Issue

Cover

Vol.46,2025,NO.6
Pages: 565-674

Full Issue

Cover

Vol.46,2025,NO.5
Pages: 457-564

Full Issue

Cover

Articles in Press
Current Issue
All Issues
Classic Articles
Virtual Issues

Development and Application Validation of a Molten Steel Composition Sensor Based on Laser-Induced Breakdown Spectroscopy

Yang Zhou, Lanxiang Sun*, Changjiang Ding, Guocai Wang, Zhengsheng Chang, Yang Li, Cong Zhang, Peng Zhang

DOI: 10.46770/AS.2026.0039s

[Abstract] (5) [PDF 2.24 M] (56)

Abstract:
The practical application of spectral sensors for molten steel composition online detection has remained limited due to the combined effects of extreme temperature, slag erosion, and transmission challenges associated with weak emissions from trace elements. In this study, a molten steel composition sensor was developed based on Laser-Induced Breakdown Spectroscopy (LIBS). The sensor incorporates a 1.5-meter-long multi-layered probe lance through which the laser beam is focused onto molten steel at the lower end, where the emitted plasma is analyzed to enable online composition measurement. During operation, the probe lance penetrates through the slag layer and maintains immersion in molten steel at a certain depth withstanding temperature exceeding 1650°C. Both the probe lance and the entire optical return path are purged with argon gas to enhance the signal. Through the acquisition of optimal parameters, the industrial application was first performed? using the LIBS sensor? during the refining of 120-ton molten steel. Test set demonstrates R2 of 0.9361, 0.9643, 0.9809, and 0.9815 with corresponding RMSE of 0.04wt.%, 0.03wt.%, 0.03wt.%, and 0.07wt.% for C, Mn, Si, and Cr respectively. Results indicate that the LIBS sensor has preliminarily achieved in-situ online detection of specific elements in molten steel, showing promising application potential.

OTTO-WDID-Based Class-Specific Variable Selection and Sequential Threshold-Rule Classification for Multiclass LIBS Modeling of Edible Salt Products

Sandeep Kumar, Vivek K. Singh, Sang-Ho Nam, Song-Hee Han, Yonghoon Lee*

DOI: 10.46770/AS.2026.0053s

[Abstract] (2) [PDF 1.67 M] (63)

Abstract:
Laser-induced breakdown spectroscopy (LIBS) provides rapid elemental fingerprints, but multiclass classification often requires both interpretable variable selection and a transparent classification rule. In this study, we propose a combined framework that links one-to-the-others wavelength-dependent interclass distance (OTTO-WDID) with sequential threshold-rule classification. OTTO-WDID evaluates each wavelength by comparing one target class with all remaining classes, thereby identifying class-specific emission lines suitable for one-to-the-others decisions. A local baseline-drift correction was applied using adjacent non-emission wavelengths to estimate the emission-line-specific contribution to the observed interclass distance. The framework was applied to LIBS spectra of five edible salt products. OTTO-WDID identified the emission peaks of Ba II at 455.4 nm, Si I at 288.2 nm, Ca I at 612.2 nm, Sr II at 407.8 nm, and Li I at 670.8 nm as class-specific variables for the corresponding sample classes (S1 – S5, respectively). These variables included weak trace-element lines, showing that highly discriminative information is not necessarily associated with the strongest emission peaks. The selected variables were then used to construct a sequential threshold-rule classifier, in which each step separates one target class from the remaining classes using a single class-specific variable and threshold. For the five-class problem, only four active threshold rules were required because the final class was assigned as the residual class. The least reliable Ba II variable was excluded from the active rule sequence, and S1 was assigned as the residual class. Using the sequence S2 → S3 → S4 → S5 → S1, the classifier achieved 100% accuracy in leave-one-out cross-validation. The results demonstrate that OTTO-WDID and sequential threshold-rule classification provide a simple, interpretable, and compact pipeline for multiclass LIBS modeling.

