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Sample records for double focusing icp-ms

  1. Titanium levels in the organs and blood of rats with a titanium implant, in the absence of wear, as determined by double-focusing ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Sarmiento-Gonzalez, Alejandro; Encinar, Jorge Ruiz; Marchante-Gayon, Juan M.; Sanz-Medel, Alfredo [University of Oviedo, Department of Physical and Analytical Chemistry, Faculty of Chemistry, Oviedo (Spain)

    2009-01-15

    Titanium (Ti) has long been regarded as an inert and biocompatible metal, ideal for biomedical applications such as dental implants or joint replacements. However, concerns about the biocompatibility of Ti have lately arisen. Unfortunately, information on reliable Ti baseline physiological levels in blood and organ tissues is still pending and the real effects of physiological corrosion as opposed to wear processes of Ti or Ti alloys implants is controversial so far. In this work a previously developed and validated methodology, based on using double-focusing inductively coupled plasma mass spectrometry (DF-ICP-MS) has been used to establish Ti basal levels in blood and organs (heart, liver, spleen, kidneys, and lungs) of Wistar rats. These data were compared with the levels found in three Wistar rats implanted with a Ti wire embedded in their femur for 18 months, in order to assign possible Ti released purely due to non-wear physiological mechanisms. Results showed that Ti content in all the selected organ tissues and blood was higher than previously determined Ti basal levels, clearly showing both corrosion of the Ti implant and systemic Ti accumulation in target tissues. These results indicate that Ti metal corrosion occurs. This seems to be the only mechanism responsible in the long term for the observed passive dissolution of Ti of the implant in the absence of wear. A comparative study of the systemic distribution of the soluble and particulate Ti potentially released from Ti implants was also carried out by intraperitoneally injection of soluble Ti(citrate){sub 3} and insoluble TiO{sub 2} particles, respectively. Different systemic Ti storage was observed. Whereas soluble Ti was rapidly transported to all distal organs under study, TiO{sub 2} particles were only accumulated in lung tissue. (orig.)

  2. Precise determination of Pb isotope ratios by simple double spike MC-ICP-MS technique without Tl addition

    Digital Repository Service at National Institute of Oceanography (India)

    Makishima, A.; Nath, B.N.; Nakamura, E.

    A double-spike multicollector ICP-MS (DS-MC-ICP-MS) technique for Pb isotope analysis without Tl addition is established and its analytical performance is examined in detail. This simple DS-MC-ICP-MS technique using 20 ng ml sup(-1) gave averages...

  3. Determination of trace elements in high pure rare earth oxide by double focusing inductively coupled plasma mass spectrometry (HR ICP-MS) and high performance liquid chromatography (HPLC) techniques

    International Nuclear Information System (INIS)

    Pedreira Filho, Walter dos Reis

    2000-01-01

    Rare earth oxides are used in several technological fields whose applications can be observed in several areas of modern technology, among which are included: lasers, semiconductors semi, high purity materials and metallic alloys. The field of applications of the rare earth elements is quite wide. Several important industrial applications are ceramics, catalysts and metallurgical as well as research areas and high technology sectors. Such applications have been presenting an accentuated growth in the last years. Chemical characterization of rare earth oxides of high purity has been constituting one of the major challenges of analytical chemistry. Several analytical techniques were used for chemical characterization of high purity rare earth the oxides. Even so, those techniques present limitations when one needs to characterize materials of a high level of purity, as in the case of rare earth oxides. Some of those limitations are associated, for example, to spectral interference. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a powerful analytical tool for quantitative analysis of metal impurities in high purity materials. The Instituto de Pesquisas Energeticas e Nucleares (IPEN) has an unit of production and purification of rare earth oxides, with above 99,9% level of purity. In this work, the rare earth impurities were characterized in samples (La 2 O 3 ; CeO 2 ; Pr 6 O 11 ; Nd 2 O 3 ; Sm 2 O 3 ; Gd 2 O 3 ; Y 2 O 3 ) produced at the IPEN and certified standard materials produced by Johnson Matthey Chemical (JMC). The technique of high performance liquid chromatography (HPLC) was used in the separation of the impurities. Quantification of metallic impurities was carried out as inductively coupled plasma mass spectrometer (HR-ICP MS). In this work it is presented a new analytical methodology in the chemical characterization of metallic impurities in rare earth oxides of high purity (> 99,9%) with and without separation of the matrix. Analyses of standard

  4. ICP-MS Workshop

    Energy Technology Data Exchange (ETDEWEB)

    Carman, April J. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Eiden, Gregory C. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2014-11-01

    This is a short document that explains the materials that will be transmitted to LLNL and DNN HQ regarding the ICP-MS Workshop held at PNNL June 17-19th. The goal of the information is to pass on to LLNL information regarding the planning and preparations for the Workshop at PNNL in preparation of the SIMS workshop at LLNL.

  5. An improved method for high precision measurement of chromium isotopes using double spike MC-ICP-MS

    Science.gov (United States)

    Zhu, J.; Wu, G. L.; Wang, X.; Zhang, L. X.; Han, G.

    2017-12-01

    Chormium(Cr) isotopes have been used to trace pollution processes and reconstruct paleo-redox conditions. However, the precise determination of Cr isotopes has still been challenged due to difficulties in purifying Cr from samples with low Cr content and complex matrices. Here we report an improved four-step column chromatographic procedure to separate Cr from matrix elements. Firstly, Cr in sample solution was mixed with 50Cr-54Cr double spike (the optimized 54Crspike/52Crsample = 0.4 and (50Cr/54Cr)spike = 1.3:1) was completely converted into Cr (III) in 8.5mol/L HCl and loaded onto 2ml of AG50W-X8(200-400m) resin conditioned with 11 mol/L HCl. The 2.65ml of eluent was adjusted to 4.5ml of 6mol/L HCl and immediately loaded onto a Bio-Rad column filled with 2ml of AG1-X8 anion resin (100-200m). These two steps can remove at least 99% of Ca, Fe and most matrix elements. Secondly, the 7.5ml of eluent was dried down and dissolved in 0.1ml of 0.5mol/L HNO3.before adding 2ml 4mol/L HF, which was then loaded onto 1ml of AG1-X8 anion resin (100-200m) to remove Ti and V. Finally, sample was dissolved in 0.1ml of 0.5 mol/L HNO3 and oxidized by 0.5mL 0.2 mol/L (NH4)2S2O8 and 4.4mL H2O, which was then centrifuged to remove Mn oxide, and supernatant was loaded onto AG1-X8 resin to remove SO42-, Ni, Al, Na and some Mg using 8ml H2O and 3ml 2mol/L HCl. Cr was eluted by 2 mol/L HNO3 containing 5% H2O2 and the dried Cr was dissolved in 3% HNO3for isotopic analysis. The total yield to Cr is great than 80% even for samples with low Cr content. Chromium isotopes was measured on a Neptune plus MC-ICP-MS in China University of Geosciences(Beijing). Using our improved method, the δ53/52CrSRM979 values of USGS reference materials BHVO-2, BCR-2 and SGR-1b are -0.12±0.06‰(n=15), -0.09±0.06‰ (n=5), and 0.30±0.06‰ (n=12), respectively, which agree well with previously reported values. The δ53/52CrSRM979 of carbonaceous shale CP0-1 and CP0-12 collected from Hubei, China are 2.05

  6. Analysis of Ba{sub x}Sr{sub y}TiO{sub 3} perovskite layers. II. Development of analytical method for the determination of the stoichiometry and trace impurities by ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, S.F. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen]|[Radiation Physics and Chemistry Problems Inst., Minsk (Belarus); Becker, J.S. [Forschungszentrum Juelich GmbH (Germany). Zentralabteilung fuer Chemische Analysen

    2000-11-01

    Determination of stoichiometry in semiconducting and non-conducting thin layers is of importance for the study of growth mechanisms and for the control of defects during their development and production. An analytical procedure for inductively coupled plasma mass spectrometry (ICP-MS) was developed using different ICP-MS instruments [one double-focusing sector field ICP-MS (DF-ICP-MS) and two quadrupole ICP-MS without and with hexapole collision cell (ICP-QMS and HEX-ICP-QMS, respectively)] for the determination of stoichiometry and trace impurities in thin Ba{sub x}Sr{sub y}TiO{sub 3} (BST) perovskite layers on silicon substrates after dissolution of layer. Maximum sensitivity, lowest detection limits and best precision was achieved in DF-ICP-MS. ICP-QMS with hexapole collision cell yielded better sensitivity and lower limits of detection in comparison to conventional quadrupole ICP-MS. (orig.)

  7. Double spike isotope dilution GC-ICP-MS for evaluation of mercury species transformation in real fish samples using ultrasound-assisted extraction.

    Science.gov (United States)

    Esteban-Fernández, Diego; Mirat, Manuela; de la Hinojosa, M Ignacia Martín; Alonso, J Ignacio García

    2012-08-29

    Sample preparation continues being a key factor to obtain fast and reliable quantification of Hg species. Assisted procedures enhance the efficiency and reduce the extraction time; however, collateral species transformations have been observed. Moreover, differential interconversions have been observed even between similar matrixes, which introduce an important uncertainty for real sample analysis. Trying to minimize Hg species transformations, we have tested a soft ultrasound-assisted extraction procedure. Species quantification and transformations have been evaluated using double spike isotope dilution analysis (IDA) together with gas chromatography inductively coupled plasma mass spectrometry (GC-ICP-MS) for a CRM material (Tort-2) and shark and swordfish muscle samples. Optimum extraction solution and sonication time led to quantitative extraction and accurate determination of MeHg and IHg in a short time, although different behaviors regarding species preservation were observed depending on the sample. Negligible species transformations were observed in the analysis of the CRM, while a small but significant demethylation factor was observed in the case of real samples. In comparison with other extraction procedures, species transformations became smaller, and fewer differences between fish species were found. Similar results were obtained for fresh and lyophilized samples of both fish samples, which permit one to analyze the fresh sample directly and save time in the sample preparation step. The high grade of species preservation and the affordability of the extraction procedure allow one to obtain accurate determinations even for routine laboratories using quantification techniques, which do not estimate species transformations.

  8. Performance of laser ablation. Quadrupole-based ICP-MS coupling for the analysis of single micrometric uranium particles

    International Nuclear Information System (INIS)

    Fabien Pointurier; Amelie Hubert; Anne-Claire Pottin

    2013-01-01

    In this paper we describe the application of laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) coupling to particle analysis, i.e., the determination of the isotopic composition of micrometric uranium particles. The performances of this analysis technique are compared with those of the two reference particle analysis techniques: secondary ion mass spectrometry (SIMS) and fission track-thermo-ionization mass spectrometry (FT-TIMS), based on the measurement of the isotopic ratios of 235 U/ 238 U in particles present in an inter-comparison particulate sample. The agreement of the results obtained using LA-ICP-MS with target values and with the results obtained using FT-TIMS and SIMS was good. Accuracy was equivalent to that of the other two techniques (±3 % deviation). However, relative experimental uncertainties present with LA-ICP-MS (7 %) were higher than those present with FT-TIMS (4.5 %) and SIMS (3 %). Furthermore, measurement yield of LA-ICP-MS coupling was close to that obtained with the same quadrupole ICP-MS for the measurement of a liquid sample (∼10 -4 ), but lower than that obtained with FT-TIMS and SIMS, respectively, by a factor of 10 and 20, although the particles analyzed using LA-ICP-MS were most likely smaller (diameter ∼0.6 μm, containing 4-7 fg of 235 U). Nevertheless, thanks to the brevity of the signals obtained, the detection capacity for low isotopic concentrations by LA-ICP-MS coupling is equivalent to that of FT-TIMS, although it remains well below that of SIMS (x 15). However, with more sensitive double focusing ICP-MS, performances equivalent to those achieved using SIMS could be obtained. (author)

  9. ICP-MS based methods to characterize nanoparticles of TiO2 and ZnO in sunscreens with focus on regulatory and safety issues.

    Science.gov (United States)

    Bocca, Beatrice; Caimi, Stefano; Senofonte, Oreste; Alimonti, Alessandro; Petrucci, Francesco

    2018-07-15

    This study sought to develop analytical methods to characterize titanium dioxide (TiO 2 ) and zinc oxide (ZnO) nanoparticles (NPs), including the particle size distribution and concentration, in cream and spray sunscreens with different sun protection factor (SPF). The Single Particle Inductively Coupled Plasma-Mass Spectrometry (SP ICP-MS) was used as screening and fast method to determine particles size and number. The Asymmetric Flow-Field Flow Fractionation (AF4-FFF) as a pre-separation technique was on-line coupled to the Multi-Angle Light Scattering (MALS) and ICP-MS to determine particle size distributions and size dependent multi-elemental concentration. Both methods were optimized in sunscreens in terms of recovery, repeatability, limit of detection and linear dynamic range. Results showed that sunscreens contained TiO 2 particles with an average size of ≤107 nm and also a minor number of ZnO particles sized ≤98 nm. The higher fraction of particles <100 nm was observed in sunscreens with SPF 50+ (ca. 80%); the lower percentage (12-35%) in sunscreens with lower SPF values. Also the higher TiO 2 (up to 24% weight) and ZnO (ca. 0.25% weight) concentrations were found in formulations of SPF 50+. Creamy sunscreens could be considered safe containing TiO 2 and ZnO NPs less than the maximum allowable concentration of 25% weight as set by the European legislation. On the contrary, spray products required additional considerations with regard to the potential inhalation of NPs. The developed methods can contribute to the actual demand for regulatory control and safety assessment of metallic NPs in consumers' products. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Fundamental and applied measurements in ICP MS

    International Nuclear Information System (INIS)

    Carter, Julian Robert

    2002-01-01

    Fundamental and applied aspects of ICP-MS have been investigated to gain an increased understanding of the technique and improve on its analytical capabilities. Dissociation temperatures of polyatomic ions were calculated using a double-focusing sector instrument, to obtain more reliable mass spectral data with controlled vapour introduction via a Dreschel bottle to allow accurate calculation of the ingredients in the plasma. The equilibrium temperature for the plasma, operated at 1280 W calculated using CO + and C 2 + as the thermometric probes, was c.a. 5800 - 7400 K, while using ArO + and ArC + as the thermometric probes the temperature calculated was c.a. 2000 - 7000 K. Calculated dissociation temperatures were used to elucidate the site of formation of these ions. Results confirmed that strongly bound ions such as CO + and C 2 + were formed in the plasma whereas weakly bound ions such as ArO + and ArC + were formed in the interface region due to gross deviation of the calculated temperatures from those expected for a system in thermal equilibrium. The use of helium gas in a hexapole collision cell attenuated the signals of ArH + Ar + , ArO + , ArC + , ArCl + and Ar 2 + allowing improved determination of 39 K + , 40 Ca + , 56 Fe + , 52 Cr + , 75 As + and 80 Se + in standard solutions. The use of the hexapole collision cell also resulted in an enhancement of analyte signals due to the thermalisation of the ion beam. The ion kinetic energy of ions sampled from the plasma and those sampled from the skimmer cone were determined using a modified lens stack to assess the significance for memory effects of material deposited on the skimmer cone. The most probable kinetic energy of Be + ions sampled from the skimmer cone was found to be 2.4 eV, which was considerably lower than the most probable kinetic energy of Be + ions sampled from the plasma, which was found to be 9.5 eV. The low kinetic energy of the ions deposited on the skimmer cone means they will only

  11. Fundamental and applied measurements in ICP MS

    Energy Technology Data Exchange (ETDEWEB)

    Carter, Julian Robert

    2002-07-01

    Fundamental and applied aspects of ICP-MS have been investigated to gain an increased understanding of the technique and improve on its analytical capabilities. Dissociation temperatures of polyatomic ions were calculated using a double-focusing sector instrument, to obtain more reliable mass spectral data with controlled vapour introduction via a Dreschel bottle to allow accurate calculation of the ingredients in the plasma. The equilibrium temperature for the plasma, operated at 1280 W calculated using CO{sup +} and C{sub 2}{sup +} as the thermometric probes, was c.a. 5800 - 7400 K, while using ArO{sup +} and ArC{sup +} as the thermometric probes the temperature calculated was c.a. 2000 - 7000 K. Calculated dissociation temperatures were used to elucidate the site of formation of these ions. Results confirmed that strongly bound ions such as CO{sup +} and C{sub 2}{sup +} were formed in the plasma whereas weakly bound ions such as ArO{sup +} and ArC{sup +} were formed in the interface region due to gross deviation of the calculated temperatures from those expected for a system in thermal equilibrium. The use of helium gas in a hexapole collision cell attenuated the signals of ArH{sup +} Ar{sup +}, ArO{sup +}, ArC{sup +}, ArCl{sup +} and Ar{sub 2}{sup +} allowing improved determination of {sup 39}K{sup +}, {sup 40}Ca{sup +}, {sup 56}Fe{sup +}, {sup 52}Cr{sup +}, {sup 75}As{sup +} and {sup 80}Se{sup +} in standard solutions. The use of the hexapole collision cell also resulted in an enhancement of analyte signals due to the thermalisation of the ion beam. The ion kinetic energy of ions sampled from the plasma and those sampled from the skimmer cone were determined using a modified lens stack to assess the significance for memory effects of material deposited on the skimmer cone. The most probable kinetic energy of Be{sup +} ions sampled from the skimmer cone was found to be 2.4 eV, which was considerably lower than the most probable kinetic energy of Be{sup +} ions

  12. ICP-MS measurement of natural radioactivity at LNGS

    Science.gov (United States)

    Nisi, S.; Copia, L.; Dafinei, I.; di Vacri, M. L.

