• 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
    2023 SCIE IF: 3.4 (JCR, Q1)

          The ATOMIC SPECTROSCOPY is a peer-reviewed journal started in 1962 for PerkinElmer by Dr. Walter Slavin and now is published by Atomic Spectroscopy Press Limited (ASPL), Hongkong, P.R. China. It is intended for the rapid publication of both original paper and reviews in the fields of AAS, AFS, XRF, LIBS, ICP-OES, ICP-MS, GD-MS, TIMS, SIMS, AMS, electron microscopy and energy spectroscopy related microbeam analysis techniques, and Synchrotron radiation related technology,etc. Manuscripts dealing with (i) fundamentals & instrumentation development, (ii) novel methodology development & applications, (iii) sample preparation related technology, and (iv) standard reference materials development, can be submitted for publication. All published papers can be downloaded freely from the journal official website (www.at-spectrosc.com), and authors are not required to pay any publication fees (or APC).

     

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      Abstract:
      Space charge effects in the measurements by inductively coupled plasma mass spectrometry were investigated about groups 1, 2, and 13 of elements in the periodic table at various radio frequency (RF) power conditions and multiple extraction electrode-1 voltage conditions. Increased suppression of signal intensities was observed at an RF power over 1.1 kW with the increase of RF power, which was majorly attributed to space charge effects due to the increase in 40Ar+ density. A stronger negative extraction electrode-1 voltage resulted in stronger space charge effects. The extent of space charge effects decreased with the increase in mass-to-charge (m/z) ratio of the elements. The RF power at 0.8 kW to 0.9 kW can be a candidate condition for the measurements of elements with an m/z ratio under 100 at relatively higher sensitivity with much less space charge effects.
      Abstract:
      Oxygen isotopes provide crucial insights into abiotic and biotic processes. Modern geosciences increasingly demand the capability to concurrently obtain in-situ oxygen isotope ratios from multiple mineral phases within rock samples. However, this is often hindered by the absence of matrix-matched standards for all target minerals on the same sample mount. To address this issue, we conducted secondary ion mass spectrometry (SIMS) analyses to investigate the variation of relative instrumental mass fractionation (RIMF) between different phases across two consecutive sample switch sessions using a series of O-isotopic standards, including glass, quartz, calcite, monazite, zircon, olivine, and apatite. Our results for the first time demonstrate that the RIMF between any two standards remains consistent within typical SIMS analytical uncertainties across two consecutive mount switch sessions. This consistency of RIMF enables us to develop a novel "bridge crossing calibration" method. In this approach, a common "bridge" standard present in both the sample mount and standard mount is used to calibrate mount-to-mount bias. This approach, combined with a matrix-matched standard in the standard mount, allow us to obtain the IMF of unknown samples even when the sample mount lacks matrix-matched standards. Additionally, this method is time- and cost-efficient, minimizes the consumption of standard samples by reusing mounts containing multiple standards, and eliminates systematic deviations when measuring different minerals in different sessions. As such, it provides a universal and robust technique for oxygen isotope analysis using SIMS.
      Abstract:
      Determining non-metallic inclusions content and distribution are essential to bearing steel as they play decisive role on the fatigue life and the number of non-metallic inclusions increases when the steel size increases. The existing analysis methods have certain limitations with accurately quantify when it comes to analyzing inclusions in oversize metal. Based on the technique of Spark Mapping Analysis for Large Sample (SMALS), the Generalized Pareto After Normal Distribution Method (GPAND) has been developed to allow for the determination of the inclusions’ distributions of oversize metallic materials. This study presents the first evidence of using the generalized Pareto distribution's statistical function to analyze the spectral signals of non-metallic inclusions, employing peak fitting to merge the Normal and Generalized Pareto functions for assessing the spectral intensity of elements derived from high throughput spectral mapping technology. With GPAND method, the content and distribution of Al-inclusions and MnS inclusions are determined in the large size of bearing steel. It showed that the number of Al inclusions in sample 2-1 is higher than that in sample 2-2 and easily enriched towards the central region of the longitudinal section during solidification. The MnS inclusions in both samples are mostly located in the middle area of the longitudinal section and 1/4 L away from the edge. MnS inclusions in sample 2-2 is higher than that in sample 2-1. The evaluation of inclusion distribution can provide essential guidance for the production of ultra-clean and highly homogeneous metallic materials.