A Homologous Detection Strategy Based on Spectrum-ultrasound-image for Precise Analysis in Coal LIBS

Xuechen Niu, Feiyu Guan, Yongtai Zhuang, Haineng Yang, Deng Zhang, Junfei Nie, Jianguo Liu, Zhenlin Hu*, Lianbo Guo*

DOI: 10.46770/AS.2026.0018s

[Abstract] (30) [PDF 1.11 M] (227) [Supporting Information]

Abstract:
Coal analysis plays a crucial role in its efficient utilization and pollution control. Laser-induced breakdown spectroscopy (LIBS) exhibits promising application prospects in coal quality analysis because of its uniquely rapid and minimally destructive capabilities. However, the complex composition of coal induces severe matrix effects, which pose a formidable challenge to the accurate quantification in traditional LIBS analysis. In this study, a novel method named spectrum-ultrasound-image multi-modal fusion model (SUI-MM) was introduced to mitigate matrix effects in coal and improve the quantitative performance. SUI-MM extends conventional LIBS to a homologous multi-modal analysis framework combining spectra, ultrasound, and image, effectively compensating for the absence of physical structural and plasma spatial morphological information in spectra. By establishing a three-dimensional feature extraction and fusion strategy, it enables comprehensive characterization of coal plasma behavior and further improves quantitative performance. To verify the effectiveness of SUI-MM, experiments were performed on elemental and proximate analysis of coal. For the elemental analysis, the average R2p is improved to above 0.998, while RMSEp and AREp are reduced by 88% and 90%, respectively. For the proximate analysis, the average R2p is increased to over 0.999, and both RMSEp and AREp are decreased by 91% on average. Furthermore, ablation experiments confirm that image and ultrasonic signals contribute significantly to the improved analytical performance. These results demonstrate that the SUI-MM scheme can effectively mitigate matrix effect and significantly improve the quantitative accuracy in coal. In summary, SUI-MM is expected to further support the low-carbon transition of the energy industry.

LIBS Analysis of Laser-ablated W Plasma at Variable Ablation Angles and Gases in Low-pressure Atmospheres

Boliang Men, Cong Li*, Huace Wu, Shiming Liu, Gaogui Feng, Zhihang Li, Longfei Li, Dongpeng Tian, Ding Wu, Ran Hai, Xingwei Wu, Hongbin Ding

DOI: 10.46770/AS.2026.0004s

[Abstract] (28) [PDF 2.30 M] (241) [Supporting Information]

Abstract:
Laser-induced breakdown spectroscopy (LIBS), as an in situ and real-time diagnostic technique, has proven effective in acquiring elemental distribution information under extreme operational conditions. Under the actual operating conditions of tokamak devices, the ablation angle and gas atmosphere exert a synergistic influence on the evolution behavior of laser-ablated plasma. However, the underlying physical mechanisms have not yet been fully elucidated, necessitating more systematic and in-depth investigations. The LIBS characteristics of laser-ablated W plasma under low-pressure (100 Pa) Ar, He, N2 gases and various incident angles were systematically investigated. LIBS spectra revealed that at low laser energy density, Ar promotes more effective electron collision excitation and plasma recombination, while the higher thermal conductivity of He facilitates free expansion of the plasma. In N? atmosphere, the signal-to-background ratio (S/B) of laser-ablated W plasma remained largely independent of the angle, which aids in optimizing LIBS signal stability. As the laser-ablated angle increases, the laser energy density decreases, leading to reduced stability and symmetry of the plasma plume. Further research indicates that as laser energy density decreases, the axial expansion of the W plasma plume remains nearly unchanged, whereas the radial expansion decreases rapidly. This study elucidates the evolution mechanism of the laser-ablated W plasma under the synergistic effects of ablation angle and gas atmosphere. The results provide an important theoretical basis for the geometric calibration and optimization of in situ LIBS diagnostic systems intended for operation under low-pressure conditions.

