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    Prof. Xian-Hua Li
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    Prof. Wei Guo
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    Prof. Michael Dürr
    Prof. Wei Hang
    Prof. Zhaochu Hu

    Print ISSN:0195-5373
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    2020 SCI IF: 2.04

    Special Thematic Issue --- Call for Papers:

    'Microanalytical Techniques for Extraterrestrial Samples'

    On December 17, 2020, the lunar sample-return capsule of the Chang’e-5 mission successfully landed at Dorbod Banner, Inner Mongolia, China. It was 44 years ago when the Luna 24 mission retrieved lunar soil samples. Now, the Chang'e-5 has returned current lunar soil samples which are not only precious and rare, but also of different uniformity and small particle size that pose a challenge for analytical techniques. The first 2022 issue of Atomic Spectroscopy is intended for the publication of Microanalytical Techniques for Extraterrestrial Samples to support the research on the mineralogy, petrology, chronology, magnetism, and geochemistry of the Chang’e-5 lunar samples and to further the studies of terrestrial as well as extraterrestrial samples in the future.

    All papers submitted for this special thematic issue will be subject to the general research review procedures as established for the Atomic Spectroscopy journal.

    Deadline for paper submission: December 1, 2021

    Publication date: February 1, 2022

    If you would like to offer a paper, please email the manuscripts to our guest editors:

    1. Jinhua Li (jinhua.li@at-spectrosc.com): Microscopy and Microspectroscopy Analysis

    2. Xiongyao Li (xiongyao.li@at-spectrosc.com): Physical Property Analysis

    3. Yongsheng He (yongsheng.he@at-spectrosc.com): High Precision Isotopic Analysis

    4. Wei Yang (wei.yang@at-spectrosc.com): In Situ Elemental and Isotopic Analysis

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      Incidental ingestion of soil containing Cr, As, Cd, Sb, and Pb has been attracting global attention as it can significantly impact human health. Many bioaccessibility methods have been developed to simulate the amount of contaminants extracted by gastrointestinal fluids following incidental ingestion. Although the continuous online leaching method (COLM) offers various advantages over conventional batch bioaccessibility methods, such as reduced analysis time, elemental source apportionment, and isotopic analysis, it has not yet been applied to soil and directly compared to validated, published methods. This study uses the COLM with simulated gastrointestinal fluids from the United States Environmental Protection Agency (US EPA), United States Pharmacopeia (USP), and unified bioaccessibility method (UBM) to measure the bioaccessibility of Cr, As, Cd, Sb, and Pb in NIST 2710, NIST 2710a, NIST 2711a, and BGS 102. When the US EPA gastrointestinal fluid was used, no significant difference was observed between the COLM bioaccessible + residual, aqua regia extraction, or certificate concentrations for all the elements and soils studied. Furthermore, COLM bioaccessibility was within the acceptable range of control limits and bioavailability (animal) studies for most reference materials. In addition, no statistically significant difference was observed between either the US EPA batch method or the stomach phase of the UBM batch method and the stomach stage of the COLM, indicating that the COLM could be incorporated into current bioaccessibility analyses to improve soil contamination characterization in the future.
      The aim of this review is to provide a brief introduction to recent research advances in in-situ online detection of atmospheric pollutants based on laser-induced breakdown spectroscopy (LIBS) under atmospheric environments. Atmospheric pollution has drawn much public attention, and there is increasing demand for rapid and accurate evaluation of atmospheric environments. LIBS has the advantages of in-situ online detection, simultaneous multi-element analysis, and noncontact measurement, making it a highly competitive analytical technique in the field of environmental monitoring. In terms of the different target samples, some typical research cases, including atmospheric particulate matter, atmospheric pollution sources, halogens in VOCs, atmospheric sulfur, and stable isotope abundance, are presented to illustrate the current development and problems of LIBS detection in this field.
      DOI: 10.46770/AS.2021.608
      MarSCoDe (Mars Surface Composition Detector) is China's first instrument for Mars material analysis, which accompanies the Zhurong Mars rover landing on Utopia Planitia and will detect interested Martian rock and soil targets based on laser-induced breakdown spectroscopy (LIBS) technique. MarSCoDe consists of a bioxial pointing mirror (BPM), an optical head, a calibration targets assembly (CTA), a spectrometer module (SM) and a payload controller. The MarSCoDe is scheduled to analyze twelve major elements. To achieve accurate quantitative analysis and classification of Mars targets, a PSO (particle swarm optimization)-based calibration scheme is adopted to correct the spectral shift due to the temperature change on Mars, and then a convolutional neural network (CNN) was proposed to implement the analysis of elements. Finally, the mineral types of Martian objects will be identified according to the alkali silica ratio. The detection results of the MarSCoDe will provide further information about the evolution of Mars.
      DOI: 10.46770/AS.2021.710
      Trends and advances in the development and application of inductively coupled plasma tandem quadrupole mass spectrometry (ICP-QMS/QMS) with a reaction cell is reviewed mainly based on publications from January 2018 to July 2021. ICP-QMS/QMS has been applied in various research fields covering the sciences of biology, energy, environmental, food/medical, geology, materials, and radionuclide. The objectives of analysis cover the determination of elemental concentration, ion-gas reaction, isotope analysis, single particle analysis, and chemical speciation analysis. Measurement of most elements in the periodic table are reported except for H, N, O, F, rare gas, and some of the radionuclides. In addition to the default reaction/collision gases (i.e., He, H2, O2, and NH3), N2O, CO2, CH4, CH3F, C2H4, and C2H6 have been used as reaction gases to improve the capability of separating spectral interferences or to study the ion-molecule reactions. Typical applications of ICP-QMS/QMS analysis in the major research fields are also discussed.
      DOI: 10.46770/AS.2021.707
      Electrothermal or graphite furnace atomic absorption spectrometry (ETAAS or GFAAS) is one of the most widely used techniques for determining elements in different matrices (e.g., foodstuffs, pharmaceuticals, biological specimens, nanomaterials, polymers, fuels and environmental media). Numerous elements can be simply and quickly determined with high precision and accuracy, low detection limits, and at moderate cost. The technique is also suitable for direct solid and slurry sample analysis. A crucial feature of this technique is that it can perform simultaneous or sequential multi-element analysis. Over the years, many instruments have come on the market for multi-elemental analysis using mostly line source (LS) GFAAS and high-resolution continuum source (HR-CS) GFAAS. This review covers publications from 2000 to 2020 related to the simultaneous or sequential multi-elemental analysis by LS-GFAAS and HR-CS-GFAAS. Mainly the applications, the limits of detection, the use of internal standardization and other aspects regarding the matrix, pyrolysis and atomization temperatures and modifiers are discussed. Finally, a critical comparison is made between the LS-GFAAS and HR-CS-GFAAS techniques.
      DOI: 10.46770/AS.2021.802
      The method of isotope dilution and tracing, based on ethylation-purge and trap-gas chromatography (GC)-inductively coupled plasma mass spectrometry (ICP-MS), has been widely used for the accurate analysis of methylmercury (MeHg) and for tracking its environmental fates (e.g., formation/degradation). However, the tedious ethylation derivatization and purge and trap processes limit analytical throughput. In this work, an automatic ethylation derivatization and purge and trap method, followed by GC separation, pyrolysis, and ICP-MS detection, was developed for MeHg analysis. The throughput and detection limits of this proposed method for MeHg were 7.5 min/sample and 0.03 ng L-1, respectively, with a relative standard deviation of 3.7%. The accuracy of the developed method was validated by the analysis of a spiked water sample and a certified reference material (DORM-4, Fish protein) using isotope dilution (Me201Hg). In addition, anaerobic Geobacter sulfurreducens PCA-mediated methylation of Hg2+ and demethylation of MeHg was monitored by using double-enriched isotope tracing (199Hg2+ and Me201Hg). This automatic ethylation-purge and trap-GC-ICP-MS method is promising for routine MeHg analysis with isotope dilution/tracing.