    2017-10-01

    Rare events search experiments, like those dedicated to the direct evidence of dark matter or neutrinoless double beta decay, are among the most exciting challenges of modern physics. The sensitivity of such experiments is driven by the background, which depends substantially on the radiopurity of the materials used for the experimental apparatus. Cutting edge measurement techniques are needed for a fast, sensitive and efficient screening of these materials and the certification of their production. Trace element measurements of high sensitivity and quick execution are mandatory also in other fields like tracing the geographical origin of food, temporal and geographical assignment of cultural heritage or monitoring environmental radioactivity. This work is an overview of the inorganic mass spectrometry facility available at Gran Sasso National Laboratory (LNGS) for radiopure material screening and is especially focused on its ICP-MS instrumentation. Analytical methods developed to achieve lowest detection limits in different types of matrix, like metals, polymers, crystals and composite materials, are also indicated. Detection limits of 10-18gg-1 for 226Ra, 10-14gg-1 for U and Th and 10-12gg-1 for K are attained through dedicated operation conditions of the instrumentation. Details are given on the results obtained for different experiments ongoing or under construction at LNGS.

  13. Soil analyses by ICP-MS (Review)

    International Nuclear Information System (INIS)

    Yamasaki, Shin-ichi

    2000-01-01

    Soil analyses by inductively coupled plasma mass spectrometry (ICP-MS) are reviewed. The first half of the paper is devoted to the development of techniques applicable to soil analyses, where diverse analytical parameters are carefully evaluated. However, the choice of soil samples is somewhat arbitrary, and only a limited number of samples (mostly reference materials) are examined. In the second half, efforts are mostly concentrated on the introduction of reports, where a large number of samples and/or very precious samples have been analyzed. Although the analytical techniques used in these reports are not necessarily novel, valuable information concerning such topics as background levels of elements in soils, chemical forms of elements in soils and behavior of elements in soil ecosystems and the environment can be obtained. The major topics discussed are total elemental analysis, analysis of radionuclides with long half-lives, speciation, leaching techniques, and isotope ratio measurements. (author)

  14. New application and future of ICP-MS

    International Nuclear Information System (INIS)

    Masuda, Kimihiko

    1994-01-01

    By ICP-MS, since high sensibility, multi-element rapid analysis and isotope ratio analysis can be carried out, the position as the analysis for ultra-minute amount of elements has been established. Further recently, sample feeder system has been developed, and the multi-collector type device for the purpose of high resolution type isotope ratio analysis has appeared, so the range of its application is spreading more and more. In this report, the examples of application which were able to be attained accompanying the development of these devices are introduced, and the development of the ICP-MS hereafter is described. At present, about 1000 apparatuses are in operation in the world, and the application spread to the fields of semiconductors and materials, earth science, environment, atomic energy and so on. The ICP-MS was developed for the purpose of easily carrying out spectral analysis with high sensibility by using argon ICP as the ion source and doing ion detection which is more efficient than light detection, and has lower background. The progress and the present status of the ICP-MS are reported. As the latest examples of application of the ICP-MS, the analysis of iron by quadrupole type ICP-MS, the small region measurement of solids by laser abrasion, ultra-minute amount analysis by high resolution ICP-MS, the isotope ratio measurement of lead by multi-collector type ICP-MS are reported. (K.I.)

  15. Determination of phosphorus in small amounts of protein samples by ICP-MS.

    Science.gov (United States)

    Becker, J Sabine; Boulyga, Sergei F; Pickhardt, Carola; Becker, J; Buddrus, Stefan; Przybylski, Michael

    2003-02-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is used for phosphorus determination in protein samples. A small amount of solid protein sample (down to 1 micro g) or digest (1-10 micro L) protein solution was denatured in nitric acid and hydrogen peroxide by closed-microvessel microwave digestion. Phosphorus determination was performed with an optimized analytical method using a double-focusing sector field inductively coupled plasma mass spectrometer (ICP-SFMS) and quadrupole-based ICP-MS (ICP-QMS). For quality control of phosphorus determination a certified reference material (CRM), single cell proteins (BCR 273) with a high phosphorus content of 26.8+/-0.4 mg g(-1), was analyzed. For studies on phosphorus determination in proteins while reducing the sample amount as low as possible the homogeneity of CRM BCR 273 was investigated. Relative standard deviation and measurement accuracy in ICP-QMS was within 2%, 3.5%, 11% and 12% when using CRM BCR 273 sample weights of 40 mg, 5 mg, 1 mg and 0.3 mg, respectively. The lowest possible sample weight for an accurate phosphorus analysis in protein samples by ICP-MS is discussed. The analytical method developed was applied for the analysis of homogeneous protein samples in very low amounts [1-100 micro g of solid protein sample, e.g. beta-casein or down to 1 micro L of protein or digest in solution (e.g., tau protein)]. A further reduction of the diluted protein solution volume was achieved by the application of flow injection in ICP-SFMS, which is discussed with reference to real protein digests after protein separation using 2D gel electrophoresis.The detection limits for phosphorus in biological samples were determined by ICP-SFMS down to the ng g(-1) level. The present work discusses the figure of merit for the determination of phosphorus in a small amount of protein sample with ICP-SFMS in comparison to ICP-QMS.

  16. LA-ICP-MS of magnetite: Methods and reference materials

    Science.gov (United States)

    Nadoll, P.; Koenig, A.E.

    2011-01-01

    Magnetite (Fe3O4) is a common accessory mineral in many geologic settings. Its variable geochemistry makes it a powerful petrogenetic indicator. Electron microprobe (EMPA) analyses are commonly used to examine major and minor element contents in magnetite. Laser ablation ICP-MS (LA-ICP-MS) is applicable to trace element analyses of magnetite but has not been widely employed to examine compositional variations. We tested the applicability of the NIST SRM 610, the USGS GSE-1G, and the NIST SRM 2782 reference materials (RMs) as external standards and developed a reliable method for LA-ICP-MS analysis of magnetite. LA-ICP-MS analyses were carried out on well characterized magnetite samples with a 193 nm, Excimer, ArF LA system. Although matrix-matched RMs are sometimes important for calibration and normalization of LA-ICP-MS data, we demonstrate that glass RMs can produce accurate results for LA-ICP-MS analyses of magnetite. Cross-comparison between the NIST SRM 610 and USGS GSE-1G indicates good agreement for magnetite minor and trace element data calibrated with either of these RMs. Many elements show a sufficiently good match between the LA-ICP-MS and the EMPA data; for example, Ti and V show a close to linear relationship with correlation coefficients, R2 of 0.79 and 0.85 respectively. ?? 2011 The Royal Society of Chemistry.

  17. Accurate determination of ultra-trace levels of Ti in blood serum using ICP-MS/MS

    International Nuclear Information System (INIS)

    Balcaen, Lieve; Bolea-Fernandez, Eduardo; Resano, Martín; Vanhaecke, Frank

    2014-01-01

    Graphical abstract: -- Highlights: •Novel method for determination of Ti at ultra-trace levels in clinical samples (serum). •Novel method based on Ti(NH 3 ) 6 + reaction product ion formation and double mass selection using recently introduced ICP-QQQ instrumentation. •Lowest limits of detection ever obtained using quadrupole-based instrumentation for Ti. •Accurate determination of basal levels of Ti in blood serum. -- Abstract: Ti is frequently used in implants and prostheses and it has been shown before that the presence of these in the human body can lead to elevated Ti concentrations in body fluids such as serum and urine. As identification of the exact mechanisms responsible for this increase in Ti concentrations, and the risks associated with it, are not fully understood, it is important to have sound analytical methods that enable straightforward quantification of Ti levels in body fluids (for both implanted and non-implanted individuals). Until now, only double-focusing sector field ICP-mass spectrometry (SF-ICP-MS) offered limits of detection that are good enough to deal with the very low basal levels of Ti in human serum. This work reports on the development of a novel method for the accurate and precise determination of trace levels of Ti in human serum samples, based on the use of ICP-MS/MS. O 2 and NH 3 /He have been compared as reaction gases. While the use of O 2 did not enable to overcome all spectral interferences, it has been shown that conversion of Ti + ions into Ti(NH 3 ) 6 + cluster ions by using NH 3 /He as a reaction gas in an ICP-QQQ-MS system, operated in MS/MS mode, provided interference-free conditions and sufficiently low limits of detection, down to 3 ng L −1 (instrumental detection limit obtained for the most abundant Ti isotope). The accuracy of the method proposed was evaluated by analysis of a Seronorm Trace Elements Serum L-1 reference material and by comparing the results obtained with those achieved by means of SF-ICP-MS

  18. Precise and accurate isotope ratio measurements by ICP-MS.

    Science.gov (United States)

    Becker, J S; Dietze, H J

    2000-09-01

    The precise and accurate determination of isotope ratios by inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) is important for quite different application fields (e.g. for isotope ratio measurements of stable isotopes in nature, especially for the investigation of isotope variation in nature or age dating, for determining isotope ratios of radiogenic elements in the nuclear industry, quality assurance of fuel material, for reprocessing plants, nuclear material accounting and radioactive waste control, for tracer experiments using stable isotopes or long-lived radionuclides in biological or medical studies). Thermal ionization mass spectrometry (TIMS), which used to be the dominant analytical technique for precise isotope ratio measurements, is being increasingly replaced for isotope ratio measurements by ICP-MS due to its excellent sensitivity, precision and good accuracy. Instrumental progress in ICP-MS was achieved by the introduction of the collision cell interface in order to dissociate many disturbing argon-based molecular ions, thermalize the ions and neutralize the disturbing argon ions of plasma gas (Ar+). The application of the collision cell in ICP-QMS results in a higher ion transmission, improved sensitivity and better precision of isotope ratio measurements compared to quadrupole ICP-MS without the collision cell [e.g., for 235U/238U approximately 1 (10 microg x L(-1) uranium) 0.07% relative standard deviation (RSD) vs. 0.2% RSD in short-term measurements (n = 5)]. A significant instrumental improvement for ICP-MS is the multicollector device (MC-ICP-MS) in order to obtain a better precision of isotope ratio measurements (with a precision of up to 0.002%, RSD). CE- and HPLC-ICP-MS are used for the separation of isobaric interferences of long-lived radionuclides and stable isotopes by determination of spallation nuclide abundances in an irradiated tantalum target.

  19. The determination of cadmium, lead and vanadium by high resolution ICP-MS in Antarctic snow samples

    Energy Technology Data Exchange (ETDEWEB)

    Lanza, F. [Joh. Gutenberg Univ., Mainz (Germany). Inst. fuer Anorganische und Analytische Chemie; Trincherini, P. [European Union Joint Research Centre, Ispra, VA (Italy). Inst. of Environment

    2000-02-01

    Double focusing ICP-MS was successfully used in this research for the direct determination of the cadmium, lead and vanadium content of a set of Antarctic samples collected during the 11. Italian Expedition to Antarctica. For cadmium and lead measurements the low resolution mode was chosen since it ensured the highest ion sensitivity and it allowed the highest detection limits to be attained; in the case of vanadium the high resolution mode was used to solve the isobaric interference. As far as vanadium and cadmium are concerned by GFAAS coupled with different preconcentration procedures. The vanadium, cadmium and lead content measured in a riverine water reference material (SRLS-3) was found in agreement with the certified values. [Italian] Si e' utilizzato uno spettrometro ICP-MS a doppia focalizzazione per la determinazione diretta di cadmio, piombo e vanadio in una serie di campioni di neve antartica superficiale raccolta durante l'undicesima spedizione italiana in Antartide. Per le determinazioni di cadmio e piombo si e' scelta la procedura a bassa risoluzione, che ha garantito la piu' elevata sensibilita' ed ha permesso di ottenere limiti di determinazione migliori; nel caso del vanadio si e' utilizzata la procedura ad alta risoluzione che ha permesso di risolvere problemi di interferenza isobarica. Per quanto riguarda cadmio e vanadio, i risultati delle determinazioni mediante ICP-MS sono risultati in buon accordo con quelli ottenuti mediante GFAAS accoppiata a diverse procedure di preconcentrazione. Il contenuto di cadmio, piombo e vanadio misurato con le procedure sviluppate in un campione certificato di acqua di fiume (SRLS-3) e' risultato in accordo con i valori certificati.

  20. Practical guide to ICP-MS: a tutorial for beginners

    National Research Council Canada - National Science Library

    Thomas, Robert

    2013-01-01

    ... for those with limited knowledge of the technique. Written by an insider with more than 20 years experience in product development, customer support, and technical marketing for an ICP-MS instrument vendor, the book highlights this powerful ultra...

  1. ICP MS selection of radiopure materials for the GERDA experiment

    Science.gov (United States)

    di Vacri, M. L.; Nisi, S.; Cattadori, C.; Janicsko, J.; Lubashevskiy, A.; Smolnikov, A.; Walter, M.

    2015-08-01

    The GERDA (GERmanium Detector Array) experiment, located in the Gran Sasso Underground Laboratory (LNGS, Italy) aims to search for neutrinoless double beta (0νββ) decay of the 76Ge isotope. Both an ultra-low radioactivity background environment and active techniques to abate the residual background are required to reach the background index (of 10-3 counts/keV kg y) at the Qββ. In order to veto and suppress those events that partially deposit energy in Ge detectors, the readout of liquid argon (LAr) scintillation light (SL) has been implemented for the second GERDA experimental Phase. A double veto system has been designed and constructed using highly radiopure materials (scintillating fibers, wavelength shifters, polymeric foils, reflective foils). This work describes the study of lead, thorium and uranium ultra-trace content, performed at the LNGS Chemistry Laboratory by High Resolution Mass Spectrometry (HR ICP MS), for the selection of all materials involved in the construction of the veto system

  2. ICP MS selection of radiopure materials for the GERDA experiment

    Energy Technology Data Exchange (ETDEWEB)

    Di Vacri, M. L., E-mail: divacrim@lngs.infn.it [INFN, Laboratori Nazionali del Gran Sasso, via G.Acitelli 22, 67100 Assergi (Italy); Dipartimento di Scienze Fisiche e Chimiche, University of L’Aquila, via Vetoio, 67100 L’Aquila (Italy); Nisi, S., E-mail: nisi@lngs.infn.it [INFN, Laboratori Nazionali del Gran Sasso, via G.Acitelli 22, 67100 Assergi (AQ) (Italy); Cattadori, C., E-mail: cattadori@lngs.infn.it [INFN Sezione di Milano Bicocca, Milano (Italy); Janicsko, J. [TUM Munich (Germany); Lubashevskiy, A. [MPIK, Heidelberg (Germany); JINR, Dubna (Russian Federation); Smolnikov, A. [MPIK, Heidelberg (Germany); Walter, M. [Physik-Institut, Universitat Zurich, 8057 Zurich (Switzerland)

    2015-08-17

    The GERDA (GERmanium Detector Array) experiment, located in the Gran Sasso Underground Laboratory (LNGS, Italy) aims to search for neutrinoless double beta (0νββ) decay of the {sup 76}Ge isotope. Both an ultra-low radioactivity background environment and active techniques to abate the residual background are required to reach the background index (of 10{sup −3} counts/keV kg y) at the Q{sub ββ}. In order to veto and suppress those events that partially deposit energy in Ge detectors, the readout of liquid argon (LAr) scintillation light (SL) has been implemented for the second GERDA experimental Phase. A double veto system has been designed and constructed using highly radiopure materials (scintillating fibers, wavelength shifters, polymeric foils, reflective foils). This work describes the study of lead, thorium and uranium ultra-trace content, performed at the LNGS Chemistry Laboratory by High Resolution Mass Spectrometry (HR ICP MS), for the selection of all materials involved in the construction of the veto system.