[Full Issue download]

[Cover download]

Invited Review

Review: Tracking Lithium Ion Transport in All-solid-state Batteries Using Neutron Depth Profiling

Caijin Xiao*, Junwei Liang*, Liang Zhao, Jiawang Meng, Ming Liu*

2026,47(4),486-498,

DOI: 10.46770/AS.2026.0019i

[Abstract] (35) [PDF 4.31 M] (334)

Abstract:
Neutron depth profiling (NDP) is a non?destructive, operando technique that directly quantifies lithium distribution and transport in all?solid?state batteries (ASSBs) by exploiting the 6Li(n, α)3H nuclear reaction. Conventional techniques (e.g., X?ray methods) rely on interactions with extranuclear electrons and thus struggle to detect lithium due to its low electron density. By contrast, NDP exploits the direct nuclear reaction, enabling unambiguous localization of 6Li atoms. Consequently, NDP provides quantitative, depth?resolved monitoring of lithium concentration profiles along the battery thickness direction with a typical depth resolution of tens of nanometers. This review systematically summarizes recent progress in applying NDP to four key aspects of ASSBs: electrolytes, electrodes, interfaces, and thin?film full batteries. In electrolytes, NDP has revealed electronic?conductivity?induced random dendrite nucleation and reversible short?circuit phenomena. In electrodes, it has guided 3D framework designs, validated surface halogenation for Si anodes, and verified longitudinal Li gradients in composite cathodes. In interfaces, NDP has visualized space?charge layers, quantified lithiophilic coating effects, and provided early detection of short?circuit failure. In thin?film batteries, NDP has tracked Li?ion transport in near real time using isotopic tracers, identified Si migration as a degradation mechanism, and pinpointed rate?limiting interfaces in combination with other techniques. Beyond these applications, the inherent advantages and current limitations of NDP—such as its sensitivity to 6Li isotope, the trade?off between depth resolution and counting statistics, and the requirement for flat sample surfaces—are critically discussed. This review establishes NDP as an indispensable tool for understanding and engineering lithium transport in ASSBs, and outlines future directions including higher?flux neutron sources, improved detector systems, and integration with complementary in situ probes.

Article

Quasi-Non-Destructive Multi-Element Characterization of Polymer Materials for 3D-Printed Firearms by Liquid Microjunction Sampling into Inductively Coupled lasma Mass Spectrometry (LMJ-ICPMS)

Jordan Chiabai, Diane Beauchemin*

2026,47(4),499-506,

DOI: 10.46770/AS.2026.0061

[Abstract] (22) [PDF 604.17 K] (94) [Supporting Information]

Abstract:
In this proof-of-concept study, liquid microjunction inductively coupled plasma mass spectrometry (LMJ-ICPMS) was used as a localized, quasi-non-destructive approach for the qualitative trace elemental characterization of polymer materials relevant to forensic investigations involving 3 dimensions (3D)-printed firearms. Blue nylon glass-fibre-reinforced polyamide 6 (PA6-GF), polyethylene terephthalate glycol (PETG), and polylactic acid (PLA) were analyzed using a custom LMJ sampling interface coupled to quadrupole-based ICPMS. Measurable transient signals were obtained for multiple elements directly from polymer surfaces, demonstrating the capability of LMJ sampling to recover and transport trace elemental constituents with minimal sample preparation and limited surface disruption. Distinct normalized elemental profiles were observed between PA6-GF and PETG, with PETG exhibiting higher relative abundances of Mg, Ca, Ti, and Sr, whereas PA6-GF exhibited elevated Ba. Complete separation between PA6-GF and PETG was achieved using Ti/Mg and Ba/Ca elemental ratios, while targeted and untargeted principal component analyses demonstrated distinct clustering based on selected elemental markers and the broader elemental profile, respectively. The first two principal components of the targeted analysis accounted for 97.7% of the total variance. Addition of 2% (v/v) methanol (MeOH) to the 2% (v/v) nitric acid (HNO3) sampling solvent improved elemental recovery of PLA, enabling multivariate differentiation of PA6-GF, PETG, and PLA, with the first two principal components accounting for 97.0% of the total variance. These results demonstrate the applicability of LMJ-ICPMS for qualitative elemental profiling and differentiation of polymer materials, while highlighting the importance of solvent optimization for extending the approach to chemically distinct polymer systems.