      Abstract:
      Deep-sea sediments are critical sinks for transition elements and rare earth elements (REE) in the modern ocean. The Cu-Fe-Zn isotopic composition of deep-sea sediments has emerged as an essential tool for tracing marine metal enrichment processes and biochemical cycles. However, significant differences in elemental composition exist between deep-sea sediments and traditional samples. The absence of targeted separation and purification processes, combined with the scarcity of corresponding reference materials for deep-sea sediments, may adversely affect the accuracy of analytical results. In this study, we selected a series of marine geologically relevant reference materials, including four self-developed REE-rich deep-sea sediment reference materials, as the research object to determine their Cu-Fe-Zn isotopic compositions. Building on prior work with AG-MP-1M resin for Cu, Fe, and Zn separation, we added an AG-1-X8 resin column for Co-rich deep-sea sediments, achieving complete Fe-Co separation with a stable, efficient method applicable to marine samples. The analytical precision of the Cu, Fe, and Zn isotopic compositions for all samples is better than ± 0.04% (2SD). We recommend that appropriate method and reference materials from this study be utilized for subsequent marine geological sample tests.
      Abstract:
      This paper presents a novel mechanistic explanation for microwave-assisted LIBS to mitigate self-absorption effects. A set of plasma characteristic equations in cylindrical coordinates, including plasma isothermal expansion and modified adiabatic expansion kinetics equations, were formulated. These equations were subsequently coupled with microwave electric field equations to develop a microwave energy-assisted model. These models were employed to numerically analyze the plasma dimensions, velocity, and spatial distribution characteristics of plasma concentration, as well as the energy consumption during plasma expansion and the microwave-assisted energy. This analysis aims to explain the self-absorption mechanism and uncover how microwave-assisted LIBS mitigates self-absorption. LIBS experiments, both with and without microwave assistance, were conducted. An improved Saha-Boltzmann planar method was proposed to quantify the degree of self-absorption in the spectral lines of Al, Si, and Ca. Based on the measured spectral data, the plasma temperature of Al was calculated using this improved method, while the electron densities of Si, Ca, and Al plasmas were determined independently of self-absorption effects, as no spectral line intensity information was involved. The evolution of plasma expansion was captured using an intensified charge-coupled device (ICCD). The experiments confirmed that microwave-assisted LIBS did not alter plasma electron temperature or electron density, but provides sufficient energy for uniform plasma expansion, thereby reducing self-absorption. This finding offers a theoretical reference for mitigating jitter following femtosecond laser wire formation. Furthermore, the experiments demonstrated that microwaves effectively reduce self-absorption and enhance spectral intensity, validating both the accuracy and feasibility of the plasma characteristic equations and the microwave energy-assisted model. These results provide theoretical guidance and experimental optimization for plasma characteristics in LIBS applications.
      Abstract:
      Tourmaline, a boron-rich mineral, serves as a robust tracer for fluid-mediated geological processes due to its chemical stability and resistance to environmental influence. Here, we present a novel data reduction scheme (DRS) LCG_B.py, integrated within the Iolite 4 program for in situ boron (B) isotope analysis of tourmaline to investigate fluid activities in subduction zones. The innovative approach enables direct observation of 11B and 10B signal variation during laser ablation, while treating the 11B/10B ratios of reference materials for calibration as a fitted timeseries curve (usually using Spline AutoSmooth), facilitating automated analysis and precise calibration of B isotope ratios across specified ablation interval. Based on this, a high-precision B isotopes analysis protocol achieving spot size below 30 μm with analytical uncertainty better than 0.5 ‰ (2sd) (except Schorl (NaFe3Al6[Si6O18](BO3)3(OH)4) of 0.7 ‰) was developed. Application of this method to tourmalines in ultrahigh-pressure (UHP) eclogites from the Dabie orogen showed positive δ11B values ranging from +4.7 ± 0.2 to +10.5 ± 0.3 ‰, derivation from B-rich fluids sourced from impure marbles. The findings provide refined constraints on fluid-mediated geological processes and enhance our understanding of the complex fluid-rock interactions in the continental subduction zones. The improved analytical protocol and data processing technique establish a powerful tool for future geochemical investigations of subduction zone dynamics.
