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

    Print ISSN:0195-5373
    Online ISSN: 2708-521X
    2021 SCI IF: 3.014 (JCR, Q2)

          The ATOMIC SPECTROSCOPY is a peer-reviewed international journal started in 1962 by Dr. Walter Slavin. In November 2019, its ownership was transferred to Atomic Spectroscopy Press Limited (ASPL), Hongkong, P.R. China. It is intended for the rapid publication of Articles, Review/Mini-review, or Letters/Communications in the fields of elements, elemental speciation, and elemental isotopic analysis by XRF, AAS, AFS, ICP-OES, ICP-MS, GD-MS/OES, TIMS, SIMS, AMS, LIBS, AMS, NAA, INAA, various microanalysis techniques, and related sample preparation techniques. Manuscripts dealing with (i) instrumentation & fundamentals, (ii) methodology development & applications, and (iii) standard reference materials (SRMs) development can be submitted for publication.

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      DOI: 10.46770/AS.2023.062
      Buffer gas-assisted high-irradiance laser ionization time-of-flight mass spectrometry (BGA-LI-TOFMS) was used to determine the elemental distribution of Lycoptera fossils from the Dawangzhangzi Bed of the Yixian Formation in Liaoning Province, China. The Sr, Ba, and Pb images of the Lycoptera fossil highlight the fine structure of the skeleton, and the distribution of Fe and Si provides data regarding the preservation pattern and nature of pyritization in the Jehol Biota. The enrichment of toxic substances such As and H2S may be one of the reasons for the cluster mortality of Lycoptera. Meanwhile, the elemental analysis of the rocks in the fossil preservation shows that the paleoclimate indices MgO/CaO and Sr/Cu indicate dry and hot climatic conditions at that time. Meanwhile, the paleosalinity indicators (m value and Sr/Ba ratio) indicate a semi-saline to slightly saline water body. The paleoredox environment indicators (Th/U and V/(V+Ni) ratio) suggest an anaerobic environment with weak stratification and H2S in the bottom water. Thus, the elemental imaging and analysis of the Lycoptera fossil suggest that the organisms of Jehol Biota were preserved in the anoxic water environment and the toxic effect of hydrogen sulfide. Overall, BGA-LI-TOFMS is an adaptable technique for acquiring comprehensive geochemical information on fossils.
      DOI: 10.46770/AS.2023.042
      MoS2 and ZnS quantum dots (QDs) were synthesized and applied as labels in magnetic immunoassays for the determination of myeloperoxidase (MPO) and osteopontin (OPN) via single-particle mode inductively coupled plasma mass spectrometry (ICP-MS). Primary MPO antibodies and primary OPN antibodies were captured by amino-modified magnetic nanoparticles, and the target biomarkers (MPO and OPN) were extracted and then specifically labeled with MoS2 QD-secondary MPO antibody and ZnS QD-secondary OPN antibody conjugates, respectively. MoS2 and ZnS QDs were employed as determination signal probes for ICP-MS measurements. Under the optimized conditions, the limits of detection obtained by magnetic immunoassay for MoS2 and ZnS QD-labeled MPO and OPN were 0.004 and 0.005 ng mL-1, respectively. The linear ranges for MPO and OPN were 0.01–50 and 0.02–50 ng mL-1, respectively. From six replicates, the relative standard deviations of MPO and OPN were found to be 3.5% and 3.2%, respectively. The proposed strategy was applied to determine the MPO and OPN levels in real human serum samples.
      DOI: 10.46770/AS.2023.091
      Microplasma-induced vapor generation (μPIVG), particularly using only hydrogen, has attracted increasing attention in the field of atomic spectrometry. However, its application for field analysis of environmental samples remains limited owing to the difficulty of hydrogen storage and transportation. Herein, a non-noble metal electrode-based hydrogen evolution reaction (HER) was utilized as a safe and environment-friendly hydrogen supply method for the efficient μPIVG of Hg, Cd and Zn. Subsequently, HER-μPIVG was used for the sensitive field detection of Hg, Cd and Zn in environmental samples via miniature point discharge optical emission spectrometry (μPD-OES). In contrast to conventional hydrogen-enhanced μPIVG, hydrogen was produced in situ and in real time using a superior cathode composed of cobalt-phosphorous nanomaterial, eliminating the storage and transport of hydrogen requirements and improving the safety, sensitivity, and feasibility of μPIVG-μPD-OES. Under the optimized conditions, the limits of detection (LODs) were 0.8, 10, and 14 μg L?1 for Hg, Cd, and Zn, respectively, with relative standard deviations (RSDs) of < 4.7%. The accuracy and practicability of the proposed method were validated through Hg, Cd, and Zn determinations in two certified reference materials (CRMs) and several water samples with satisfactory results.
      DOI: 10.46770/AS.2023.089
      In this study, a small platinized tungsten coil (TC) with a composite structure was utilized for the first time in a liquid sampling electrothermal vaporizer (ETV) setup. A novel direct sampling mercury (Hg) analyzer coupled with a dielectric barrier discharge (DBD) and a miniature fiber optic spectrometer (FOS) as an optical emission spectrometer was fabricated for the sensitive determination of Hg in environmental water. This ETV setup displayed a maximum sample volume of 100 μL and fulfilled the task of sequestering Hg during the dehydration and ashing processes under high temperature due to the formation of a platinum (Pt) and Hg amalgam. Under optimized conditions, the limit of detection (LOD) of Hg was 0.1 μg L-1 for a 100 μL liquid sample and the relative standard deviation (RSD) of 11 repeated measurements of Hg standard solution was 3.2%; the linearity (R2) was > 0.999 in the range of 0.4-100 μg L-1. The results for the GBW08063 sample (9.89 μg L-1) agreed with the certified values of certified reference materials (CRMs) (10 μg L-1), and the spiked recoveries were 94-100%, which proved favorable analytical accuracy and precision. The total analysis time was observed to be less than 3 min, and this small-sized ETV-DBD-OES system consumes only ~100 W of power while weighting less than 12 kg. Therefore, the proposed ETV-DBD-OES method demonstrates simplicity, suitable sensitivity, precision, and robustness, with promising application in the field for rapid water analysis for Hg.