  3. Inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Shimamura, Tadashi

    1997-01-01

    The period of investigation for the previous general remarks on the progress of ICP-MS was from January, 1991 to September, 1993. In the investigation of this time, for the object of the Chemical Abstracts from January, 1994 to September, 1996, retrieval was carried out by using the STN International. As the key words, ICP-MS, Inductively Coupled Plasma Mass Spectrometry or Inductively Coupled Plasma Mass Spectrometer was used. The number of hit was 373 in 1994, 462 in 1995, and 356 as of September, 1996, 1191 in total. The cumulative number of the papers from 1980 to 1996 is shown. It is known how rapidly the ICP-MS has pervaded as the means of analysis. In order to cope with the enormous number of papers, this time, it was decided to do the review by limiting to the papers which were published in the main journals deeply related to analytical chemistry. As to the tendency in the last three years, it is summarized as how to overcome the spectrum interference and matrix effect in the ICP-MS and the trend of using the ICP-MS as the high sensitivity detector for separation techniques. The technical basic research of the ICP-MS on spectrum interference, sample introduction method and others and the analysis of living body samples are reported. (K.I.)

  4. Separation of Pu from soil prior to determination by ICP-MS

    International Nuclear Information System (INIS)

    Nygren, U.; Baxter, D.C.

    2002-01-01

    In the determination of plutonium in environmental materials by ICP-MS, chemical separation is often needed to remove, e.g., heavy sample matrices and interference from UH + on m/z 239. This separation can be, and often is, performed in the same way as for alpha-spectrometric analysis. There are, however, somewhat different demands on separation for ICP-MS compared to alpha-spectrometry, but so far little has been published on the optimisation of separation procedures for plutonium determination by ICP-MS. This paper describes the development of a separation procedure especially suited for the determination of Pu by ICP-MS. Focus has been on parameters such as chemical yield of plutonium and decontamination from uranium, as well as time requirements and ease of performance. The separation of plutonium was performed using various resins, such as anion exchange resin and extraction chromatographic materials. The procedures were carried out on water spiked with 238 U and 240 Pu to concentrations of approximately 300 ppb and 50 ppt, respectively. The basic separation procedure was: 1. Adjustment of oxidation state for Pu 2. Loading on column 3. Rinsing using 4*5 free column volumes (FCVs) of load solution - if needed in combination with 1*5 FCVs of an other rinsing agent 4. Elution of Pu - if needed followed by evaporation and dissolution in a solution suitable for ICP-MS determination 5. Determination by high resolution ICP-MS The elution of plutonium was performed using various media, based on either reduction of Pu(IV) to Pu(III) or complex formation. The chemical yield of plutonium and the decontamination from uranium for various resin/elution combinations can be seen in Figs. 1 and 2. It was found that the most efficient separation procedure in terms of yield and uranium decontamination was the combination of two extraction chromatographic materials, UTEVA followed by TRU, and elution of Pu by 0.1 % 1-hydroxyethane-1,1-diphosphonic acid (HEDPA). In this procedure

  5. Laser ablation ICP-MS for quantitative biomedical applications

    International Nuclear Information System (INIS)

    Konz, Ioana; Fernandez, Beatriz; Fernandez, M.L.; Pereiro, Rosario; Sanz-Medel, Alfredo

    2012-01-01

    LA-ICP-MS allows precise, relatively fast, and spatially resolved measurements of elements and isotope ratios at trace and ultratrace concentration levels with minimal sample preparation. Over the past few years this technique has undergone rapid development, and it has been increasingly applied in many different fields, including biological and medical research. The analysis of essential, toxic, and therapeutic metals, metalloids, and nonmetals in biomedical tissues is a key task in the life sciences today, and LA-ICP-MS has proven to be an excellent complement to the organic MS techniques that are much more commonly employed in the biomedical field. In order to provide an appraisal of the fast progress that is occurring in this field, this review critically describes new developments for LA-ICP-MS as well as the most important applications of LA-ICP-MS, with particular emphasis placed on the quantitative imaging of elements in biological tissues, the analysis of heteroatom-tagged proteins after their separation and purification by gel electrophoresis, and the analysis of proteins that do not naturally have ICP-MS-detectable elements in their structures, thus necessitating the use of labelling strategies. (orig.)

  6. Applications of ICP-MS in marine analytical chemistry

    Energy Technology Data Exchange (ETDEWEB)

    McLaren, J W; Siu, K W.M.; Lam, J W; Willie, S N; Maxwell, P S; Palepu, A; Koether, M; Berman, S S [National Research Council of Canada, Ottawa, ON (Canada). Analytical Chemistry Section

    1990-07-01

    The versatility of ICP-MS in marine analytical chemistry is illustrated with applications to the multielement trace analysis of two recently released marine reference materials, the coastal seawater CASS-2 and the non-defatted lobster hepatopancreas tissue LUTS-1, and to the determination of tributyltin and dibutyltin in the harbour sediment reference material PACS-1 by HPLC-ICP-MS. Seawater analyses were performed after separation of the trace elements either by adsorption on immobilized 8-hydroxyquinoline or by reductive coprecipitation with iron and palladium. Simultaneous determination of seven trace elements in LUTS-1, including mercury, by isotope dilution ICP-MS, was achieved after dissolution by microwave digestion with nitric acid and hydrogen peroxide. Butyltin species in PACS-1 were separated by cation exchange HPLC of an extract of the sediment; method detection limits for tributyltin and dibutyltin in sediment samples are estimated to be 5 ng Sn/g and 12 ng Sn/g, respectively. (orig.).

  7. Analysis of nanoparticles using the ICAP Q ICP-MS

    DEFF Research Database (Denmark)

    Kutscher, Daniel; McSheehy-Ducos, Shona; Lindemann, Torsten

    2014-01-01

    The analysis of Nanoparticles (NPs) has become one of the hot topics in analytical chemistry. However, detailed knowledge about potential risks or hazards is still unavailable. Two approaches have been developed in recent years using ICP-MS as a detection system: hyphenation of an appropriate...... separation technique like Field-Flow-Fractionation (FFF), or direct analysis using spICP-MS. The separation of particles and particle mixtures using FFF is based on the differing mobilities of different particle sizes in a laminar liquid flow. FFF is compatible for particle sizes in the low nm to low μm...... range and is thus perfectly suited for the separation of different NPs. Combined with other detection systems such as dynamic light scattering, it can provide also additional information about the particles of interest, like shape. In comparison, spICP-MS is able to analyze NPs directly based...

  8. ICP-MS analysis for long-lived radionuclides

    International Nuclear Information System (INIS)

    Roos, P.

    2010-01-01

    Full text: Inductively coupled plasma mass spectrometry (ICP-MS) is an attractive alternative for the analysis of radioisotopes having a half-life in the order of several hundred years and above. The technique should not be considered a replacement for radiometric measurements of these isotopes but merely an alternative. Similarly to radiometric techniques like alpha and beta spectrometry most analysis of 'low-level' concentrations by ICP-MS requires chemical isolation of the element in question. For 'ultra-low-level' concentrations this clean-up of the sample is usually even more necessary than for the alternative radiometric techniques. The presentation gives an overview of advantages and disadvantages in using ICP-MS and compares it to relevant radiometric alternatives. (author)

  9. ICP-MS and elemental tags for the life sciences

    Energy Technology Data Exchange (ETDEWEB)

    Giesen, Charlotte

    2012-08-07

    Inductively coupled plasma mass spectrometry (ICP-MS) has been applied for the analysis of biomolecules due to its high sensitivity, wide linear dynamic range, and multielement capabilities. However, outside the elemental MS community the potential of this technique, e.g. for life sciences applications, is not yet fully exploited. Thus, the development of ICP-MS-based (immuno) assays for a wide range of medical (cancer diagnostics, cisplatin toxicity studies), biochemical (DNA microarray, single cell analysis), and environmental (analysis of comestible goods) applications was accomplished by utilization of chemical labels. Laser ablation (LA)-ICP-MS was employed for the direct analysis of solid samples like microarrays and thin tissue sections. An immunoassay was developed for ochratoxin A (OTA) determination in wine, and ICP-MS detection was compared to conventional photometry by gold nanoparticle tagging and horseradish peroxidase, respectively. Detection limits of the assay were optimized to 0.003 {mu}g L{sup -1}, and the quantification range was 0.01-1 {mu}g L{sup -1} for both methods. For LA-ICP-MS-based DNA microarray detection, gold nanoparticle tags were specifically introduced via a streptavidin-biotin linkage. In immunohistochemistry (IHC), up to 20 tumor markers are routinely evaluated for one patient and thus, a common analysis results in a series of time consuming staining procedures. Hence, LA-ICP-MS was elaborated as a detection tool for a novel, multiplexed IHC analysis of tissue sections. Different lanthanides were employed for the simultaneous detection of up to three tumor markers (Her 2, CK 7, and MUC 1) in a breast cancer tissue. Additionally, iodine was employed as a labeling reagent, and a new LA-ICP-MS method for single cell and cell nucleus imaging was developed at 4 {mu}m laser spot size. Iodine was also applied as a new internal standard for tissue samples. Moreover, Pt-protein complexes separated by an optimized 1D and 2D gel

  10. Determination of rhenium traces in river water by Q-ICP-MS and HR-ICP-MS

    International Nuclear Information System (INIS)

    Uchida, S.; Tagami, K.; Saito, M.

    2003-01-01

    A simple separation method was applied to determine rhenium in river water using Q-ICP-MS and HR-ICP-MS. Re was concentrated from 420-925 ml river water using a TEVA resin minicolumn. Such extraction using a resin could separate Re from most sample matrices and trace elements. Almost 100% recovery was found throughout the method as determined with radioactive multitracers. The HR-ICP-MS was also used for the direct determination because of its low detection limit for Re (0.007 pg/ml). The Re concentration in the river water samples ranged from 0.9 to 6.5 pg/ml and the three analysis results showed good agreement with each other. (author)

  11. Determination of neptunium in soil by ICP-MS

    International Nuclear Information System (INIS)

    Ayranov, M.; Kraehenbuehl, U.

    2005-01-01

    A fast and simple method for the determination of 237 Np in soil is presented. The borate fusion decreases the sample pre-treatment time and a TEVA extraction chromatography separates neptunium from uranium and the interfering matrix components. A comparison of the sensitivities of alpha spectrometry and sector field ICP-MS for determination of 237 Np is presented. (orig.)

  12. Some practical applications of an ICP-MS instrument

    International Nuclear Information System (INIS)

    Meddings, B.; Ng, R.

    1987-01-01

    An early model commercial ICP-MS instrument (PlasmaQuad from VG Isotopes Limited) was acquired more than two years ago. As a typical analytical laboratory in the metallurgical field, the application of the ICP-MS technique to real sample analysis is the authors prime concern. The process of introducing this state-of-the-art instrument into routine analysis will be described. The modifications and limitations necessary to achieve acceptable precision under normal working conditions will be outlined. In most cases, practical problems can be circumvented with some sacrifice in analytical performance in the area of detection limits and dynamic range. In this presentation, specific applications of the ICP-MS technique in the authors laboratory will be discussed. These include trace analysis on high purity metals such as copper, aluminum, cobalt, nickel etc., on refinery feed samples such as nickel sulfate, mixed cobalt and nickel sulfide, cobalt cathode, samarium oxide etc., on alloys such as cobalt-samarium magnetic materials, nickel or cobalt based alloys used in turbine blades etc. Other applications such as the determination of uranium in phosphate rock, trace analysis on fertilizers, water samples and high purity acids will also be mentioned. The solutions to the practical problems encountered in these applications will be discussed. The analytical power of the ICP-MS technique for real sample analysis will be assessed

  13. Quality control of Al alloy by ICP-MS

    International Nuclear Information System (INIS)

    Zahran, N.F.; Amr, M.A.; Helal, A.I.; Waly, S.A.; Afifi, Y.K.

    2000-01-01

    Laser ablation sample introduction system in combination with an inductive coupled plasma mass spectrometer (ICP-MS) is used for the investigation of elemental distribution of Al alloy. The samples are ablated by an ultraviolet laser beam at 266 nm with an energy of 4mJ/shot at a repetition rate of 20 Hz. Samples are digested using HNO 3 in a microwave system and analyzed in a solution form by ICP-MS. The quantification of the analytical results is carried out using multielement solution. Quantitative data from the solution samples are used as a standard data for the laser ablation technique. The effect of Aluminum as a matrix is studied. High-resolution mass spectrometer is used to identify the Aluminum polyatomic ions in the ICP-ion source

  14. Fundamental studies of interferences in ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Rowley, L.K

    2000-11-01

    Methods of temperature measurement by mass spectrometry have been critically reviewed. It was concluded that the most appropriate method depended critically on the availability of fundamental data, hence a database of fundamental spectroscopic constants, for diatomic ions which cause interferences in ICP-MS, was compiled. The equilibration temperature, calculated using the different methods and using various diatomic ions as the thermometric probes, was between c.a. 400 - 10,000 K in the central channel, and between c.a. 600 - 16,000 K when the plasma was moved 1.8 mm off-centre. The wide range in temperature reflected the range of temperature measurement methods and uncertainty in the fundamental data. Optical studies using a fibre optic connected to a monochromator were performed in order to investigate the presence of interferences both in the plasma and the interface region of the ICP-MS, and the influence of a shielded torch on these interferences. It was possible to determine the presence of some species in the plasma, such as the strongly bound metal oxides, however, no species other than OH were detected in the interface region of the ICP-MS. The OH rotational temperature within the interface region of the ICP-MS was calculated to be between 2,000 - 4,000 K. The effect of sampling depth, operating power, radial position and solvent loading, with and without the shielded torch, on the dissociation temperature of a variety of polyatomic interferences was investigated. These calculated temperatures were then used to elucidate the site of formation for different polyatomic interferences. Results confirmed that strongly bound ions such as MO{sup +} were formed in the plasma, whereas weakly bound ions such as ArO{sup +} were formed in the interface region due to gross deviation of the calculated temperatures from those expected for a system in thermal equilibrium. (author)

  15. Elemental Analysis in Biological Matrices Using ICP-MS.

    Science.gov (United States)

    Hansen, Matthew N; Clogston, Jeffrey D

    2018-01-01

    The increasing exploration of metallic nanoparticles for use as cancer therapeutic agents necessitates a sensitive technique to track the clearance and distribution of the material once introduced into a living system. Inductively coupled plasma mass spectrometry (ICP-MS) provides a sensitive and selective tool for tracking the distribution of metal components from these nanotherapeutics. This chapter presents a standardized method for processing biological matrices, ensuring complete homogenization of tissues, and outlines the preparation of appropriate standards and controls. The method described herein utilized gold nanoparticle-treated samples; however, the method can easily be applied to the analysis of other metals.

  16. Lead isotope measurements on aerosol samples with ICP-MS

    International Nuclear Information System (INIS)

    Widmer, C.R.; Kraehenbuehl, U.; Kramers, J.; Tobler, L.

    2000-01-01

    Size fractionated aerosols were collected with low pressure Berner impactors on a radio/TV tower 110 m above ground on a hill 10 km east of Bern at a total elevation of 1060 m asl. Two different wind sectors were chosen with the goal of assessing any differences in lead concentration and the 3 radiogenic lead isotopes (206,207,208) for east and west wind, respectively. A leaching technique was used to extract the lead quantitatively from the surface of the impaction foils. This method has been proven to be better suited for airborne particles than complete microwave digestion because it is less time consuming and contamination risk is smaller. Blank considerations played a major role in choosing all the chemicals, tubes, beakers and selecting the analytical method. Lead concentrations were determined with GF-AAS and lead isotopes with two different ICP-MS systems, one being a multicollector system. Precision of the simultaneous multicollector system was found to be at least a factor of 3 better than that of the sequentially operating ICP-MS. The small variations in isotope ratios from the two wind sectors can be distinctly seen with this enhanced precision. The observed relative difference in isotope ratios between east- and westwind was ∝0.6% for 207 Pb/ 206 Pb and ∝0.5% for 208 Pb/ 206 Pb. (orig.)