      Abstract:
      Concentration of trace elements through TeCl4 volatilization in a flow reactor is presented for the first time and the potential of this approach for analysis was assessed. The method was developed for the multi-element analysis of high-purity Te. The matrix was volatilized through the reaction of Te with chlorine gas, which was obtained by the electrolysis of hydrochloric acid. The behavior of 61 trace elements during Te chlorination at 200–270 °С was studied. The maximum number of trace elements (39) quantitatively remained in the concentrate at a volatilization temperature of 240 °С. Trace element concentrations were analyzed using inductively coupled plasma optical emission spectrometry (ICP-OES). The limits of detection (LODs) of the 39 trace elements were 0.2–30 ng g–1. The possibility of reaching lower trace element LODs was demonstrated. For Ag, Cd, Mn, and Pd, the LODs were reduced by 3–25 times by using electrothermal atomic absorption spectrometry (ETAAS), with trace element LODs of 0.04–2 ng g–1. The precision of the matrix chemical volatilization procedure was evaluated using spike experiments. Recovery rates ranged from 80 to 119%. The analysis of a Te sample with unknown composition using ICP-OES and ETAAS methods after the proposed matrix chemical volatilization procedure gave comparable results to those obtained by ICP-OES without volatilization.
      Abstract:
      In this study, we present the novel use of a microwave digestion system (CEM BLADE) to digest geological materials for Re-Os isotopic analysis. This technique employs quartz digestion vessels that are easy to clean and reusable, avoid the complicated steps of opening and sealing, and enable complete digestion of the samples within 30 min at high temperature (max. 310℃) and pressure (max. 700 psi). The microwave digestion system was used to digest samples of four ultramafic rock reference materials (GBW07101, GBW07102, GBW07291, and WPR-1a), one basalt reference material (BIR-1a), and one black shale reference material (SGR-1b). The Re-Os isotope measurement results for GBW07291, BIR-1a, and SGR-1b were in agreement with previously published values, and we are the first to report Re-Os isotopes for GBW07101, GBW07102, and WPR-1a. Therefore, this new microwave digestion system is a simple, efficient, reliable, and safe sample digestion method for prospective applications in Re-Os isotopic analysis.
      Abstract:
      Although various methods have been developed for total organic carbon (TOC) analysis, most of them usually consume large amounts of samples, chemicals, and energy, thus making them only suitable for laboratory analysis. In this work, a new simple liquid electrode discharge microplasma-induced vapor generation (MPI-VG) was successfully developed to efficiently convert the organic compounds contained in water into CO2 on a microfluidic chip. Consequently, the generated CO2 was separated from the liquid phase and further swept into a miniature point discharge optical emission spectrometer (μPD-OES) for the detection of total organic carbon (TOC) in water samples via monitoring the carbon atom emission at 193.0 nm. Under optimal conditions, a limit of detection of 0.15 mg L?1 (as C) was obtained for TOC with a relative standard deviation better than 3.7%. The system is environmentally-friendly and efficient, which consumes only 43 μL of sample and 60 μg oxidant for each analysis. The total analytical time can be significantly reduced to one minute. The reaction mechanism was carefully investigated using quenching tests and gas chromatography. The practicality and anti-interference capabilities of the system were verified by measuring TOC in seawater and river water. Compared to conventional methods, this system demonstrates considerable potential for miniaturization due to the compact size of the microfluidic chip-based MPI-VG and μPD-OES.
      2024,45(6),448-455
      DOI: 10.46770/AS.2024.205
      Abstract:
      Atom probe tomography (APT) is a cutting-edge technology capable of imaging three-dimensional atom distribution and measuring chemical composition at the sub-nano scale. Since APT samples are tip-shaped and have specific size requirements, several manufacturing methods based on focused ion beam (FIB) have been developed. In order to precisely preserve the region of interests (ROI) into the tip and also satisfy the need of correlative characterization between crystallographic information and chemical information, we developed a new approach of directly fabricating APT tips from the twin-jet electropolished transmission electron microscopy (TEM) thin disc. This method has been successfully demonstrated on a Ni-B disc sample. After its nanocrystalline structure been observed by TEM, APT tips were prepared and analyzed from the selected region of the very-edge of the center hole. The distributions of major elements from the sample itself and induced by FIB processing were also discussed. This approach exhibits universal applications, which can not only feature in the correlation between TEM and APT analysis, but also benefit for the Ga-sensitive materials as only minimum FIB processing is required.