      DOI: 10.46770/AS.2021.803
      U–Pb geochronology of carbonate by laser ablation multiple collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) is a rapidly growing research field due to its great potential to solve geological problems related to basin, tectonic, magmatism, and environmental evolution. In this paper, grid diagram was used to improve analytical efficiency. Two analytical modes of mixed collectors and multiple ion counting collectors were used on a Thermo Fisher Neptune Plus for carbonate U–Pb dating. Jet sample cone and X skimmer cone with Ar-N2 plasma (small addition of nitrogen into the sample gas flow) was used to enhance signal sensitivity of U and Pb. Our results showed that the sensitivity with Jet + X cones and adding nitrogen was a factor of two and eight greater than using standard sample cone and H skimmer cone in Ar-N2 plasma and Ar plasma, respectively. The fluence, repetition rate and spot size of the laser were investigated to assess effects on U–Pb results of different laser parameters. Medium energy fluences (~6 J/cm2) and medium ablation frequency (6 or 8 Hz) are suitable laser parameters for most samples to gain good U–Pb dating results for carbonate. Our new technique was evaluated by investigating five carbonate standards with U–Pb ages ranging from 2.4 to 254 Ma, in good agreement with their reference values. Our improved method was successfully applicable to date carbonate concretion, hydrothermal calcite vein, and peperite, which yielded new age results coinciding with stratigraphic relationship, structure analysis, and other dating methods.
      DOI: 10.46770/AS.2021.099
      Laser-induced breakdown spectroscopy (LIBS) was applied for the characterization of the methane-air laminar diffusion flame, revealing the spatial distribution of its composition. From the measurement, it was found that distribution of the atomic and ionic N emissions produced by the flame had obvious differences, which were mainly distributed in the air area and flame area, respectively. A comparison of the LIBS spectra of air, methane gas, and methane-air laminar diffusion flame showed that the atomic N emissions were mainly produced by the excitation of N2, and the ionic N emissions were more related to the N-containing combustion products. In addition, the correlation between typical emissions and the flame temperature measured by thermocouple was estimated to show that the tendency of the changes in temperature can be characterized by C2 emission intensities. This work provides a new method for real-time online flame temperature measurement, and also provides a reference for revealing the formation process and conversion pathway of each component in the flame.
      DOI: 10.46770/AS.2021.098
      Rare earth elements (REE) are important tools in geological studies. Accurate determination of REE concentrations can be affected in geological samples with low REE levels and/or high levels of interfering barium. Development of chemical separation methods allowing to isolate REE from other matrix components is a thorough approach to overcome this issue. In this study, a simple, RE resin-based separation method was developed and tested for a variety of sample solutions (mixed element solutions, shale, carbonate and granite). The method shows a good REE recovery and is efficient for the removal of matrix element, and notably Ba. The method is suitable for precise determination of the Eu contents in rock samples with high barium content.
      DOI: 10.46770/AS.2021.724
      With the increasing popularity of alternative breads, investigating their health benefits and risks is vitally important. The bioaccessibility of potentially toxic elements (PETs) in these breads could indicate a potential risk to consumers. The continuous online leaching method (COLM) involves the sequential leaching of a mini-column of food by artificial saliva, gastric juice, and intestinal fluid with real time monitoring of elements being released. Because the dissolution equilibrium is shifted to the right from continuous exposure to fresh reagent, it assesses bioaccessibility in three gastrointestinal matrices in less than 30 min and includes valuable kinetic extraction information. In this study, a gluten-free (GF) and a rye bread were analyzed for As, Cd, and Pb before and after toasting. Toasting lowered all PTE concentrations by a factor of 1.5 (As in rye bread) to 2.5 (Cd in rye bread). Most of the PTEs present were bioaccessible whether the bread was toasted or not. In the case of As, a significant portion is in the form of As(III) and As(V). COLM analysis allowed for Pb sourcing, revealing two potential sources of Pb being released separately in gastric juice from rye bread based on their significantly different 206Pb/207Pb and 208Pb/206Pb isotope ratios. Comparison with Pb ratios reported in previous literature revealed that some of the gastric-mobile Pb in rye bread came from the Pb historically added to gasoline in North America. This source completely vanished upon toasting rye bread.
      DOI: 10.46770/AS.2021.906
      A valid method for trace silver (Ag) detection in geological samples was developed in this study using aerosol dilution inductively coupled plasma-mass spectrometry after extraction with inverse aqua regia. This was proposed primarily to reduce the interference from Nb and Zr during mass spectrometric measurements. Almost 93% of Nb and Zr was removed after the extraction. By mixing an appropriate amount of Ar with the sample aerosol using an aerosol dilution system prior to plasma, the residual Nb oxides and Zr oxides or hydroxides could be successfully removed. The relative yields of the interfering oxides and hydroxides were as low as 0.087% (NbO/Nb) and 0.013% (ZrOH/Zr), which were 3–5 times lower than those in the traditional mode without the addition of Ar. Moreover, the signal-to-noise ratio of Ag was five times higher than that in the traditional mode. The proposed method was applied to the determination of Ag in 68 standard reference materials (SRMs) of soil, sediment, and rock. The results for 47 of these geological SRMs were in good agreement with the reference values. The Ag levels in three SRMs (GSP-2 Granodiorite, STM-2, and SGR-1b) are being reported for the first time herein. For these SRMs, 10 separate aliquots of the sample were digested and analyzed over a period of three months, and analysis revealed that the determined values were reasonable. Thus, the proposed method shows significant potential for the accurate determination of trace Ag in various geological samples.
      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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