  17. Development and application of a calibration technique for laser ablation - ICP - MS

    Energy Technology Data Exchange (ETDEWEB)

    Boue-Bigne, F

    2000-08-20

    Laser Ablation - Inductively Coupled Plasma - Mass Spectrometry (LA-ICP-MS) is a powerful analytical technique for the direct elemental analysis of solid samples, with spatial resolution down to a few microns. However, calibration remains the limiting factor in obtaining quantitative analysis by LA-ICP-MS for a wide range of sample types. No universal method exists as yet and the ones that are currently used tend to employ matrix-matched solid standards. Matrix-matched solid standards are not available for many types of sample, such as polymers, biological materials, fluid inclusions, etc. The need for a universal method of calibration that involves standards that are easy to prepare and suitable for any type of sample is required. Additional to matrix-matching, internal standards are widely used in LA-ICP-MS for quantitative analyses. The internal standard compensates for the different ablation yields from the sample and the standard and for the laser shot-to-shot variation. Given that the use of an internal standard is required to obtain reliable results, the need for matrix-matching might be regarded as questionable. This project has focused on the development and application of a new method of calibration for LA-ICP-MS. It involves the use of aqueous standards whose absorption characteristics are modified by the addition of a chromophore to the solution. Additives were selected for ablation with KrF excimer, and Nd:YAG lasers. The influence of the additive concentration on the ablation yield was investigated for different laser energies. Response curves were obtained showing that as the additive concentration was increased, less energy was required to ablate the modified standard solutions efficiently. A general procedure was then defined for the preparation and use of the modified standard solutions for a given sample. The new method of calibration was used for the quantitative analysis of different sample types: low density polyethylene (LDPE), polyketone (PK

  18. Development and application of a calibration technique for laser ablation - ICP - MS

    International Nuclear Information System (INIS)

    Boue-Bigne, F.

    2000-01-01

    Laser Ablation - Inductively Coupled Plasma - Mass Spectrometry (LA-ICP-MS) is a powerful analytical technique for the direct elemental analysis of solid samples, with spatial resolution down to a few microns. However, calibration remains the limiting factor in obtaining quantitative analysis by LA-ICP-MS for a wide range of sample types. No universal method exists as yet and the ones that are currently used tend to employ matrix-matched solid standards. Matrix-matched solid standards are not available for many types of sample, such as polymers, biological materials, fluid inclusions, etc. The need for a universal method of calibration that involves standards that are easy to prepare and suitable for any type of sample is required. Additional to matrix-matching, internal standards are widely used in LA-ICP-MS for quantitative analyses. The internal standard compensates for the different ablation yields from the sample and the standard and for the laser shot-to-shot variation. Given that the use of an internal standard is required to obtain reliable results, the need for matrix-matching might be regarded as questionable. This project has focused on the development and application of a new method of calibration for LA-ICP-MS. It involves the use of aqueous standards whose absorption characteristics are modified by the addition of a chromophore to the solution. Additives were selected for ablation with KrF excimer, and Nd:YAG lasers. The influence of the additive concentration on the ablation yield was investigated for different laser energies. Response curves were obtained showing that as the additive concentration was increased, less energy was required to ablate the modified standard solutions efficiently. A general procedure was then defined for the preparation and use of the modified standard solutions for a given sample. The new method of calibration was used for the quantitative analysis of different sample types: low density polyethylene (LDPE), polyketone (PK

  19. The influence of laser pulse duration and energy on ICP-MS signal intensity, elemental fractionation, and particle size distribution in NIR fs-LA-ICP-MS

    Science.gov (United States)

    Diwakar, Prasoon K.; Harilal, Sivanandan S.; LaHaye, Nicole L.; Hassanein, Ahmed; Kulkarni, Pramod

    2015-01-01

    Laser parameters, typically wavelength, pulse width, irradiance, repetition rate, and pulse energy, are critical parameters which influence the laser ablation process and thereby influence the LA-ICP-MS signal. In recent times, femtosecond laser ablation has gained popularity owing to the reduction in fractionation related issues and improved analytical performance which can provide matrix-independent sampling. The advantage offered by fs-LA is due to shorter pulse duration of the laser as compared to the phonon relaxation time and heat diffusion time. Hence the thermal effects are minimized in fs-LA. Recently, fs-LA-ICP-MS demonstrated improved analytical performance as compared to ns-LA-ICP-MS, but detailed mechanisms and processes are still not clearly understood. Improvement of fs-LA-ICP-MS over ns-LA-ICP-MS elucidates the importance of laser pulse duration and related effects on the ablation process. In this study, we have investigated the influence of laser pulse width (40 fs to 0.3 ns) and energy on LA-ICP-MS signal intensity and repeatability using a brass sample. Experiments were performed in single spot ablation mode as well as rastering ablation mode to monitor the Cu/Zn ratio. The recorded ICP-MS signal was correlated with total particle counts generated during laser ablation as well as particle size distribution. Our results show the importance of pulse width effects in the fs regime that becomes more pronounced when moving from femtosecond to picosecond and nanosecond regimes. PMID:26664120

  20. Establishment of a method for determination of arsenic species in seafood by LC-ICP-MS.

    Science.gov (United States)

    Zmozinski, Ariane V; Llorente-Mirandes, Toni; López-Sánchez, José F; da Silva, Márcia M

    2015-04-15

    An analytical method for determination of arsenic species (inorganic arsenic (iAs), methylarsonic acid (MA), dimethylarsinic acid (DMA), arsenobetaine (AB), trimethylarsine oxide (TMAO) and arsenocholine (AC)) in Brazilian and Spanish seafood samples is reported. This study was focused on extraction and quantification of inorganic arsenic (iAs), the most toxic form. Arsenic speciation was carried out via LC with both anionic and cationic exchange with ICP-MS detection (LC-ICP-MS). The detection limits (LODs), quantification limits (LOQs), precision and accuracy for arsenic species were established. The proposed method was evaluated using eight reference materials (RMs). Arsenobetaine was the main species found in all samples. The total and iAs concentration in 22 seafood samples and RMs ranged between 0.27-35.2 and 0.02-0.71 mg As kg(-1), respectively. Recoveries ranging from 100% to 106% for iAs, based on spikes, were achieved. The proposed method provides reliable iAs data for future risk assessment analysis. Copyright © 2014 Elsevier Ltd. All rights reserved.

  1. The use of ICP-MS and LA-ICP-MS techniques for uranium analysis in real-life swipe samples for safeguards purposes

    International Nuclear Information System (INIS)

    Pestana, Rafael C.B.; Sarkis, Jorge E.S.; Carvalho, Elita F.U.; Abreu Junior, Cassio H.

    2013-01-01

    Environmental swipe sampling for safeguards purposes is a powerful tool to detect undeclared materials and activities, and has been used by the International Atomic Energy Agency since 1997. This work describes the utilization of the inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for determining uranium isotopic ratios in a real-life swipe samples collected in a conversion plant at IPEN/CNEN, Brazil. Uncertainties were estimated by following the International Organization for Standardization - Guide to the Expression of Uncertainties in Measurement (ISO GUM), with a confidence level of 95%. The major uncertainties percentage for n( 235 U)/n( 238 U) ratio for ICP-MS was 3% and for LA-ICP-MS was 30% The values of uranium isotopic ratios obtained for each technique demonstrate the viability of these analytical techniques as an alternative tool for uranium analysis in swipe samples for safeguards purposes. (author)

  2. Theoretical Investigation of Spectral-Interferences of Cadmium Isotopes in ICP-MS

    International Nuclear Information System (INIS)

    Rashad, A.M.; Rashad, A.M.

    2015-01-01

    Thermal properties of polyatomic ions which can interfere with cadmium during the analysis process using the inductively coupled plasma mass spectrometer ICP-MS are studied. Ionization energies and heats of formation, of the selected species at 0 K and 298 K of the expected reactions to occur under the effect of plasma conditions in ICP-MS, are calculated using Gaussian 03

  3. Salpeterzuurdestructie en ICP-MS analyse van biotisch materiaal en voeding

    NARCIS (Netherlands)

    Velde-Koerts T van der; LAC

    2000-01-01

    Voor de bepaling van elementen in voeding en biotisch materiaal werd een analytische methode ontwikkeld, bestaande uit een salpeterzuurdestructie en een ICP-MS-analyse. De destructie werd geoptimaliseerd op basis van de salpeterzuurconcentratie en de destructietijd. De ICP-MS-analyse werd

  4. Comparative study for toxic elements determination in air particulate reference material by INAA, CCT-ICP-MS, and ICP-MS

    International Nuclear Information System (INIS)

    Lim, J.M.; Lee, J.H.; Kim, K.H.; Moon, J.H.; Chung, Y.S.

    2005-01-01

    Although toxic elements are minor components in the atmospheric environment, they play a significant role as important marker for atmospheric science such as risk assessment, long-range transfer study, and source apportionment. Therefore, the techniques, which allow accurate and fast elemental analysis with a minimum pre-treatment, are very important. INAA has a main advantage of non-destruction of air particulate samples, while inductively Coupled plasma with mass spectrometry (ICP-MS) encounters the most significant difficulties in pre-treatment (digestion, fusion, and dilution) and polyatomic spectral interferences for interest toxic elements, Although INAA is still reference method, a number of factors (disadvantages of cost, complexity of the instruments, and scarcity of nuclear reactor) limit its applications. To date, the use of collision cell technology ICP-MS (CCT-ICP-MS) is recommended instead of typical ICP-MS for the analysis of the toxic elements; this is because CCT-ICP-MS technique prevents polyatomic spectral interferences despite of contamination and volatile effects. In this study, a number of toxic elements in reference material, NIST SRM 2783 (air particulate on filter media) were determined by INAA, CCT-ICP-MS, and ICP-MS. For both ICP methods, the filters were decomposed by microwave digestion with 5mL nitric acid. The analytical results by three methods were compared with certificated data; the INAA results showed the most accurate and precise data sets for all target elements among three methods. In detail, the deviation between analytical results and SRM's by INAA fell below 10% for all elements excluding As (14%), while those by CCT-ICP-MS were about 20%. For ICP-MS, the result does not agree with certificated data for several elements, because polyatomic spectral interference (due to 40 Ar 35 Cl, 40 Ar 23 Na, and 35 Cl 16 O) generate positive error of analytical result for As, Cu, and V. Based on our result, INAA is still one of the most

  5. Application of on-line HPLC-ICP-MS for the determination of the nuclide abundances of lanthanides produced via spallation reactions in an irradiated tantalum target of a spallation neutron source

    International Nuclear Information System (INIS)

    Kerl, W.; Becker, J.S.; Dietze, H.J.

    1998-01-01

    An analytical procedure has been developed for the determination of spallation nuclides in an irradiated tantalum target using HPLC coupled on-line to ICP-MS after dissolution and separation of the tantalum matrix. Pieces of tantalum were taken from different locations of the irradiated tantalum target which had been used as the target material in a spallation neutron source. Tantalum was dissolved in a HNO 3 /HF mixture and the tantalum matrix was separated by liquid-liquid extraction so that only the spallation nuclides were left in the sample solutions. The major fraction of the spallation nuclides in the tantalum target are lanthanide metals in the μg g -1 concentration range determined in the present study. Additional reaction products are formed by the irradiation of trace impurities in the original tantalum target. The nuclide abundances of the lanthanide metals measured in the tantalum target differ significantly from the natural isotopic composition so that a lot of isobaric interferences of long-lived radionuclides and stable isotopes in the mass spectrum are to be expected. Therefore, all the lanthanide metals had to be separated chemically prior to their mass spectrometric determination. The separation of all rare earth elements was performed by ion chromatography on-line to ICP-MS. The nuclide abundances of each lanthanide were determined using a sensitive double-focusing sector field inductively coupled plasma mass spectrometer. The nuclide abundances of the lanthanides in the irradiated tantalum target calculated theoretically and the experimental results obtained by on-line HPLC-ICP-MS proved to be in good agreement. (orig.)

  6. Multielemental analysis of Korean geological reference samples by INAA, ICP-AES and ICP-MS

    International Nuclear Information System (INIS)

    Naoki Shirai; Hiroki Takahashi; Yuta Yokozuka; Mitsuru Ebihara; Meiramkhan Toktaganov; Shun Sekimoto

    2015-01-01

    Six Korean geological reference samples (KB-1, KGB-1, KT-1, KD-1, KG-1 and KG-2) prepared by Korea Institutes of Geoscience and Mineral Resources were analyzed by using INAA, ICP-AES and ICP-MS. Some elements could be determined by both INAA and non-INAA methods (ICP-AES and ICP-MS), and these data are consistent with each other. This study confirms that a combination of ICP-AES and ICP-MS is comparable to INAA in determining a wide range of major, minor and trace elements in geological materials. (author)

  7. Metal ion transport quantified by ICP-MS in intact cells

    Science.gov (United States)

    Figueroa, Julio A. Landero; Stiner, Cory A.; Radzyukevich, Tatiana L.; Heiny, Judith A.

    2016-01-01

    The use of ICP-MS to measure metal ion content in biological tissues offers a highly sensitive means to study metal-dependent physiological processes. Here we describe the application of ICP-MS to measure membrane transport of Rb and K ions by the Na,K-ATPase in mouse skeletal muscles and human red blood cells. The ICP-MS method provides greater precision and statistical power than possible with conventional tracer flux methods. The method is widely applicable to studies of other metal ion transporters and metal-dependent processes in a range of cell types and conditions. PMID:26838181

  8. LA-ICP-MS Results: 3 Siple Dome A Glacial Age Archives, Version 1

    Data.gov (United States)

    National Aeronautics and Space Administration — This data set contains the results of Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) performed on an archive of the Siple Dome A ice core...

  9. ICP-MS: Analytical Method for Identification and Detection of Elemental Impurities.

    Science.gov (United States)

    Mittal, Mohini; Kumar, Kapil; Anghore, Durgadas; Rawal, Ravindra K

    2017-01-01

    Aim of this article is to review and discuss the currently used quantitative analytical method ICP-MS, which is used for quality control of pharmaceutical products. ICP-MS technique has several applications such as determination of single elements, multi element analysis in synthetic drugs, heavy metals in environmental water, trace element content of selected fertilizers and dairy manures. ICP-MS is also used for determination of toxic and essential elements in different varieties of food samples and metal pollutant present in the environment. The pharmaceuticals may generate impurities at various stages of development, transportation and storage which make them risky to be administered. Thus, it is essential that these impurities must be detected and quantified. ICP-MS plays an important function in the recognition and revealing of elemental impurities. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  10. Determination of Long-lived Radionuclides in the Environment using ICP-MS and AMS

    DEFF Research Database (Denmark)

    Hou, Xiaolin

    2011-01-01

    ICP-MS and AMS have been widely used for the measurement of radionuclides, especially long-lived radionculides. The new progress, major advantages of these two techniques and their major applications for measurement of important radionculides are summarized.......ICP-MS and AMS have been widely used for the measurement of radionuclides, especially long-lived radionculides. The new progress, major advantages of these two techniques and their major applications for measurement of important radionculides are summarized....