Accurate and Rapid Determination of 99Tc in Seawater Samples Using Triple-quadrupole ICP-MS with C2H4-He Mode

Jie Chen, Yiman Lu, Zongjie Xie, Zhilong Yang, Man Wang, Hao Wang, Jing Lin, Shan Xing*

2026,47(4),507-514,

DOI: 10.46770/AS.2026.0033

[Abstract] (15) [PDF 1.89 M] (98) [Supporting Information]

Abstract:
Accurate and rapid monitoring of 99Tc is crucial for the radiological risk assessment in nuclear emergency situations. However, accurate determination of 99Tc by ICP-MS is always hindered by the interferences of 98Mo and 99Ru. In this work, a rapid and accurate analytical method of 99Tc in seawater samples was established, and 185Re as a non-isotopic tracer was used for the monitoring of 99Tc yield in the whole procedure. TiCl3 was chosen as a reducing agent and co-precipitant for the 99Tc preconcentration. 98Mo and 99Ru were effectively removed using two TK200 resin columns under novel alkaline loading conditions, and the excellent decontamination factors (DFs) of 4.28 × 106 for Mo and 5.16 × 105 for Ru were achieved. Importantly, the interferences of 98Mo+ tailing, 99Ru+ and 98Mo1H+ can be efficiently suppressed using C2H4 as a new reaction gas for 99Tc measurement, and 98Mo1H+/98Mo+ of 1.31 × 10?7 was achieved at 0.28 mL/min C2H4-1.0 mL/min He. The overall decontamination factor of Ru reached 3.76 × 107, which are at least 2 orders of magnitude higher than that of the conventional methods. The detection limit of 3.18 pg/L (2.00 mBq/L) was obtained with a whole analytical time of 4 hours for 12 samples, which was suitable for the application of nuclear emergency. More importantly, this correction-free alternative method was found to accurately measure 99Tc by ICP-MS without any mathematical correction of 99Ru for the first time.

Determination of Radioactive Selenium-79 in Environmental Samples by ICP-MS after Solid Phase Microextraction - Dielectric Barrier Discharge Vapor Generation

Zhenqi Gao, Shanshan Chen, Zenghui Zhu, Junrong Wang, Shengkang Liang, Qian He*

2026,47(4),515-525,

DOI: 10.46770/AS.2026.0038

[Abstract] (11) [PDF 992.95 K] (79) [Supporting Information]

Abstract:
Accurate determination of 79Se level in environmental samples is critical for evaluating radioactive contamination risk. A new pretreatment method for 79Se determination by inductively coupled plasma-mass spectrometry (ICP-MS) through solid phase microextraction (SPME) - dielectric barrier discharge vapor generation (DBDVG) - ammonia water absorption-evaporation (AAE) was proposed in this work. The sorbent of nano-ZrO2 was used in SPME, which could both enrich Se and selectively adsorb Se from Br, which has an identical mass of 79 to 79Se. DBDVG was used to reduce the species of Se from Se(IV) or Se(VI) to volatile H2Se vapor to eliminate the sample matrix interferences. Ammonia water was used to absorb the volatile H2Se and then evaporated to enrich Se. The adsorption, DBDVG and absorption parameters were optimized in detail. The mass interference of 38Ar40ArH+ was effectively eliminated by the addition of He gas in the collision/reaction cell, and the other potential interferences of 39K40Ar+, 63Cu16O+, 158Gd2+, 158Dy2+ and 78SeH+ were all not obvious in this method. The detection limit of 79Se was 10.1 ng L-1 and the inter-batch reproducibility between different SPME tubes was 1.9 %. The concentration of 79Se in environmental samples such as lake water and plant leaves were assessed. Compared with conventional ion exchange resin methods for enrichment of 79Se, our SPME approach achieves desorption via DBD plasma without the need of acidic or alkaline reagent for elution. In contrast to conventional ICP-MS sample introduction methods for ??Se determination, such as hydride generation and electrothermal vaporization, the proposed DBDVG technique drives redox reactions entirely via free radicals and electrons generated in the discharge plasma. This design fully eliminates the need for additional redox reagents or chemical modifiers, and thus drastically lowers the associated reagent blank levels.