      2024,45(6),456-461
      DOI: 10.46770/AS.2024.156
      Abstract:
      An air-cooling torch was developed for argon-based inductively coupled plasma mass spectrometry (ICP-MS). The plasma gas aperture-width was decreased to 0.5 mm to permit the ignition of argon plasma at an RF power of 800 W with a plasma gas of 8.0 L/min. A stable argon plasma was achieved at an RF power up to 1,600 W by introducing 20 L/min of air as cooling-gas. The signal intensity of 89Y+ obtained with the present air-cooling torch at an RF power of 1,550 W and a plasma gas of 8.0 L/min argon was around 20 % higher than that obtained with a normal torch operated at normal condition. The ratio of oxide ion (<2.0 %) for Ce with the present torch was comparable to those obtained with a normal torch. Long-term stability (over 12 h) and the service life (over one year) of the present torch were also comparable to a normal torch.
      2024,45(6),462-472
      DOI: 10.46770/AS.2024.245
      Abstract:
      Duplex stainless steel Z3CN20-09M serves as the predominant material for the primary pipeline within the first circuit of pressurized water reactor (PWR) nuclear power plants. Its aging grade estimation plays a crucial role in ensuring the safety of the nuclear island infrastructure. To achieve this goal, fiber-laser-based laser-induced breakdown spectroscopy (FL-LIBS) was introduced as the non-destructive and in-situ rapid detection technique for aging grade estimation. The spectral signals laser-induced plasma properties, and laser ablation processes of various Z3CN20-09M specimens with different aging grades were analyzed together with their microstructure and metallography. It was found that the spectral signal intensities of the matrix element (Fe) and the alloying element (Cr) increased with increasing aging grade, which was well explained by the increase in plasma temperature and ablation mass. Most importantly, reliable linear relationships were obtained between the signal intensity ratios of Fe Ⅱ/Fe Ⅰ, Cr Ⅱ/Cr Ⅰ, and Fe Ⅰ/Cr Ⅰ, to the aging grades, with the coefficient of determination (R2) ranging from 0.94 to 0.99. These results demonstrate that FL-LIBS is a feasible method for aging grade estimation of the Z3CN20-09M from nuclear power plants.
      2024,45(6),473-480
      DOI: 10.46770/AS.2024.204
      Abstract:
      Inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) has the advantage of effective separation of spectral interference. Based on ICP-MS/MS technology, a method for the determination of ultra-trace levels of titanium in bearing steel was established by investigating the effects of spectral interference elimination in different collision/reaction modes (no gas, He, H2, and O2 modes). The spectral interference from Mo++ plasma on Ti+ was eliminated using the O2 mass-shift mode. Considering the signal intensity and signal-to-background ratio of the element to be measured, the optimal O2 flow rate was determined to be 15%. 45Sc was used as an internal standard to correct the influence of instrument fluctuations, and matrix interference was eliminated using the standard addition method. Under optimized conditions, a calibration curve for titanium was established. The mass fraction was in the range of 0.0001%–0.010%, the linear correlation coefficient was greater than 0.999, and the limit of detection values of the four isotopes ranged from 0.00001% to 0.00003%. The relative standard deviation (RSD) was less than 5.0% when steel samples with three additive levels were measured six times. The recovery of titanium ranged from 90.0% to 120.0%. This method is simple to use, easy to popularize, and meets the requirements for daily analysis. In addition, the critical value of titanium in high-quality bearing steel was evaluated by calculating the uncertainty.