  11. Determination of Pu and U by ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Muramatsu, Y.; Yoshida, S. [National Inst. of Radiological Sciences, Chiba (Japan)

    2002-06-01

    In order to understand the distribution and behaviour of long-lived radionuclides in the terrestrial environment, we have developed analytical methods for {sup 238}U, {sup 232}Th and {sup 239},{sup 240}Pu and determined them in several environmental samples. ICP-MS was applied to the analyses. Concentrations of {sup 238}U and {sup 232}Th were determined in variety of soils, plants and environmental waters. The mean concentration of U and Th in 77 soils, collected several parts of Japan, were 2.3 and 7.0 ppm (dry wt). Red and yellow soils, which are mainly found in western Japan, have high concentrations of Th, suggesting the contribution from granitic rocks. Higher concentration of U in agricultural soils than forest soils suggested the possible accumulation of this element from phosphate fertilizer. The soil-to-plant transfer factors (concentration ratios between plants and soils) of U and Th were estimated from the analytical results of these nuclides in soils and in several crops. The factors for U were about 0.0005 in leaf vegetables, 0.0002 in root vegetables, 0.0001 in potatoes and 0.00001 in rice (polished). For Th, the factors were about 0.0005 in leaf vegetables, 0.0008 in root vegetables, 0.0005 in potatoes and 0.00003 in rice (polished). For the analysis of plutonium, chromatographic resin, Dowex 1x8, was examined for their applicability in the separation of Pu from the matrix elements. Sufficient decontamination factors (10{sup 4}-10{sup 5}) for many matrix elements including U, which interferes in the detection of mass 239, were obtained in both resins. Analytical results of {sup 239+240}Pu in standard reference materials (IAEA-135, -SOIL-6, -368 and -134) indicated that the accuracy of this method was satisfactory. Data on the {sup 240}Pu/{sup 239}Pu atom ratios in these reference materials, which are rare in the literature, were also obtained. Soil samples from the Marshall Islands showed a large variation of the {sup 240}Pu/{sup 239}Pu atom ratios

  12. Obsidian provenance studies in archaeology: A comparison between PIXE, ICP-AES and ICP-MS

    International Nuclear Information System (INIS)

    Bellot-Gurlet, Ludovic; Poupeau, Gerard; Salomon, Joseph; Calligaro, Thomas; Moignard, Brice; Dran, Jean-Claude; Barrat, Jean-Alix; Pichon, Laurent

    2005-01-01

    Elemental composition fingerprinting by PIXE technique is very attractive for obsidian provenance studies as it may proceed in a non-destructive mode, even if a more complete elemental characterization can be obtained by ICP-MS and/or ICP-AES. Only few studies have compared results obtained by both methods for solid rock samples. In this work, elemental compositions were determined by ICP-MS/-AES for international geochemical standards and by ICP-MS/-AES and PIXE for inter-laboratory reference obsidians. In addition 49 obsidian source samples and artefacts were analysed by both ICP-MS/-AES and PIXE. Instrumental work and measurement quality control performed for obsidian chemical characterization, underline that PIXE and ICP-MS/-AES provide reproducible, accurate and comparable measurements. In some volcanic districts the limited number of elements dosed by PIXE is sufficient for the discrimination of the potential raw sources of obsidians. Therefore, PIXE can be an advantageous substitute to ICP-MS/-AES techniques for provenance studies

  13. Micro-extraction procedures for the determination of Ra-226 in well waters by SF-ICP-MS

    International Nuclear Information System (INIS)

    Lariviere, D.; Epov, V.N.; Reiber, K.M.; Cornett, R.J.; Evans, R.D.

    2005-01-01

    The radium-226 (t 1/2 = 1622 years) content of highly alkaline well water collected from the United Arab Emirates (UAE) was measured by double focusing sector-field inductively coupled plasma-mass spectrometry (SF-ICP-MS) after separation of the radium from other alkaline earth elements using a newly developed procedure. The results were comparable with those obtained by α-spectrometry for samples with concentrations ranging from 6.75 to 459 pg/L (0.25 to 17 Bq/L). Instrumental sensitivity on matrix-free samples was compared for two sample introduction systems, i.e. an Apex-Q high sensitivity system and a concentric nebulizer. A 12-fold improvement in sensitivity (instrumental detection limit = 1.5 pg/L or 55 mBq/L) was found when the Apex-Q system was used. Two chromatographic methods were tested for the sequential separation of the alkaline earth elements contained in the well water samples in order to reduce matrix and polyatomic interference effects. Optimal elution parameters were determined and used for the separation and pre-concentration of Ra-226 in those samples. A method detection limit of 0.189 pg/L (7 mBq/L), which corresponds to a mass of 0.38 fg of Ra-226 in the sample, was achieved. Only 2 mL of sample is necessary when a combination of 50 W-X8 and Sr*Spec resin, which are reusable, are utilized for the separation. This new analytical protocol significantly reduces sample preparation time resulting in a throughput rate of approximately 20 samples in only 8 h; faster than the other published extraction procedures

  14. Highlights of analytical chemistry in Switzerland. Spatially resolved plant physiological analysis using LA-HR-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Ulrich, A. [Swiss Federal Laboratories for Material Testing and Research (EMPA), Duebendorf (Switzerland); Barrelet, T. [Federal Office of Public Health (FOPH), Berne (Switzerland); Kraehenbuehl, U. [University of Berne, Department for Chemistry and Biochemistry, Berne (Switzerland)

    2007-06-15

    Investigations of elemental distribution in trees are interesting in plant physiological and environmental research. Seasonal element variations within single tree rings would provide important information on metabolism studies but they have not been accessible so far. Thus, a direct micro-analytical method involving laser ablation (LA) coupled to high-resolution double-focusing magnetic sector field inductively coupled plasma mass spectrometry (HR-ICP-MS) was developed. Particularly challenging aspects in method development were the high background levels of certain elements and the lack of appropriate calibration standards. Seasonal element profiles of macronutrients in Norway spruce trees from different sampling sites, altitudes and environmental conditions could be established for the first time. The method allows the measurement of low concentrations even in narrow year rings. Depending on the tree ring width, the number of laser spots per ring varied between four and eight. For discussion purposes, each ring was divided in four distinct zones commonly used in dendrology: early earlywood (EEW), late earlywood (LEW), early latewood (ELW) and late latewood (LLW). The sulphur profile displayed seasonal variations with decreasing contents in LEW and ELW, which leads to the assumption that stem sulphur is used for seasonal growth. When accrescence stops in autumn, sulphur reserves are stored in preparation for next year's growth, since methionine in tree sap was found to increase in March until July and decrease in August. A seasonal pattern was also found for phosphorus. This contradicts the hypothesis of a constant supply by mycorrhizal fungi and implies that reserves are stored towards the end of growing season for use the following spring. The linear relationship between phosphorus and sulphur underlines a strong biochemical coupling of both elements. Other macronutrients like potassium show different profiles. Potassium is of particular importance in

  15. Highlights of analytical chemistry in Switzerland. Spatially resolved plant physiological analysis using LA-HR-ICP-MS

    International Nuclear Information System (INIS)

    Ulrich, A.; Barrelet, T.; Kraehenbuehl, U.

    2007-01-01

    Investigations of elemental distribution in trees are interesting in plant physiological and environmental research. Seasonal element variations within single tree rings would provide important information on metabolism studies but they have not been accessible so far. Thus, a direct micro-analytical method involving laser ablation (LA) coupled to high-resolution double-focusing magnetic sector field inductively coupled plasma mass spectrometry (HR-ICP-MS) was developed. Particularly challenging aspects in method development were the high background levels of certain elements and the lack of appropriate calibration standards. Seasonal element profiles of macronutrients in Norway spruce trees from different sampling sites, altitudes and environmental conditions could be established for the first time. The method allows the measurement of low concentrations even in narrow year rings. Depending on the tree ring width, the number of laser spots per ring varied between four and eight. For discussion purposes, each ring was divided in four distinct zones commonly used in dendrology: early earlywood (EEW), late earlywood (LEW), early latewood (ELW) and late latewood (LLW). The sulphur profile displayed seasonal variations with decreasing contents in LEW and ELW, which leads to the assumption that stem sulphur is used for seasonal growth. When accrescence stops in autumn, sulphur reserves are stored in preparation for next year's growth, since methionine in tree sap was found to increase in March until July and decrease in August. A seasonal pattern was also found for phosphorus. This contradicts the hypothesis of a constant supply by mycorrhizal fungi and implies that reserves are stored towards the end of growing season for use the following spring. The linear relationship between phosphorus and sulphur underlines a strong biochemical coupling of both elements. Other macronutrients like potassium show different profiles. Potassium is of particular importance in needles

  16. Application of ICP-MS and HPLC-ICP-MS for diagnosis and therapy of a severe intoxication with hexavalent chromium and inorganic arsenic.

    Science.gov (United States)

    Heitland, Peter; Blohm, Martin; Breuer, Christian; Brinkert, Florian; Achilles, Eike Gert; Pukite, Ieva; Köster, Helmut Dietrich

    2017-05-01

    ICP-MS and HPLC-ICP-MS were applied for diagnosis and therapeutic monitoring in a severe intoxication with a liquid containing hexavalent chromium (Cr(VI)) and inorganic arsenic (iAs). In this rare case a liver transplantation of was considered as the only chance of survival. We developed and applied methods for the determination of Cr(VI) in erythrocytes and total chromium (Cr) and arsenic (As) in blood, plasma, urine and liver tissue by ICP-MS. Exposure to iAs was diagnosed by determination of iAs species and their metabolites in urine by anion exchange HPLC-ICP-MS. Three days after ingestion of the liquid the total Cr concentrations were 2180 and 1070μg/L in whole blood and plasma, respectively, and 4540μg/L Cr(VI) in erythrocytes. The arsenic concentration in blood was 206μg/L. The urinary As species concentrations were <0.5, 109, 115, 154 and 126μg/L for arsenobetaine, As(III), As(V), methylarsonate (V) and dimethylarsinate (V), respectively. Total Cr and As concentrations in the explanted liver were 11.7 and 0.9mg/kg, respectively. Further analytical results of this case study are tabulated and provide valuable data for physicians and toxicologists. Copyright © 2017. Published by Elsevier GmbH.

  17. The use of ICP-MS and LA-ICP-MS techniques for uranium analysis in real-life swipe samples for safeguards purposes

    Energy Technology Data Exchange (ETDEWEB)

    Pestana, Rafael C.B.; Sarkis, Jorge E.S.; Carvalho, Elita F.U., E-mail: rcbpestana@gmail.com, E-mail: jesarkis@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Abreu Junior, Cassio H. [Centro de Energia Nuclear na Agricultura (CENA/USP), Piracicaba, SP (Brazil)

    2013-07-01

    Environmental swipe sampling for safeguards purposes is a powerful tool to detect undeclared materials and activities, and has been used by the International Atomic Energy Agency since 1997. This work describes the utilization of the inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for determining uranium isotopic ratios in a real-life swipe samples collected in a conversion plant at IPEN/CNEN, Brazil. Uncertainties were estimated by following the International Organization for Standardization - Guide to the Expression of Uncertainties in Measurement (ISO GUM), with a confidence level of 95%. The major uncertainties percentage for n({sup 235}U)/n({sup 238}U) ratio for ICP-MS was 3% and for LA-ICP-MS was 30% The values of uranium isotopic ratios obtained for each technique demonstrate the viability of these analytical techniques as an alternative tool for uranium analysis in swipe samples for safeguards purposes. (author)

  18. Calibration and correction of LA-ICP-MS and LA-MC-ICP-MS analyses for element contents and isotopic ratios

    Directory of Open Access Journals (Sweden)

    Jie Lin

    2016-06-01

    Full Text Available LA-ICP-MS and LA-MC-ICP-MS have been the techniques of choice for achieving accurate and precise element content and isotopic ratio, the state-of-the-art technique combines the advantages of low detection limits with high spatial resolution, however, the analysis accuracy and precision are restricted by many factors, such as sensitivity drift, elemental/isotopic fractionation, matrix effects, interferences and the lack of sufficiently matrix-matched reference materials. Thus, rigorous and suitable calibration and correction methods are needed to obtain quantitative data. This review systematically summarized and evaluated the interference correction, quantitative calculation and sensitivity correction strategies in order to provide the analysts with suitable calibration and correction strategies according to the sample types and the analyzed elements. The functions and features of data reduction software ICPMSDataCal were also outlined, which can provide real-time and on-line data reduction of element content and isotopic ratios analyzed by LA-ICP-MS and LA-MC-ICP-MS.

  19. Determination of (187)Os in molybdenite by ICP-MS with neutron-induced (186)Os and (188)Os spikes.

    Science.gov (United States)

    Qu, W; Du, A; Zhao, D

    2001-10-31

    The article describes a method for the determination of (187)Os in molybdenite by isotope dilution inductively coupled plasma-mass spectrometry (ID-ICP-MS) with neutron-induced (186)Os and (188)Os spike. The spike used in the present work was prepared in line with the principle by which artificial nuclides are produced in a nuclear reaction. The concentration and isotopic composition of osmium in the prepared spike were evaluated accurately with the isotope dilution method, using negative thermal ion mass spectrometry (N-TIMS). The advantage of this method is that using (186)Os and (188)Os double spikes can effectively compensate for the mass discrimination effects of ICP-MS. Thus, the common correction practice for mass bias in the isotope dilution method with a single spike is unnecessary. In addition, the method enables one to reduce the determined error arising from instrumental instability. The precision for the (187)Os/((186)Os+(188)Os) ratio was approximately 2% (2sigma, RSD), but in the case of (187)Os/(186)Os, (187)Os/(188)Os and (186)Os/(188)Os, precision ranged from 2.0 to 8% (2sigma, RSD). The results for (187)Os concentration in a molybdenite sample determined with this method showed good agreement with reference values.

  20. The influence of room temperature on Mg isotope measurements by MC-ICP-MS.

    Science.gov (United States)

    Zhang, Xing-Chao; Zhang, An-Yu; Zhang, Zhao-Feng; Huang, Fang; Yu, Hui-Min

    2018-03-24

    We observed that the accuracy and precision of magnesium (Mg) isotope analyses could be affected if the room temperature oscillated during measurements. To achieve high quality Mg isotopic data, it is critical to evaluate how the unstable room temperature affects Mg isotope measurements by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). We measured the Mg isotopes for the reference material DSM-3 using MC-ICP-MS under oscillating room temperatures in spring. For a comparison, we also measured the Mg isotopes under stable room temperatures, which was achieved by the installation of an improved temperature control system in the laboratory. The δ 26 Mg values measured under oscillating room temperatures have a larger deviation (δ 26 Mg from -0.09 to 0.08‰, with average δ 26 Mg = 0.00 ± 0.08 ‰) than those measured under a stable room temperature (δ 26 Mg from -0.03 to 0.03‰, with average δ 26 Mg = 0.00 ± 0.02 ‰) using the same MC-ICP-MS system. The room temperature variation can influence the stability of MC-ICP-MS. Therefore, it is critical to keep the room temperature stable to acquire high precise and accurate isotopic data when using MC-ICP-MS, especially when using the sample-standard bracketing (SSB) correction method. This article is protected by copyright. All rights reserved.

  1. Current role of ICP-MS in clinical toxicology and forensic toxicology: a metallic profile.

    Science.gov (United States)

    Goullé, Jean-Pierre; Saussereau, Elodie; Mahieu, Loïc; Guerbet, Michel

    2014-08-01

    As metal/metalloid exposure is inevitable owing to its omnipresence, it may exert toxicity in humans. Recent advances in metal/metalloid analysis have been made moving from flame atomic absorption spectrometry and electrothermal atomic absorption spectrometry to the multi-elemental inductively coupled plasma (ICP) techniques as ICP atomic emission spectrometry and ICP-MS. ICP-MS has now emerged as a major technique in inorganic analytical chemistry owing to its flexibility, high sensitivity and good reproducibility. This in depth review explores the ICP-MS metallic profile in human toxicology. It is now routinely used and of great importance, in clinical toxicology and forensic toxicology to explore biological matrices, specifically whole blood, plasma, urine, hair, nail, biopsy samples and tissues.

  2. [Progress in the application of laser ablation ICP-MS to surface microanalysis in material science].

    Science.gov (United States)

    Zhang, Yong; Jia, Yun-hai; Chen, Ji-wen; Shen, Xue-jing; Liu, Ying; Zhao, Leiz; Li, Dong-ling; Hang, Peng-cheng; Zhao, Zhen; Fan, Wan-lun; Wang, Hai-zhou

    2014-08-01

    In the present paper, apparatus and theory of surface analysis is introduced, and the progress in the application of laser ablation ICP-MS to microanalysis in ferrous, nonferrous and semiconductor field is reviewed in detail. Compared with traditional surface analytical tools, such as SEM/EDS (scanning electron microscopy/energy dispersive spectrum), EPMA (electron probe microanalysis analysis), AES (auger energy spectrum), etc. the advantage is little or no sample preparation, adjustable spatial resolution according to analytical demand, multi-element analysis and high sensitivity. It is now a powerful complementary method to traditional surface analytical tool. With the development of LA-ICP-MS technology maturing, more and more analytical workers will use this powerful tool in the future, and LA-ICP-MS will be a super star in elemental analysis field just like LIBS (Laser-induced breakdown spectroscopy).