Comparative Evaluation of a Novel Lithium Metaborate Fusion Approach and Phosphate Fusion for Multielement ICP‑OES Analysis of Nb–Ta Ores

Lucie ?imoníková, Lubomír Proke?, Jan Loun, Viktor Kanicky, Karel Novotny*

2026,47(4),526-537,

DOI: 10.46770/AS.2026.0042

[Abstract] (10) [PDF 1.06 M] (94) [Supporting Information]

Abstract:
Reliable determination of niobium and tantalum in Nb–Ta ores is analytically challenging due to the refractory nature of the matrix and pronounced spectral and matrix effects in ICP?OES. In this study, two chemically distinct fusion procedures – an established phosphate fusion and an optimized lithium metaborate (LiBO2) fusion followed by dissolution in a dilute HF/HNO3 mixture – were systematically compared. A dataset of 69 natural Nb–Ta mineral concentrates and one industrial synthetic material analyzed over a ten-year period was used for the comparison. Method equivalence was assessed using Deming regression with a heteroscedastic error structure. Trueness was evaluated using the CRM X1808 certified reference material and an in-house reference material characterized by X-ray fluorescence (XRF). Both fusion methods provided analytically equivalent results for Nb2O5 and Ta2O5 across the entire concentration range. However, borate fusion allowed simultaneous determination of a broader range of elements, including Na2O, P2O5, and SiO2. Although both approaches can be used to quantify most analytes, their applicability is partly complementary: phosphate digestion does not allow reliable determination of sodium and phosphorus, and SiO2 determination may be limited at higher concentrations. In addition, while both fusion techniques are considerably more rapid and more robust than conventional acid digestion, borate fusion also allows slightly faster sample preparation. Overall, fusion-based approaches represent an efficient and reliable strategy for the comprehensive analysis of complex Nb–Ta matrices.

Spatiotemporal DVS Event-stream Fusion for Robust LIBS Contamination-level Classification under Laser-energy Perturbation

Hongyu Wang, Tao Deng, Weiliang Liu, Bin Cao, Honglin Jian, Junchen Li, Lei Deng, Xilin Wang*

2026,47(4),538-554,

DOI: 10.46770/AS.2026.0035

[Abstract] (15) [PDF 5.76 M] (124)

Abstract:
Laser-induced breakdown spectroscopy (LIBS) is promising for rapid contamination analysis of power insulators, but its reliability is limited by laser-energy perturbation during field detection. To improve the robustness of LIBS-based contamination-level classification, this study proposes a LIBS–DVS Hybrid Gated Fusion Spiking Neural Network (LD-HGF-SNN) by integrating LIBS spectra with raw dynamic vision sensor (DVS) event streams. Unlike methods based on reconstructed event images, LD-HGF-SNN constructs a raw-event-derived spatiotemporal DVS event tensor to preserve the time–height–width evolution of laser-induced plasma and encodes it using an LIF-neuron-based spiking branch. A 1D convolutional branch extracts LIBS spectral features, while a sample-adaptive gated fusion module regulates the contributions of spectral and event-stream information. Broad-energy classification and cross-energy evaluation tasks were constructed using paired LIBS–DVS data collected under seven laser-energy conditions. LD-HGF-SNN achieved 97.50% accuracy and 97.49% macro-F1 under the reference-energy condition, and maintained 87.50% accuracy and 87.52% macro-F1 under full-range laser-energy perturbation. In the most challenging task, its accuracy exceeded the strongest ablation model, the ungated fusion model, and the reconstructed-image fusion baseline by 15.50, 21.00, and 22.50 percentage points, respectively. These results indicate that raw-event-derived DVS event streams provide complementary plasma-dynamic information for LIBS spectra, and that preserving the spatiotemporal structure of DVS events can improve LIBS classification robustness under laser-energy perturbation.