      2024,45(6),481-489
      DOI: 10.46770/AS.2024.201
      Abstract:
      Insufficiently excited plasmas generated in aqueous media with incompressibility and high thermal conductivity result in an anisotropic optical emission. The emission characteristics of underwater plasmas produced from an immersed Cu plate acquired with backward and lateral detections were investigated by irradiating with short and long pulse LIBS, respectively. We found that the plasma emission collected backward shows clear emission lines with high intensities by using long pulses, while different types of spectral lines were exhibited at different wavelengths using short pulses, including Fraunhofer-type absorption and broadened emission lines. For the lateral emission, it was unfortunately no remarkable spectral lines observed with a short pulse. By contrast, absorption lines at the resonant atomic lines of Cu and three emission lines near the wavelength of 515 nm were obtained simultaneously with a long pulse. Consequently, a weak intensity and wide line broadening occur in the spectral lines with the short pulse, while a long pulse can notably provide an enhanced line intensity and narrow line broadening. Since backward and lateral emissions exhibit significant differences, the use of long pulses allows for better observation of Fraunhofer-type absorption spectra in the lateral direction and better observation of emission spectra in the backward direction. There is a remarkable enhancement for the emission lines collected from the backward than those of the lateral direction with the line intensity being increased by more than 17 times. Therefore, a desired spectrum can be obtained by combining the lateral and backward collection methods with a long pulse. These results not only contribute to a better understanding of the radiation mechanisms in backward and lateral directions of underwater plasmas, but especially facilitate the qualitative and quantitative analysis of underwater LIBS.
      2024,45(6),490-497
      DOI: 10.46770/AS.2024.277
      Abstract:
      The selection of an appropriate reference material is crucial for correcting instrument-induced mass discrimination and validating B and Sr isotopic determinations in laser-ablation multi-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) analyses. This study investigates the potential of a natural tourmaline as a reference material for B and Sr isotopic determinations. Major and trace element data showed that the HGL-3 tourmaline can be classified as dravite and belongs to the alkali group tourmaline. The HGL-3 tourmaline has high B contents (36830 to 43700 μg g-1), moderate Sr contents (216 to 260 μg g-1), and low Rb/Sr ratios (< 0.0013). In-situ LA-MC-ICP-MS analyses of the HGL-3 tourmaline yielded a mean δ11B value of -12.83 ± 0.38‰ (2SD, n = 485) and a mean 87Sr/86Sr ratio of 0.70835 ± 0.00019 (2SD, n = 515). These values are identical to those of powder samples determined by thermal ionization mass spectrometry (TIMS), which gave a mean δ11B value of -12.56 ± 0.24‰ (2SD, n = 6) and a mean 87Sr/86Sr ratio of 0.70833 ± 0.00004 (2SD, n = 8). The elemental and isotopic homogeneities suggest that the HGL-3 tourmaline can be used as a suitable reference material for LA-MC-ICP-MS B and Sr isotopic determinations in tourmaline.
      2024,45(6),498-507
      DOI: 10.46770/AS.2024.242
      Abstract:
      Three high-temperature and high-pressure sintered cassiterites doped with HfO2 were produced for use as potential reference materials for Hf isotopic analysis of cassiterite by laser ablation multi-collector inductively-coupled plasma mass spectrometry (LA-MC-ICP-MS). Ultrafine milled cassiterite powder particles (d50 = 6.3 μm) produced by wet milling were doped with HfO2 and subsequently sintered at high temperature and high-pressure to obtain homogeneous reference material for in-situ Hf isotope measurements. The sintered cassiterites have a homogeneous Hf isotopic composition at the 30 μm scale, as verified by solution nebulizer MC-ICP-MS analyses of Hf chemically separated from multiple mircodrilled sintered cassiterites, and 1065 laser ablation MC-ICP-MS analyses. The analytical results indicate a strong matrix e?ect between zircon and cassiterite during LA-MC-ICP-MS analysis. Due to low Yb and Lu contents, βHf rather than βYb was used to correct for 176Yb interference to obtain accurate 176Hf/177Hf ratios. The homogeneity of Hf isotopic compositions observed both within and between di?erent batches of sintered cassiterites suggests the potential utility of sintered cassiterite as a valuable tool for in situ isotope measurements and as an isotopic reference material.
      2024,45(6),508-515
      DOI: 10.46770/AS.2024.241
      Abstract:
      Respiration is an important index to evaluate the life status of organisms, thus monitoring respiration is of great significance. This study proposes a new methodology for non-invasive and real-time monitoring of organismal respiration based on laser-induced breakdown spectroscopy (LIBS). The study comprises two main components: dynamic monitoring and static analysis. In the dynamic monitoring section, LIBS is used to continuously detect and analyze multiple elements (C, H, O, and N) exhaled steadily by participants, with the carbon signal showing the closest correlation to the respiratory cycle. Fast Fourier Transform (FFT) is then applied to the carbon signal to achieve frequency domain analysis. Furthermore, it is also found that the presence of organismal respiration should be inferred from multiple element signals, rather than relying solely on the presence of carbon signal. In the static analysis, linear discriminant analysis (LDA) and backpropagation artificial neural networks (BP-ANN) are employed after LIBS measurement indicating the traceability of respiration sources is possible. This study offers a novel perspective on respiratory monitoring, demonstrating the potential of this method for real-time, convenient, and cost-effective respiration monitoring.