  3. Plutonium bioassay by inductively coupled plasma mass spectrometry ICP/MS

    International Nuclear Information System (INIS)

    Wyse, E.J.; Fisher, D.R.

    1993-04-01

    The determination of plutonium in urine poses several analytical challenges, e.g., detectability, matrix, etc. We have investigated the feasibility of analyzing plutonium in processed urine by inductively coupled plasma mass spectrometry (ICP/MS). The urine samples are first spiked with 244 Pu as a tracer and internal standard, then processed by co-precipitation and column chromatography using TRU-Spec trademark, an extraction resin. By enhancing ICP/MS detection capabilities via improved sample introduction and data acquisition efficiencies, an instrumental detection limit of 5 to 50 fg (0.3 to 3 fCi for 239 pu) is typically obtained, depending on the desired degree of quantitation. A brief summary of the analytical method as well as the basis for measuring radionuclides by ICP/MS are submitted; the separation procedure, methods of sample introduction, and data acquisition techniques are then highlighted

  4. A New Multielement Method for LA-ICP-MS Data Acquisition from Glacier Ice Cores.

    Science.gov (United States)

    Spaulding, Nicole E; Sneed, Sharon B; Handley, Michael J; Bohleber, Pascal; Kurbatov, Andrei V; Pearce, Nicholas J; Erhardt, Tobias; Mayewski, Paul A

    2017-11-21

    To answer pressing new research questions about the rate and timing of abrupt climate transitions, a robust system for ultrahigh-resolution sampling of glacier ice is needed. Here, we present a multielement method of LA-ICP-MS analysis wherein an array of chemical elements is simultaneously measured from the same ablation area. Although multielement techniques are commonplace for high-concentration materials, prior to the development of this method, all LA-ICP-MS analyses of glacier ice involved a single element per ablation pass or spot. This new method, developed using the LA-ICP-MS system at the W. M. Keck Laser Ice Facility at the University of Maine Climate Change Institute, has already been used to shed light on our flawed understanding of natural levels of Pb in Earth's atmosphere.

  5. Multi-elemental analysis of aqueous geochemical samples by quadrupole inductively coupled plasma-mass spectrometry (ICP-MS)

    Science.gov (United States)

    Wolf, Ruth E.; Adams, Monique

    2015-01-01

    Typically, quadrupole inductively coupled plasma-mass spectrometry (ICP-MS) is used to determine as many as 57 major, minor, and trace elements in aqueous geochemical samples, including natural surface water and groundwater, acid mine drainage water, and extracts or leachates from geological samples. The sample solution is aspirated into the inductively coupled plasma (ICP) which is an electrodeless discharge of ionized argon gas at a temperature of approximately 6,000 degrees Celsius. The elements in the sample solution are subsequently volatilized, atomized, and ionized by the ICP. The ions generated are then focused and introduced into a quadrupole mass filter which only allows one mass to reach the detector at a given moment in time. As the settings of the mass analyzer change, subsequent masses are allowed to impact the detector. Although the typical quadrupole ICP-MS system is a sequential scanning instrument (determining each mass separately), the scan speed of modern instruments is on the order of several thousand masses per second. Consequently, typical total sample analysis times of 2–3 minutes are readily achievable for up to 57 elements.

  6. Environmental radioactivity research on the Fukushima Dai-ichi Nuclear Power Plant accident by ICP-MS

    International Nuclear Information System (INIS)

    Ohno, Takeshi; Muramatsu, Yasuyuki

    2015-01-01

    Inductively coupled plasma (ICP) is characterized by high ionization efficiency for almost all elements. Recently, a triple quadrupole ICP-MS (ICP-MS/MS) has been applied to the measurements of isotope ratios for ultra-low level radioisotopes. The ICP-MS/MS features an additional quadrupole mass filter situated in front of the octopole reaction cell and quadrupole mass filter, which allows only the analyte ion to enter the cell by rejecting all the other ions. In this manuscript, we review recent studies on environmental radioactivity in Fukushima achieved by ICP-MS/MS techniques. (author)

  7. {sup 99}Tc bioassay by inductively coupled plasma mass spectrometry (ICP-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Lewis, L.A.

    1998-05-01

    A means of analyzing {sup 99}Tc in urine by inductively coupled plasma mass spectrometry (ICP-MS) has been developed. Historically, {sup 99}Tc analysis was based on the radiometric detection of the 293 keV E{sub Max} beta decay product by liquid scintillation or gas flow proportional counting. In a urine matrix, the analysis of{sup 99}Tc is plagued with many difficulties using conventional radiometric methods. Difficulties originate during chemical separation due to the volatile nature of Tc{sub 2}O{sub 7} or during radiation detection due to color or chemical quenching. A separation scheme for {sup 99}Tc detection by ICP-MS is given and is proven to be a sensitive and robust analytical alternative. A comparison of methods using radiometric and mass quantitation of {sup 99}Tc has been conducted in water, artificial urine, and real urine matrices at activity levels between 700 and 2,200 dpm/L. Liquid scintillation results based on an external standard quench correction and a quench curve correction method are compared to results obtained by ICP-MS. Each method produced accurate results, however the precision of the ICP-MS results is superior to that of liquid scintillation results. Limits of detection (LOD) for ICP-MS and liquid scintillation detection are 14.67 and 203.4 dpm/L, respectively, in a real urine matrix. In order to determine the basis for the increased precision of the ICP-MS results, the detection sensitivity for each method is derived and measured. The detection sensitivity for the {sup 99}Tc isotope by ICP-MS is 2.175 x 10{sup {minus}7} {+-} 8.990 x 10{sup {minus}9} and by liquid scintillation is 7.434 x 10{sup {minus}14} {+-} 7.461 x 10{sup {minus}15}. A difference by seven orders of magnitude between the two detection systems allows ICP-MS samples to be analyzed for a period of 15 s compared to 3,600 s by liquid scintillation counting with a lower LOD.

  8. Determination of iron in highly-saline matrices by FIA-ICP-MS

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    Analysis of iron by inductively-coupled-plasma mass-spectrometry (ICP-MS) may be significantly improved by applying a protocol of flow-injection analysis. The iron species of the sample was preconcentrated by an ammonia buffer at pH = 9.2 on a filterless nylon-knotted reactor, and the adsorbed...... species were subsequently eluted by hydrochloric acid and analysed by ICP-MS. During the FIA step of preconcentration, a high degree of salinity did not influence the adsorption mechanism of iron, which may be related to formation of iron-hydroxide complexes at the sites of amide moieties of the nylon...

  9. Development of analytical procedures for determination of total chromium by quadrupole ICP-MS and high-resolution ICP-MS, and hexavalent chromium by HPLC-ICP-MS, in different materials used in the automotive industry.

    Science.gov (United States)

    Séby, F; Gagean, M; Garraud, H; Castetbon, A; Donard, O F X

    2003-10-01

    A European directive was recently adopted limiting the use of hazardous substances such as Pb, Hg, Cd, and Cr(VI) in vehicle manufacturing. From July 2003 a maximum of 2 g Cr(VI) will be authorised per vehicle in corrosion-preventing coatings of key components. As no standardised procedures are available to check if produced vehicles are in agreement with this directive, the objective of this work was to develop analytical procedures for total chromium and Cr(VI) determination in these materials. The first step of this study was to optimise digestion procedures for total chromium determination in plastic and metallic materials by inductively coupled plasma mass spectrometry (ICP-MS). High resolution (HR) ICP-MS was used to examine the influence of polyatomic interferences on the detection of the (52)Cr(+) and (53)Cr(+) isotopes. If there was strong interference with m/ z 52 for plastic materials, it was possible to use quadrupole ICP-MS for m/ z 53 if digestions were performed with HNO(3)+H(2)O(2). This mixture was also necessary for digestion of chromium from metallic materials. Extraction procedures in alkaline medium (NH(4)(+)/NH(3) buffer solution at pH 8.9) assisted by sonication were developed for determining Cr(VI) in four different corrosion-preventing coatings by HPLC-ICP-MS. After optimisation and validation with the only solid reference material certified for its Cr(VI) content (BCR 545; welding dusts), the efficiency of this extraction procedure for screw coatings was compared with that described in the EN ISO 3613 standard generally used in routine laboratories. For coatings comprising zinc and aluminium passivated in depth with chromium oxides the extraction procedure developed herein enabled determination of higher Cr(VI) concentrations. This was also observed for the screw covered with a chromium passivant layer on zinc-nickel. For coating comprising a chromium passivant layer on alkaline zinc the standardized extraction procedure was more efficient

  10. Multielemental speciation analysis by advanced hyphenated technique - HPLC/ICP-MS: A review.

    Science.gov (United States)

    Marcinkowska, Monika; Barałkiewicz, Danuta

    2016-12-01

    Speciation analysis has become an invaluable tool in human health risk assessment, environmental monitoring or food quality control. Another step is to develop reliable multielemental speciation methodologies, to reduce costs, waste and time needed for the analysis. Separation and detection of species of several elements in a single analytical run can be accomplished by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry (HPLC/ICP-MS). Our review assembles articles concerning multielemental speciation determination of: As, Se, Cr, Sb, I, Br, Pb, Hg, V, Mo, Te, Tl, Cd and W in environmental, biological, food and clinical samples analyzed with HPLC/ICP-MS. It addresses the procedures in terms of following issues: sample collection and pretreatment, selection of optimal conditions for elements species separation by HPLC and determination using ICP-MS as well as metrological approach. The presented work is the first review article concerning multielemental speciation analysis by advanced hyphenated technique HPLC/ICP-MS. Copyright © 2016 Elsevier B.V. All rights reserved.

  11. Determination of heavy metals in groundwater samples - ICP-MS analysis and evaluation

    International Nuclear Information System (INIS)

    Leiterer, M.; Muench, U.

    1994-01-01

    An analytical programme which permits the direct, simultaneous determination of Al, As, Cd, Cr, Cu, Mn, Ni, Pb and Zn in groundwater samples was developed for ICP-MS. Spectral mass interferences, attributable to great differences in groundwater matrices, precision and accuracy have been discussed. The evaluation of analytical results was demonstrated for selected sampling points of the groundwater observation network of Thuringia. (orig.)

  12. Ir and Rare Earth's Elements determination by Neutron Activation Analysis and ICP - MS in soil samples

    Science.gov (United States)

    Salvini, A.; Cattadori, C.; Broggini, C.; Cagnazzo, M.; Ori, Gian Gabriele; Nisi, S.; Borio, A.; Manera, S.

    2006-05-01

    The platinum metals depleted in the earth's crust are relative to their cosmic abundance; concentration of these elements in sediments may thus indicate influxes of extraterrestrial material. Analysis of these parameters are done easily by Neutron Activation Analysis (NAA) and comparative results with ICP-MS technique show a good match. Results, adjust parameters and limits of this method will be displayed in tables.

  13. Analysis of trace uranium and plutonium in environmental water sample by ICP-MS

    International Nuclear Information System (INIS)

    Liu Xuemei

    2004-12-01

    The analysis of trace Uranium and Plutonium in environmental water is very important in the environment inspect. The preparation method of water samples are introduced and several common used method are compared. The analysis process and the calibration method with ICP-MS are discussed in detail considering present conditions. (author)

  14. Application of ICP-MS to a trace elements mass balance study in a power plant

    NARCIS (Netherlands)

    Bettinelli, M.; Spezia, S.; Fiore, A.; Pastorelli, N.; Terni, C.; Holland, G.; Tanner, S.D.

    2001-01-01

    The distributions of seven trace elements in a power plant are detd. in 3 fuels (Orimulsion, coal, and fuel oil) and output flows, i.e., ash, wastewater, gypsum, and emulsions by using ICP-MS. The power plant is equipped with sulfur oxide and nitrogen oxide removal facilities. [on SciFinder (R)

  15. Determination of Trace Elements in Uranium by HPLC-ID-ICP-MS: NTNFC Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Manard, Benjamin Thomas [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Wylie, Ernest Miller II [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Xu, Ning [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Tandon, Lav [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-10-19

    This report covers the FY 16 effort for the HPLC-ID-ICP-MS methodology 1) sub-method validation for the group I&II elements, 2) sub-method stood-up and validation for REE, 3) sub-method development for the transition element, and 4) completion of a comprehensive SOP for three families of elements.

  16. Operationalisering van de flow-injectietechniek in combinatie met ICP-MS

    NARCIS (Netherlands)

    Velde-Koerts T van der; Boer JLM de; LAC

    1994-01-01

    In dit onderzoek werd de flow-injectietechniek gecombineerd met ICP-MS. Hoewel de onderste analysegrenzen iets hoger waren dan bij continue verstuiving, heeft de flow-injectietechniek een aantal belangrijke voordelen: ten eerste het kleine monstervolume dat nodig is voor de analyse (0,7 ml,

  17. Sulfur-induced offsets in MC-ICP-MS silicon-isotope measurements

    NARCIS (Netherlands)

    van den Boorn, S.; Vroon, P.Z.; van Bergen, M.J.

    2009-01-01

    Sample preparation methods for MC-ICP-MS silicon-isotope measurements often involve a cation-exchange purification step. A previous study has argued that this would suffice for geological materials, as the occasional enrichment of anionic species would not compromise silicon-isotope analysis. Here

  18. Application of ICP-MS in Environmental Sampling Analysis for Safeguards

    International Nuclear Information System (INIS)

    Eko Pudjadi; Petrus Zacharias; Budi Prayitno

    2004-01-01

    Environmental samples measured by ICP-MS were analyzed for safeguards. There are two isotopes in environmental sampling that is used to find out the origin of nuclear materials and verify undeclared nuclear activities. Uranium isotopes are 234 U, 235 U, 236 U and 238 U and Plutonium isotopes are 239 Pu, 240 Pu, 241 Pu and 242 Pu. Uranium isotopes are used to verify an existing of nuclear power plants, enrichment plants or reprocessing plants. Plutonium isotopes are used to clarify global fallout from nuclear weapon testing and accident of nuclear facility or military purposes. The high sensitivity of ICP-MS can detect the isotopic fingerprint and trace elements in ppb concentration; ICP-MS has been applied to measure 235 U isotopic ratio and 240 Pu/ 239 Pu isotopic ratios. The sensitivity of ICP-MS is high precision and low operational cost in environmental sampling and can be considered in nuclear power design based on safeguards for development countries. (author)

  19. Sulphur-induced offsets in MC-ICP-MS silicon-isotope measurements

    NARCIS (Netherlands)

    van den Boorn, S.; Vroon, P.Z.; van Bergen, M.J.

    2010-01-01

    Sample preparation methods for MC-ICP-MS silicon-isotope measurements often involve a cation-exchange purification step. A previous study has argued that this would suffice for geological materials, as the occasional enrichment of anionic species would not compromise silicon-isotope analysis. Here

  20. Online immunocapture ICP-MS for the determination of the metalloprotein ceruloplasmin in human serum.

    Science.gov (United States)

    Bernevic, Bogdan; El-Khatib, Ahmed H; Jakubowski, Norbert; Weller, Michael G

    2018-04-02

    The human copper-protein ceruloplasmin (Cp) is the major copper-containing protein in the human body. The accurate determination of Cp is mandatory for the reliable diagnosis of several diseases. However, the analysis of Cp has proven to be difficult. The aim of our work was a proof of concept for the determination of a metalloprotein-based on online immunocapture ICP-MS. The immuno-affinity step is responsible for the enrichment and isolation of the analyte from serum, whereas the compound-independent quantitation with ICP-MS delivers the sensitivity, precision, and large dynamic range. Off-line ELISA (enzyme-linked immunosorbent assay) was used in parallel to confirm the elution profile of the analyte with a structure-selective method. The total protein elution was observed with the 32 S mass trace. The ICP-MS signals were normalized on a 59 Co signal. The human copper-protein Cp could be selectively determined. This was shown with pure Cp and with a sample of human serum. The good correlation with off-line ELISA shows that Cp could be captured and eluted selectively from the anti-Cp affinity column and subsequently determined by the copper signal of ICP-MS.

  1. Elemental mapping of structural materials for a nuclear reactor by means of LA-ICP-MS

    Czech Academy of Sciences Publication Activity Database

    Vaculovič, T.; Warchilová, T.; Šimo, T.; Matal, O.; Otruba, V.; Mikuška, Pavel; Kanický, V.