From Site Assessment to Simulated Experiment: A Parallel Investigation of Heavy Metal Pollution in a Soil-Taraxacum mongolicum Hand.-Mazz. System Impacted by Tungsten-Beryllium Mining in Haba Snow Mountain

Ning Lu#, Linjun Zhang#, Xiaofang Yang, Jiayi Hu, Xin Liu, Xiangdong Yu*, Xiaodong Wen*

2026,47(4),555-573,

DOI: 10.46770/AS.2026.0048

[Abstract] (28) [PDF 6.77 M] (86) [Supporting Information]

Abstract:
Accurate detection and systematic assessment centered on atomic spectrometry techniques serve as an essential foundation for elucidating the pollution characteristics, ecological risks, and health hazards of heavy metals (HMs) farmland soils around mining areas. In this study, inductively coupled plasma optical emission spectrometry (ICP-OES) was employed as the core analytical technique to precisely quantify ten HMs in farmland soils approximately 20 km from a tungsten (W) beryllium mining area. Based on the measured ICP-OES data, GIS visualization was integrated with the geo-accumulation index (Igeo), pollution load index (PLI), potential ecological risk index (PERI), human health risk assessment (HHRA), and positive matrix factorization (PMF) source apportionment model to systematically evaluate the pollution characteristics, risk levels, and source contributions of HMs in the farmland. Meanwhile, the stress effects of W on Taraxacum mongolicum Hand.-Mazz. (T. mongolicum) were investigated through a pot experiment under W stress. The comprehensive pollution assessment revealed that the Igeo values of Cd, W, and As reached 3.88, 3.76, and 3.51, respectively, all indicating heavy contamination, and the PLI values corresponded to heavy to extremely heavy pollution levels. PMF identified five pollution sources. HHRA indicated that all population groups faced both carcinogenic and non-carcinogenic risks, with children exhibiting the most pronounced risks and direct ingestion serving as the primary carcinogenic exposure pathway. The pot experiment demonstrated that, under W stress, HMs accumulation capacity followed the order: roots > leaves, whereas the content of active components exhibited no significant change. This study validates the effectiveness and reliability of ICP-OES in the precise quantification of soil HMs and environmental risk assessment, providing a reliable data foundation and methodological support for the comprehensive assessment, prevention, and control of HM pollution in farmland soils.

Quantitative Analysis of Microstrain and Investigation of Microscopic Mechanism Based on Laser-Induced Breakdown Spectroscopy

Shuoyu Yang, Yazi Wang, Yongyi Du, Jiaqi Zhao, Yue Lv, Xiaoning Yang, Yifan Luo, Ruibin Liu*

2026,47(4),574-584,

DOI: 10.46770/AS.2026.0055

[Abstract] (2) [PDF 2.81 M] (67) [Supporting Information]

Abstract:
The microstructure of metallic materials, particularly their strain characteristics, constitutes the core determinant of macroscopic physicochemical properties; therefore, achieving rapid, precise, and in-situ characterization of microstructure is important for research on metallic materials. Since the microstructure of materials can modulate plasma excitation conditions, microstrain information in metallic materials can be reflected through plasma emission spectra. Laser-induced breakdown spectroscopy (LIBS) has been conventionally employed for detecting elemental composition and conducting quantitative analysis of elemental content; however, investigations of microstrain based on LIBS remain unreported. In this study, we, for the first time, utilized spectroscopic information from laser-induced plasma to establish a classification model for microstrain. Furthermore, by integrating artificial intelligence algorithms, we constructed a quantitative relationship model between spectral characteristics and microstrain, thereby realizing online in-situ quantitative analysis of microstrain. We also conducted an in-depth investigation into the influence mechanism of microstructure on plasma spectra, providing a solid theoretical and experimental foundation for rapid diagnosis of material microstrain based on LIBS technology.