      2024,45(6),516-524
      DOI: 10.46770/AS.2024.276
      Abstract:
      The rapid and simultaneous analysis of cadmium (Cd) and mercury (Hg), as heavy metals known to be hazardous to public health, is always a challenge in complicated soil matrices. A novel solid sampling electrothermal vaporization atomic absorption spectrometry (SS-ETV-AAS) based on integrated catalytic pyrolysis technique was fabricated to develop a fast and sensitive method for the direct determination of Cd and Hg in soil. However, direct solid sampling of soil results in matrix interferences that affect the accurate analysis of Cd. In this work, modifier mixture of NaCl and citric acid (2:1 for soil: modifier) was optimized and employed to promote Cd release from soil for rapid and accurate detection, of which 30% citric acid (m:m) was added to alleviate soil coagulation at high temperatures. Under optimized conditions, the limits of detection (LODs) for Cd and Hg were 0.7 and 0.3 ng g-1 using sample size of 0.1 g. The linearity (R2) was both >0.999 and the recoveries were in the range of 81-115% with the relative standard deviation (RSD) 0.3-10.1%, showing excellent sensitivity, precision and accuracy. The complete analysis time can be controlled within ~3 min without any digestion process. The proposed method is suitable for the simultaneous detection of Cd and Hg in soil samples with features of simple, rapid and green.
      2024,45(6),525-531
      DOI: 10.46770/AS.2024.246
      Abstract:
      Investigating the spatial distribution of ultra-trace mercury (ng L-1) in volcanic and geothermal areas can provide insights into geological anomalies and regional volcanism. In this study, an accurate and precise method for Hg determination in geothermal water was developed using inductively coupled plasma tandem quadrupole mass spectrometry (ICP-MS/MS) and a collision/reaction cell (CRC). The experimental conditions, including the Hg isotope type and CRC gas, were optimized to eliminate severe tungsten oxide (WO) interference that occurs in conventional ICP-MS analysis of Hg. When O2 was used as the CRC gas in the MS/MS mode, the limit of quantitation (LOQ) for Hg was 0.5 ng L-1. The proposed method was successfully applied to the direct determination of Hg in a groundwater-certified reference material (ERM-CA615) and five geothermal water samples, two of which had a high W content. The satisfactory results indicate the significant potential of the proposed for determining ultra-trace levels of Hg in geological samples.
      2024,45(6),532-540
      DOI: 10.46770/AS.2024.053
      Abstract:
      The advent of laser ablation multi-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) has opened new avenues for investigating iron isotope cycling across various temporal and spatial scales in biological and geological processes. However, accurate and precise measurements of iron isotopes in hematite have been hindered by the lack of matrix-matched reference materials. In this study, we developed hematite reference materials (RMs) by combining nanopowder pelletization and solid-phase sintering techniques. Nano-Fe2O3 powder was compressed into pellets and subsequently sintered at 1000°C for 120 min. This method produced stable targets with sufficient mechanical strength suitable for in-situ analysis. The prepared hematite exhibited excellent cohesion, smooth surfaces, and dense structures, making it highly suitable for laser ablation analysis. We demonstrated the homogeneity of iron isotopic composition through repeated measurements using LA-MC-ICP-MS. The δ56FeIRMM014 values for the initial powder, sintered pellets, and unsintered pellets were 0.45 ± 0.04‰ (2SD, N=20), 0.44 ± 0.04‰ (2SD, N=21), and 0.45 ± 0.02‰ (2SD, n=3), respectively, indicating high consistency. The integration of pressed powder pellet techniques with high-temperature sintering provides a rapid and convenient method for developing matrix-matched RMs. This approach shows potential for creating diverse matrix-matched reference materials for various analytical applications.
      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.
      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.
      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.
      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.
      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.
      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.
      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.
      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.
      Abstract:
      Theory, design, and operation of a dynamic reaction cell for ICP-MS

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