    2012-01-01

    Roč. 27, č. 8 (2012), s. 1321-1326 ISSN 0267-9477 Institutional research plan: CEZ:AV0Z40310501 Keywords : LA- ICP -MS * ICP -OES * LiF–NaF salts Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.155, year: 2012

  2. Prestatiekenmerken van een TotalQuant-elementanalyse met ICP-MS

    NARCIS (Netherlands)

    Velde-Koerts T van der; LAC

    1998-01-01

    TotalQuant-analyse met ICP-MS is een geschikte methode om snel oplossingen van diverse materialen te scannen op alle elementen van het periodieke systeem, behalve H, N, O, F, edelgassen en kortlevende (radio-actieve) elementen. Bij een TotalQuant-analyse wordt gebruik gemaakt van een standaard

  3. Analysis of I-Br-Cl in single fluid inclusions by LA-ICP-MS

    Science.gov (United States)

    Giehl, C.; Fusswinkel, T.; Beermann, O.; Garbe-Schönberg, D.; Scholten, L.; Wagner, T.

    2017-12-01

    Halogens are excellent tracers of hydrothermal fluid sources and in-situ LA-ICP-MS analysis of Cl and Br in single fluid inclusions has provided fundamentally new insight into hydrothermal fluid flow and ore formation. There is mounting evidence that enrichment and depletion of Br relative to Cl may be caused by a number of processes beyond seawater evaporation and halite dissolution which cannot be discriminated on the basis of Br/Cl ratios alone. Expanding the analytical capabilities of fluid inclusion LA-ICP-MS analysis to include iodine would allow to discern between selective and coupled enrichment processes of Cl, Br and I, even in geologically complex samples that are inaccessible to bulk extraction techniques. We present iodine concentration data determined by LA-ICP-MS analysis of synthetic fluid inclusions, using the Sca17 scapolite reference material for external standardization (Seo et al., 2011). Iodine concentrations in Sca17 were determined using the Durango apatite standard. Four starting solutions containing I (0.3, 1.5, 27, 78 µg/g), Br (941, 1403, 2868, 4275 µg/g), Na (30.7, 94.7 mg/g), and Cl (50, 137 mg/g) (analyzed by ICP-OES and ICP-MS at CAU Kiel) were prepared by dissolving reagent grade chemical powders in ultra-pure water. Spherical inclusions (up to 40 µm) were synthesized from the starting solutions in pre-cracked, HF-treated synthetic quartz crystals which were placed in gold capsules and equilibrated at 600°C, 100/200 MPa in cold seal pressure vessels. Fluid inclusion LA-ICP-MS analysis (University of Helsinki) yielded average I concentrations in excellent agreement with the starting solutions (27.3 µg/g ± 14 %RSD for the 27 µg/g solution and 77.6 µg/g ± 8.3 %RSD for the 78 µg/g solution). Average Br and I concentrations deviate less than 10 % from solution concentration values. For the low I concentration solutions, the synthetic inclusions were too small to detect I. Thus, given suitable standard materials and sufficient

  4. On the application of ICP-MS techniques for measuring uranium and plutonium: a Nordic inter-laboratory comparison exercise

    DEFF Research Database (Denmark)

    Qiao, Jixin; Lagerkvist, Petra; Rodushkin, Ilia

    2018-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) techniques are widely used for determination of long-lived radionuclides and their isotopic ratios in the nuclear fields. Uranium (U) and Pu (Pu) isotopes have been determined by many researchers with ICP-MS due to its relatively high sensitiv...

  5. ICP-MS determination of rare earth elements, yttrium, uranium and thorium in niobium-tantalum rich samples

    International Nuclear Information System (INIS)

    Sunilkumar, Beena; Padmasubashini, V.

    2013-01-01

    ICP-MS is a powerful and extremely sensitive technique which has been applied successfully for the determination of REEs in diverse geological samples. In the present work, ICP-MS has been applied for the rapid determination of REEs, yttrium as well as uranium and thorium in niobium and tantalum rich samples, using a fluoride fusion method for sample dissolution

  6. Dating of Uranium Materials by Using Combination of ICP-MS and SIMS

    International Nuclear Information System (INIS)

    Stebelkov, Y.; Aleshin, M.; Elantyev, I.; Grachev, A.; Zhizhin, K.; Stebelkov, V.

    2015-01-01

    The age of nuclear and some other radioactive materials can be determined undoubtedly by using ICP-MS techniques. But it can be correct if only one nuclear or another radioactive material is presented in analyzed sample and no isotope-chronograph presented in background particles in significant quantities. For particle analysis, which can be implemented by using SIMS, these restrictions are not valid. Practically one particle always characterizes only one material and does not contain background isotopes-chronographs. But age determination is based on the result of measuring of the content ratio of Th230 and U234. The difference of ionization coefficients of uranium and thorium and dependence of these coefficients on composition of particle does not allow using this method directly for age determination. Nevertheless SIMS is useful for dating of uranium materials, especially if the sample can contain small amounts of different materials. In this case the analysis of different fragments of materials by SIMS can confirm or not confirm the result, had been obtained by ICP-MS. If all detected and analyzed particles and fragments will have the same ratio of ion currents of Th230 and U234, the result of ICP-MS is true. If particles and fragments will have different ratios the result of ICP-MS cannot be related to any of presented materials. But in the last case the ages of different materials can be still estimated if different fragments have different ages, but the same elemental composition. The ''age'' had been determined by ICP-MS can be correlated with the average ratio of ion currents of Th230 and U234 had been determined by SIMS for all analyzed particles or fragments. This correlation determines the ratio of ionization coefficients of uranium and thorium, which should be the same for particles with the same elemental composition. (author)

  7. Trace element analyses of fluid inclusions using laser ablation ICP-MS

    Directory of Open Access Journals (Sweden)

    Cong-ying Li

    2018-03-01

    Full Text Available Fluid inclusions are records of the physico-chemical conditions of fluid–rock interactions during magmatism, mineralization and fluid percolation and mixing processes. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS is a powerful tool for in situ analyses of small samples at micrometer levels. Here we report in situ analyses of fluid inclusions using LA-ICP-MS method. NIST SRM glasses and 23Na are generally used as external and internal standards for LA-ICP-MS analysis of fluid inclusion, respectively, although the RSD of microthermometric estimation of 23Na is about 20% and even worse, the background signal of Na is high for most ICP-MS. Using well-characterized natural fluids inclusion, we show that RESOlution S-155 laser system analyze fluid inclusions in quartz and determine the trace element concentrations. Resonetics RESOlution S-155 laser has the advantage of the motorized Z stage can be used to accommodate variation of sample height or sample topography and height difference between samples, which is very important for analyzing the fluid inclusion in quartz. Our results suggest laser energy density is 25 J/cm2, laser pulse repetition rates are commonly between 6 and 10 Hz to avoid the fissuring of quartz and obtain adequate results. For this LA-ICP-MS analysis, uncertainty on 35Cl content is around 40% because of intensity of the 35Cl signal is three orders of magnitude less intense than the intensity of the 23Na signal. Nevertheless, it is still a useful reference for fluid inclusion analyses in addition to 23Na. This technique can be applied to a range of hydrothermal geology problems, including determining the origins of ore forming brines and ore deposition processes, mapping metamorphic and hydrothermal fluid provinces and pathways, and constraining the effects of fluid–rock reactions and fluid mixing.

  8. Breaking through the uncertainty ceiling in LA-ICP-MS U-Pb geochronology

    Science.gov (United States)

    Horstwood, M.

    2016-12-01

    Sources of systematic uncertainty associated with session-to-session bias are the dominant contributor to the 2% (2s) uncertainty ceiling that currently limits the accuracy of LA-ICP-MS U-Pb geochronology. Sources include differential downhole fractionation (LIEF), `matrix effects' and ablation volume differences, which result in irreproducibility of the same reference material across sessions. Current mitigation methods include correcting for LIEF mathematically, using matrix-matched reference materials, annealing material to reduce or eliminate radiation damage effects and tuning for robust plasma conditions. Reducing the depth and volume of ablation can also mitigate these problems and should contribute to the reduction of the uncertainty ceiling. Reducing analysed volume leads to increased detection efficiency, reduced matrix-effects, eliminates LIEF, obviates ablation rate differences and reduces the likelihood of intercepting complex growth zones with depth, thereby apparently improving material homogeneity. High detection efficiencies (% level) and low sampling volumes (20um box, 1-2um deep) can now be achieved using MC-ICP-MS such that low volume ablations should be considered part of the toolbox of methods targeted at improving the reproducibility of LA-ICP-MS U-Pb geochronology. In combination with other strategies these improvements should be feasible on any ICP platform. However, reducing the volume of analysis reduces detected counts and requires a change of analytical approach in order to mitigate this. Appropriate strategies may include the use of high efficiency cell and torch technologies and the optimisation of acquisition protocols and data handling techniques such as condensing signal peaks, using log ratios and total signal integration. The tools required to break the 2% (2s) uncertainty ceiling in LA-ICP-MS U-Pb geochronology are likely now known but require a coherent strategy and change of approach to combine their implementation and realise

  9. Bioimaging of isosteric osmium and ruthenium anticancer agents by LA-ICP-MS.

    Science.gov (United States)

    Klose, Matthias H M; Theiner, Sarah; Kornauth, Christoph; Meier-Menches, Samuel M; Heffeter, Petra; Berger, Walter; Koellensperger, Gunda; Keppler, Bernhard K

    2018-03-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was used to study the spatial distribution of two metallodrugs with anticancer activities in vivo, namely the organoruthenium plecstatin-1 (1) and its isosteric osmium analogue (2), in liver, kidneys, muscles and tumours of treated mice bearing a CT-26 tumour after single-dose i.p. administration. To the best of our knowledge, this is the first time that the spatial distribution of an osmium drug candidate has been investigated using LA-ICP-MS in tissues. Independent measurements of the average ruthenium and osmium concentration via microwave digestion and ICP-MS in organs and tumours were in good agreement with the LA-ICP-MS results. Matrix-matched standards (MMS) ranging from 1 to 30 μg g -1 were prepared to quantify the spatial distributions of the metals and the average metal content of the MMS samples was additionally quantified by ICP-MS after microwave digestion. The recoveries for osmium and ruthenium in the MMS were 105% and 101% on average, respectively, validating the sample preparation procedure of the MMS. Preparation of MMS was carried out under an argon atmosphere to prevent oxidation of osmium-species to the volatile OsO 4 . The highest metal concentrations were found in the liver, followed by kidney, lung and tumour tissues, while muscles displayed only very low quantities of the respective metal. Both metallodrugs accumulated in the cortex of the kidneys more strongly compared to the medulla. Interestingly, osmium from 2 was largely located at the periphery and tissue edges, whereas ruthenium from 1 was observed to penetrate deeper into the organs and tumours.

  10. Application of elemental bioimaging using laser ablation ICP-MS in forest pathology: distribution of elements in the bark of Picea sitchensis following wounding.

    Science.gov (United States)

    Siebold, Magdalena; Leidich, Patrick; Bertini, Martina; Deflorio, Giuliana; Feldmann, Jörg; Krupp, Eva M; Halmschlager, Erhard; Woodward, Steve

    2012-04-01

    Element distribution in the bark of two 20-year-old clones of Picea sitchensis following wounding was studied using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Bark was sampled at 0, 3, and 43 days after wounding and analysed using a focused Nd:YAG laser (266 nm). Intensities of (13)C, (25)Mg, (27)Al, (31)P, (32)S, (39)K, (48)Ca, (55)Mn, (57)Fe, (63)Cu and (64)Zn were measured by ICP-MS to study elemental distribution across the bark samples during the wound repair process. A clear accumulation of Mg, P and K at the boundary zone between the lesion and healthy tissue was detected in the wounded samples and was more distinctive at 43 than at 3 days after treatment. This zone of accumulation mapped onto the position of formation of the ligno-suberised boundary zone and differentiation of the wound periderm. These accumulations suggest major roles for Mg, P and K in the non-specific response of Sitka spruce both to wounding, possibly as co-factors to enzymes and energy utilisation. The LA-ICP-MS method developed in this work proved useful to study spatial element distribution across bark samples and has great potential for applications in other areas of plant pathology research.

  11. Application of elemental bioimaging using laser ablation ICP-MS in forest pathology: distribution of elements in the bark of Picea sitchensis following wounding

    International Nuclear Information System (INIS)

    Siebold, Magdalena; Leidich, Patrick; Bertini, Martina; Feldmann, Joerg; Deflorio, Giuliana; Woodward, Steve; Krupp, Eva M.; Halmschlager, Erhard

    2012-01-01

    Element distribution in the bark of two 20-year-old clones of Picea sitchensis following wounding was studied using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Bark was sampled at 0, 3, and 43 days after wounding and analysed using a focused Nd:YAG laser (266 nm). Intensities of 13 C, 25 Mg, 27 Al, 31 P, 32 S, 39 K, 48 Ca, 55 Mn, 57 Fe, 63 Cu and 64 Zn were measured by ICP-MS to study elemental distribution across the bark samples during the wound repair process. A clear accumulation of Mg, P and K at the boundary zone between the lesion and healthy tissue was detected in the wounded samples and was more distinctive at 43 than at 3 days after treatment. This zone of accumulation mapped onto the position of formation of the ligno-suberised boundary zone and differentiation of the wound periderm. These accumulations suggest major roles for Mg, P and K in the non-specific response of Sitka spruce both to wounding, possibly as co-factors to enzymes and energy utilisation. The LA-ICP-MS method developed in this work proved useful to study spatial element distribution across bark samples and has great potential for applications in other areas of plant pathology research. (orig.)

  12. Application of elemental bioimaging using laser ablation ICP-MS in forest pathology: distribution of elements in the bark of Picea sitchensis following wounding

    Energy Technology Data Exchange (ETDEWEB)

    Siebold, Magdalena [University of Aberdeen, Department of Plant and Soil Science, Institute of Biological and Environmental Sciences, Aberdeen (United Kingdom); University of Natural Resources and Applied Life Sciences Vienna, Department of Forest and Soil Sciences, Institute of Forest Entomology, Forest Pathology and Forest Protection, Vienna (Austria); Georg-August University Goettingen, Division of Plant Pathology and Crop Protection, Department of Crop Sciences, Goettingen (Germany); Leidich, Patrick; Bertini, Martina; Feldmann, Joerg [University of Aberdeen, TESLA, Trace Element Speciation Laboratory, Department of Chemistry, Aberdeen (United Kingdom); Deflorio, Giuliana; Woodward, Steve [University of Aberdeen, Department of Plant and Soil Science, Institute of Biological and Environmental Sciences, Aberdeen (United Kingdom); Krupp, Eva M. [University of Aberdeen, TESLA, Trace Element Speciation Laboratory, Department of Chemistry, Aberdeen (United Kingdom); University of Aberdeen, ACES, Aberdeen Centre of Environmental Sustainability, Aberdeen (United Kingdom); Halmschlager, Erhard [University of Natural Resources and Applied Life Sciences Vienna, Department of Forest and Soil Sciences, Institute of Forest Entomology, Forest Pathology and Forest Protection, Vienna (Austria)

    2012-04-15

    Element distribution in the bark of two 20-year-old clones of Picea sitchensis following wounding was studied using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Bark was sampled at 0, 3, and 43 days after wounding and analysed using a focused Nd:YAG laser (266 nm). Intensities of {sup 13} C, {sup 25}Mg, {sup 27}Al, {sup 31}P, {sup 32}S, {sup 39}K, {sup 48}Ca, {sup 55}Mn, {sup 57}Fe, {sup 63}Cu and {sup 64}Zn were measured by ICP-MS to study elemental distribution across the bark samples during the wound repair process. A clear accumulation of Mg, P and K at the boundary zone between the lesion and healthy tissue was detected in the wounded samples and was more distinctive at 43 than at 3 days after treatment. This zone of accumulation mapped onto the position of formation of the ligno-suberised boundary zone and differentiation of the wound periderm. These accumulations suggest major roles for Mg, P and K in the non-specific response of Sitka spruce both to wounding, possibly as co-factors to enzymes and energy utilisation. The LA-ICP-MS method developed in this work proved useful to study spatial element distribution across bark samples and has great potential for applications in other areas of plant pathology research. (orig.)