Direct Determination of 206Pb/204Pb and 208Pb/204Pb Ratios by Triple Quadrupole ICP-MS Without Pb Purification: Opportunities and Limitations for Source Tracing

Yangjunjie Xu-Yang*, Sophie Ayrault, Delphine Thomas

2026,47(4),585-594,

DOI: 10.46770/AS.2026.0047

[Abstract] (3) [PDF 5.07 M] (94) [Supporting Information]

Abstract:
Lead stable isotope ratios 206Pb/204Pb, 207Pb/204Pb and 208Pb/204Pb are widely used to trace the origin of natural or artificial materials in geochemistry, environmental science and archaeology. Time consuming sequential column chemistry for purification of Pb are often necessary for preparing the analysis of Pb isotopes ratios with MC-ICP-MS, with a precision (uncertainties) reaching 0.001. However, such a high precision is not always necessary for source tracing when the end-members have significant different signatures. Here, 206Pb/204Pb, 207Pb/204Pb and 208Pb/204Pb ratios were analyzed for 7 certified reference materials (CRM: SL-1, RGM-1, MAG-1, BHVO-1, BCR-723, BCR-1 and BCR-2), including sediments and urban road dusts, using Triple Quadrupole Inductively Coupled Plasma Mass Spectrometry (TQ-ICP-MS) after conventional total digestion without sequential column chemistry. The solutions from the digestion were measured at four Pb concentrations (0.5, 1, 1.5 and 2 ng ml-1). Among 56 measurements on 33 SL-1 samples at a lead concentration of 2 ng ml-1 (sample digestion was realized between 2018 and 2024 while lead isotopic ratio measurements were conducted between 2022 and 2025), the first and third quartile of the uncertainties are 0.07 and 0.1 for 206Pb/204Pb, 0.05 and 0.09 for 207Pb/204Pb and 0.16 and 0.21 for 208Pb/204Pb. The 206Pb/204Pb and 208Pb/204Pb ratios obtained with TQ-ICP-MS can be especially useful for source tracing while uncertainties related to 207Pb/204Pb are in the same range of differences between terrestrial sources. This study employs TQ-ICP-MS to complement earlier ICP-QMS-based research, while also validating lead isotope ratio analysis using a larger set of certified reference materials (CRMs). In addition, the analytical protocol, spanning digestion and measurement over multiple years, enables an assessment of the long-term stability and reproducibility of the entire methodological workflow. We conclude that some studies can benefit from the simple and fast analysis of 206Pb/204Pb and 208Pb/204Pb ratios by TQ-ICP-MS with very small amount of additional works and investment, when potential end-members display sufficiently distinct isotopic signatures. Moreover, the here developed approach can be used to select samples which deserve more detailed geochemical analyses, lowering costs and environmental impacts.

Impurities Determination in High-purity Cerium Oxide by Aerosol Dilution ICP-MS After Solvent Extraction Separation

Shuang Zou, Shengnan Wang, Lanlan Jin, Wei Guo*

2026(4),595-600,

DOI: 10.46770/AS.2026.037

[Abstract] (0) [PDF 471.34 K] (0)