      DOI: 10.46770/AS.2023.088
      Magnetic covalent organic frameworks (COFs) were prepared using aminated Fe3O4 nanoparticles as the magnetic core and 1,3,5-tris(4-aminophenyl)benzene (TPB) and 2,5-dimethoxyterephthalaldehyde (DMTA) as monomers. The resultant Fe3O4@TPB-DMTP-COF was then post-modified with 3-ethynylthiophene through the “Aza D-A reaction”. The Fe3O4@COF-thiophene composite showed a high Brunauer-Emmett-Teller surface area of 898 m2?g-1, as well as a high content of S (5.27 w.t.%). Trace mercury (Hg), lead (Pb), and bismuth (Bi) ions were extracted from environmental water samples, followed by inductively coupled plasma mass spectrometry (ICP-MS) detection. Extraction conditions, such as extraction pH, sample volume, adsorbent amount, extraction/desorption time and elution volume, were optimized. Under the optimal conditions, the three heavy metal ions were extracted from 150 mL of aqueous solution within 20 min and eluted with 0.1 mol L-1 HNO3 containing 8% cysteamine hydrochloride within 20 min. The method exhibited a high enrichment factor (188) and wide linear range of 3-5000 ng?L-1 for Hg2+/Pb2+ and 2-2000 for Bi3+, with the detection limits of 0.41, 0.97 and 0.47 ng?L-1, respectively. Furthermore, the reproducibility of the method was evaluated, and the relative standard deviations of Hg2+, Pb2+ and Bi3+ were found to be 7.5, 6.8 and 6.2% (n = 7, c = 3 ng?L-1), respectively. The accuracy of this method was verified by analyzing certified reference materials in environmental water, including GSB 07-1185-2000 (202047), GSB 07-1185-2000 (201239) and BY 400143 (B2003113). The application potential of this method was further evaluated by analyzing real environmental water samples. Target Hg2+ and Pb2+ ions concentrations were found to be 4.91 and 62.5 ng?L-1, respectively, in the East Lake water sample and 10.2 and 103 ng?L-1, respectively, in the Yangtze River water sample. The recoveries of target three metal ions were found to be 86.1-104 % in the two environmental water samples at three spiked concentration levels.
      DOI: 10.46770/AS.2023.012
      Matrix-matched reference materials are important for in situ trace and isotope analyses. In this study, we developed an efficient method for preparing chemically homogeneous magnetite (MtTR-1) without adding a binder. The initial magnetite powder (d90 = ~80 μm) was milled to form micron (d90 = 3.0 μm) particles in an anhydrous ethanol suspension and argon environment using a high-energy vibration ball mill. The obtained particles were pressed into a magnetite cylinder (10 mm in diameter and 9.2 mm in height), sealed into a silver tube, and sintered at 500 °C and 1.2 GPa for 2 h. Laser Raman spectroscopy results indicated that high-temperature and high-pressure sintering did not induce any phase transformation. The smooth surface after polishing was subjected to repeated analyses via electron probe microanalyzer using a spot size of 5 μm and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) using spot sizes of 38-60 μm. The results indicated that the texture and chemical composition are homogeneous in MtTR-1. The smooth time-resolved signal intensities of elements, steep wall, and flat bottom of ablation craters also suggested homogeneity in the depth profile. Line profile analyses across the entire pressed pellet further demonstrated that the pellet is homogenous for the investigated elements. The concentrations of major and trace elements in MtTR-1 determined by ICP-OES and ICP-MS are used as the preferred values. The MtTR-1 can be cut into slices, repeatedly polished and used for in situ analyses. The proposed technique for producing magnetite can also be applicable to other minerals or rocks by optimizing the conditions, thus providing a new method for preparing reference materials for in-situ microanalysis.
      DOI: 10.46770/AS.2023.080
      In this study, a laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) method is developed for in -situ quantitative imaging of trace impurity elements in Bi4Si3O12 (BSO) crystals. This method has unique advantages of low detection limit and high spatial resolution for the analysis of defects in crystal microregions. The regression coefficients of the calibration curves for each element were greater than 0.99, and the detection limits (DLs) were 17, 5, 7, 48, 5, 7, 16, 27, and 7 ng/g for 24Mg, 45Sc, 48Ti, 90Zr, 139La, 146Nd, 172Yb and 208Pb, respectively. The LA-ICP-MS measurements were in good agreement with the results obtained using conventional ICP-MS method. Segregation phenomena of elemental impurities in the axial direction of the BSO crystal can exist during crystal growth. Finally, the distribution of the impurity elements in the dendritic crystal defect region of the crystal was visualized. We believe that this work proposes a novel less-invasive analysis method for exploring the composition-defect relationship of crystals.
      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.
      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.
      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.
      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.
      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.
      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?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.
      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



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