Abstract:
High-purity cerium dioxide (CeO?) powder serves as a key raw material for chemical mechanical planarization (CMP) slurries, wherein trace impurities can severely degrade its polishing efficiency and surface modification performance. This study established a reliable method for the determination of trace rare earth element (REE) impurities in high-purity (CeO?) via online aerosol dilution inductively coupled plasma mass spectrometry (AD-ICP-MS) combined with solvent extraction pretreatment. Using 2-ethylhexylhydrogen-2-ethylhexylphosphonate (EHEHP) as the extractant, the tetravalent cerium matrix was efficiently separated with a separation efficiency of ~99.8 %, and the recoveries of target REEs ranged from 92 % to 98 %. Furthermore, residual Ce-derived mass interferences on gadolinium (Gd) and terbium (Tb) detection were effectively eliminated by introducing 0.80 L min?1 argon into the sample aerosol before the ICP. Under the optimized conditions, the formation yields of interfering polyatomic ions were suppressed to as low as 0.12 % for CeO?/Ce? and 0.008 % for CeOH?/Ce?. The limits of quantification (LOQs, 10σ) for 14 REE impurities were determined to be 0.2–1.3 ng g?1. The proposed method was successfully applied to the analysis of two high-purity CeO? samples. The satisfactory spike recoveries of 93–103% verified that the proposed approach is robust and promising for the trace analysis of REE impurities in high-purity cerium oxide materials.

Laser-Induced Breakdown Spectroscopy for In Situ Analysis of Immovable Polychrome Cultural Heritage

Yikang Hou, Zhuoxi Li, Jie Lian*

2026(4),601-614,

DOI: 10.46770/AS.2026.0012

[Abstract] (0) [PDF 2.93 M] (0)

Abstract:
Immovable polychrome cultural heritage—including grotto murals, architectural wall paintings, painted plasters, and rock art—presents an analytical problem defined by three simultaneous constraints: the objects are stratified and materially heterogeneous, the key questions are usually conservation-driven rather than purely descriptive, and the investigation must be performed in situ with a level of intervention acceptable to conservation practice. In this context, laser-induced breakdown spectroscopy (LIBS) has moved well beyond its early role as a rapid elemental screening tool. Its practical significance lies in the fact that it can provide elemental information, micrometric sampling, and depth-resolved data within the same analytical sequence, thereby addressing problems that are difficult to solve by fully non-contact techniques alone, which is why depth-resolved investigation is often conservation-critical rather than merely technically attractive. This review focuses specifically on immovable polychrome heritage and examines how LIBS has been used to identify mineral pigments, disentangle repainting and overpaint, diagnose salts and surface deposits, estimate layer thickness, and support decisions on cleaning and consolidation. Emphasis is placed on the analytical logic of field deployment: acceptable micro-destructivity, parameter selection under fragile surface conditions, pulse-to-depth calibration, chemometric interpretation, and the role of multimodal workflows with Raman spectroscopy, X-ray fluorescence, optical coherence tomography, and imaging methods. Recent computational and calibration strategies—numerical simulation, machine-learning-assisted calibration, and micro-CT-aided depth calibration—are also considered as ways to reduce dependence on ideal physical standards when exact mural analogues cannot be prepared. The review argues that the present frontier is no longer whether LIBS can generate useful spectra from wall paintings, but whether its outputs can be standardized, reproduced, and translated into evidence that conservators can trust. Its long-term value therefore depends less on broadening application claims than on consolidating low-damage protocols, uncertainty-aware interpretation, and explicit integration into conservation decision-making.

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] (576) [PDF 146.88 K] (4052)

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] (516) [PDF 86.02 K] (3942)

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] (513) [PDF 99.16 K] (4253)

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] (558) [PDF 154.90 K] (4114)

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] (656) [PDF 135.56 K] (4499)

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] (442) [PDF 167.98 K] (3760)

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] (429) [PDF 116.38 K] (3647)

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] (609) [PDF 283.26 K] (4155)

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] (509) [PDF 0.00 Byte] (0)

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

Virtual Issue: Environmental Analysis in Atomic Spectroscopy for PerkinElmer, August, 2021

[Full Issue download]

More+

Advertisements

PDF Download

Download
News & Announcements

External Links