  13. A novel procedure for Rubidium separation and its isotope measurements on geological samples by MC-ICP-MS

    Science.gov (United States)

    Ma, J.; Zhang, Z.; Wei, G.; Zhang, L.

    2017-12-01

    A method including a novel column Rb separation procedure and high-precision Rb isotope measurement in geological materials by using multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) in standard-sample-bracketing (SSB) mode has been developed. Sr-Spec resin was employed, in which the distribution coefficients for Rb, K, Ba and Sr are different in nitric acid, to sequentially separate them from the matrix. The dissolved samples were loaded on the column in 3 M HNO3, the main matrix such as Al, Ca, Fe, Mg, Mn and Na were removed by rinsing with 4.5 mL HNO3, Rb and K were then sequentially eluted by 3 M HNO3 in different volumes. After that, Ba was eluted by 8 M HNO3, and Sr was finally eluted by Milli-Q water. This enable us to collect the pure Rb, K, Ba and Sr one by one with recovery close to 100% for their isotopic compositions measurement on MC-ICP-MS. We here focus on Rb isotope measurement. The measurement using MC-ICP-MS yielded an internal precision for δ87Rb of external precision was generally better than ± 0.06‰ (2SD) based on the long-term results of the Rb standard solutions NIST SRM 984. A series of geological rock standards, were analyzed using this method, and the results indicate significant Rb isotope differences in different geologic materials. This will provide a powerful tool to investigate Rb isotope fractionation during geological processes.Based on this method, Rb isotope compositions from a basaltic weathering profile were carried out. The data show the lighter Rb (85Rb) isotope is preferentially leached from the weathering profile and remains heavy Rb isotope (87Rb) in the weathered residues during the incipient weathering stage. From the moderate to advanced weathering stage, the significant variations of Rb isotope were observed and multiple factors, such as leaching, adsorption, desorption, and precipitation, should play important role in fractionating Rb isotope.

  14. High-precision isotopic characterization of USGS reference materials by TIMS and MC-ICP-MS

    Science.gov (United States)

    Weis, Dominique; Kieffer, Bruno; Maerschalk, Claude; Barling, Jane; de Jong, Jeroen; Williams, Gwen A.; Hanano, Diane; Pretorius, Wilma; Mattielli, Nadine; Scoates, James S.; Goolaerts, Arnaud; Friedman, Richard M.; Mahoney, J. Brian

    2006-08-01

    The Pacific Centre for Isotopic and Geochemical Research (PCIGR) at the University of British Columbia has undertaken a systematic analysis of the isotopic (Sr, Nd, and Pb) compositions and concentrations of a broad compositional range of U.S. Geological Survey (USGS) reference materials, including basalt (BCR-1, 2; BHVO-1, 2), andesite (AGV-1, 2), rhyolite (RGM-1, 2), syenite (STM-1, 2), granodiorite (GSP-2), and granite (G-2, 3). USGS rock reference materials are geochemically well characterized, but there is neither a systematic methodology nor a database for radiogenic isotopic compositions, even for the widely used BCR-1. This investigation represents the first comprehensive, systematic analysis of the isotopic composition and concentration of USGS reference materials and provides an important database for the isotopic community. In addition, the range of equipment at the PCIGR, including a Nu Instruments Plasma MC-ICP-MS, a Thermo Finnigan Triton TIMS, and a Thermo Finnigan Element2 HR-ICP-MS, permits an assessment and comparison of the precision and accuracy of isotopic analyses determined by both the TIMS and MC-ICP-MS methods (e.g., Nd isotopic compositions). For each of the reference materials, 5 to 10 complete replicate analyses provide coherent isotopic results, all with external precision below 30 ppm (2 SD) for Sr and Nd isotopic compositions (27 and 24 ppm for TIMS and MC-ICP-MS, respectively). Our results also show that the first- and second-generation USGS reference materials have homogeneous Sr and Nd isotopic compositions. Nd isotopic compositions by MC-ICP-MS and TIMS agree to within 15 ppm for all reference materials. Interlaboratory MC-ICP-MS comparisons show excellent agreement for Pb isotopic compositions; however, the reproducibility is not as good as for Sr and Nd. A careful, sequential leaching experiment of three first- and second-generation reference materials (BCR, BHVO, AGV) indicates that the heterogeneity in Pb isotopic compositions

  15. Potassium Stable Isotopic Compositions Measured by High-Resolution MC-ICP-MS

    Science.gov (United States)

    Morgan, Leah E.; Lloyd, Nicholas S.; Ellam, Robert M.; Simon, Justin I.

    2012-01-01

    Potassium isotopic (K-41/K-39) compositions are notoriously difficult to measure. TIMS measurements are hindered by variable fractionation patterns throughout individual runs and too few isotopes to apply an internal spike method for instrumental mass fractionation corrections. Internal fractionation corrections via the K-40/K-39 ratio can provide precise values but assume identical K-40/K-39 ratios (e.g. 0.05% (1sigma) in [1]); this is appropriate in some cases (e.g. identifying excess K-41) but not others (e.g., determining mass fractionation effects and metrologically traceable isotopic abundances). SIMS analyses have yielded measurements with 0.25% precisions (1sigma) [2]. ICP-MS analyses are significantly affected by interferences from molecular species such as Ar-38H(+) and Ar-40H(+) and instrument mass bias. Single collector ICP-MS instruments in "cold plasma" mode have yielded uncertainties as low as 2% (1sigma, e.g. [3]). Although these precisions may be acceptable for some concentration determinations, they do not resolve isotopic variation in terrestrial materials. Here we present data from a series of measurements made on the Thermo Scientific NEPTUNE Plus multi-collector ICP-MS that demonstrate the ability to make K-41/K-39 ratio measurements with 0.07% precisions (1sigma). These data, collected on NIST K standards, indicate the potential for MC-ICP-MS measurements to look for K isotopic variations at the sub-permil level. The NEPTUNE Plus can sufficiently resolve 39K and 41K from the interfering 38ArH+ and 40ArH+ peaks in wet cold plasma and high-resolution mode. Measurements were made on small but flat, interference-free, plateaus (ca. 50 ppm by mass width for K-41). Although ICP-MS does not yield accurate K-41/K-39 values due to significant instrumental mass fractionation (ca. 6%), this bias can be sufficiently stable over the time required for several measurements so that relative K-41/K-39 values can be precisely determined via sample

  16. Study of HPLC/ICP-MS coupling for the As speciation; Estudo de um acoplamento de HPLC/ICP-MS para a especiacao do As

    Energy Technology Data Exchange (ETDEWEB)

    Cortez, Bruna C.G.; Oliveira, Arno Heeren de [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear]. E-mail: brunacortez2004@yahoo.com.br; heeren@nuclear.ufmg.br

    2005-07-01

    Trace metals in the environment may provide benefit or risk to humans, other life forms, and the environment. More robust and information-rich trace and ultra-trace analyses are needed to all adequate risk/benefit assessments. Further, it is no longer adequate to consider only the total trace metal or metalloid, because the impact of elements on ecological systems or biological organisms is not necessarily given by total element concentrations alone. It is necessary to determine the chemical form (species) of the element, primarily the oxidation state or the organometallic nature, because different species of the same metal can range from essential to innocuous to toxic. The actual toxicity levels from different arsenic compounds vary greatly. Inorganic arsenic is considered the most acutely toxic form; arsenite (As{sup III}) is more toxic than arsenate (As{sup V}). The chronic toxicity of arsenic compounds is currently not well understood and is actively being researched. In this study, the viability of the ICP-MS detector coupled with High Performance Liquid Chromatography (HPLC) was tested in 21 water samples from the Das Velhas River, Minas Gerais state, in Brazil. The results showed that the low detection limits and the ease coupling HPLC system - which offers a rugged and versatile separation technique - makes ICP-MS a successful detection method for arsenic speciation analysis. (author)

  17. ICP-MS: suitable method to study the metals distribution in estuarine regions; ICP-MS metodo adequado para o estudo da distribuicao de metais em regioes estuarinas

    Energy Technology Data Exchange (ETDEWEB)

    Vasconcelos, Danilo C.; Oliveira, Arno H. [Minas Gerais Univ., Belo Horizonte, MG (Brazil). Dept. de Engenharia Nuclear]. E-mail: danilochagas@yahoo.com.br; heeren@nuclear.ufmg.br; Santos, Silvio J. dos; Brito, Veronica F.O.; Severo, Maria Isabel G. [Universidade Estadual de Santa Cruz, Ilheus, BA (Brazil). Dept. de Ciencias Biologicas

    2005-07-01

    Anthropogenic inputs of pollutants such as heavy metals into the marine environment have increased their levels to large extents within past a few decades. These pollutants tend to accumulate in the bottom sediments. As a result, ecosystems such as seaports or other industrialized coastal areas that have chronic inputs of metals have highly contaminated sediments. This characteristic has led to concerns over the ecological effects that may be associated with sediment quality. Of particular concern are toxic effects and the potential for bioaccumulation of metals in biota exposed to the sediments. The bivalves Crassostrea rhizophorae, Lucina pectinata and Mytella falcata have been used as biomonitors of trace metal contamination in two estuaries from Ilheus city, Bahia state, in Brazil. Bivalves, sediment and water samples were collected in March 2004 in Acuipe and Rio do Engenho mangroves. The proposed technique to analyze the studied matrices was the inductively coupled plasma mass spectrometry (ICP-MS). The results suggested that the studied molluscs are bioaccumulators of metals and showed the Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) as an adequate technique to determine a large range of inorganic elements, because its high sensibility and low detection limits. (author)

  18. Quantitative Evaluation of Cisplatin Uptake in Sensitive and Resistant Individual Cells by Single-Cell ICP-MS (SC-ICP-MS).

    Science.gov (United States)

    Corte Rodríguez, M; Álvarez-Fernández García, R; Blanco, E; Bettmer, J; Montes-Bayón, M

    2017-11-07

    One of the main limitations to the Pt-therapy in cancer is the development of associated drug resistance that can be associated with a significant reduction of the intracellular platinum concentration. Thus, intracellular Pt concentration could be considered as a biomarker of cisplatin resistance. In this work, an alternative method to address intracellular Pt concentration in individual cells is explored to permit the evaluation of different cell models and alternative therapies in a relatively fast way. For this aim, total Pt analysis in single cells has been implemented using a total consumption nebulizer coupled to inductively coupled plasma mass spectrometric detection (ICP-MS). The efficiency of the proposed device has been evaluated in combination with flow cytometry and turned out to be around 25% (cells entering the ICP-MS from the cells in suspension). Quantitative uptake studies of a nontoxic Tb-containing compound by individual cells were conducted and the results compared to those obtained by bulk analysis of the same cells. Both sets of data were statistically comparable. Thus, final application of the developed methodology to the comparative uptake of Pt-species in cisplatin resistant and sensitive cell lines (A2780cis and A2780) was conducted. The results obtained revealed the potential of this analytical strategy to differentiate between different cell lines of different sensitivity to the drug which might be of high medical interest.

  19. Determination of trace elements in seawater by air-flow injection/ICP-MS with chelating resin preconcentration

    International Nuclear Information System (INIS)

    Lee, Kyue-Hyung; Ohshima, Mitsuko; Motomizu, Shoji

    2002-01-01

    Multielement determination of major to trace metals in a deep seawater malt was accomplished by inductively coupled plasma-mass spectrometry (ICP-MS) together with inductively coupled plasma-atomic emission spectrometry (ICP-AES). Major elements, such as Na, K, Mg, and Ca, were measured by ICP-AES and normal continuos nebulization ICP-MS after sample dilution by 10 3 -10 6 fold. Fifteen trace elements in the concentrated metal solutions pretreated with cation-exchange resin or chelating resin could be simultaneously determined by air-flow injection/ICP-mass spectrometry (AFI/ICP-MS). Since the injection volume for AFI/ICP-MS was 25 μl, final samples volumes less than 500 μl were enough for several replicate measurements. Three different preconcentration methods assisted with AFI/ICP-MS were examined and could be successfully applied to a deep seawater malt. The analytical results of rate earth elements (REEs) and Co, Ni, Cu, Zn, Cd, and Pb obtained by AFI/ICP-MS coupled with disk filtration method using iminodiacetate (IDA)-type chelating resin were favorably agreed with the data obtained by AFI/ICP-MS coupled with column preconcentration method using chitosan-based chelating resin. (author)

  20. Study on the ICP-MS technology of trace uranium and plutonium in environmental water

    International Nuclear Information System (INIS)

    Zeng Min; Tian Junhua; Li Ye

    2006-10-01

    The method of detecting U and 239 Pu of the water in the environment was founded. 100 L water of river, reservoir and tap water were respectively sampled. The concentration of 239 Pu was analyzed by ICP-MS after the treatment by coprecipitation-anion exchange, the detection limit was 0.06 ng/L. Standard fitting curve and internal standard method was used to quantity, the result showed that the concentration of 239 Pu of the water of river, tap water was below the detection limit, the concentration of the water of reservoir was 10-14 g/L; all of the water were directly filtrated then detected by ICP-MS, the concentration of U of all the water was 0.5-1 μg/L. (authors)

  1. A laser ablation ICP-MS based method for multiplexed immunoblot analysis

    DEFF Research Database (Denmark)

    de Bang, Thomas Christian; Petersen, Jørgen; Pedas, Pai Rosager

    2015-01-01

    developed a multiplexed antibody-based assay and analysed selected PSII subunits in barley (Hordeum vulgare L.). A selection of antibodies were labelled with specific lanthanides and immunoreacted with thylakoids exposed to Mn deficiency after western blotting. Subsequently, western blot membranes were...... analysed by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), which allowed selective and relative quantitative analysis via the different lanthanides. The method was evaluated against established liquid chromatography electrospray ionization tandem mass spectrometry (LC...... by more than one technique. The developed method enables a higher number of proteins to be multiplexed in comparison to existing immunoassays. Furthermore, multiplexed protein analysis by LA-ICP-MS provides an analytical platform with high throughput appropriate for screening large collections of plants....

  2. ICP-MS Technology and Its Application to Study of Environmental Radioactivity

    International Nuclear Information System (INIS)

    Syarbaini

    2000-01-01

    Study on the behaviour of artificial radionuclides in environment can be performed by investigation of fallout radionuclides that were distributed in ecosystem components. Fall out radionuclides are artificial radionuclides distributed by the nuclear weapon test explosions at atmosphere in several ten years ago. The concentration of these radionuclides in ecosystem components are very low. For the measurement of their concentrations in environmental samples by conventional radiometric methods need a large samples, complicated chemical separation and long counting time. Application of ICP-MS is good alternative to solve this problem. ICP-MS (Inductively Coupled Plasma Mass Spectrometry) is multi elements analysis instrument that wide used in the field of analytical chemistry. It can determine elements at a concentration level of pg/ml in several minutes per sample without a long chemical separation and preconcentration process. (author)

  3. Analytical developments in ICP-MS for arsenic and selenium speciation. Application to granitic waters

    International Nuclear Information System (INIS)

    Garraud, Herve

    1999-01-01

    Nuclear waste storage in geological areas needs the understanding of the physico-chemistry of groundwaters interactions with surrounding rocks. Redox potential measurements and speciation, calculated from geochemical modelling are not significant for the determination of water reactivity. We have thus chosen to carry out experimental speciation by developing sensitive analytical tools with respect of specie chemical identity. We have studied two redox indicators from reference sites (thermal waters from Pyrenees, France): arsenic and selenium. At first, we have determined the concentrations in major ions (sulphide, sulphate, chloride, fluoride, carbonate, Na, K, Ca). Speciation was conducted by HPLC hyphenated to quadrupole ICP-MS and high resolution ICP-MS. These analyses have shown the presence of two new arsenic species in solution, in addition of a great reactivity of these waters during stability studies. A sampling, storage and analysis method is described. (author) [fr

  4. Electrothermal Vaporization-QQQ-ICP-MS for Determination of Chromium in Mainstream Cigarette Smoke Particulate.

    Science.gov (United States)

    Fresquez, Mark R; Gonzalez-Jimenez, Nathalie; Gray, Naudia; Valentin-Blasini, Liza; Watson, Clifford H; Pappas, R Steven

    2017-05-01

    Chromium is transported in mainstream tobacco smoke at very low concentrations. However, when chromium is deposited too deeply in the lungs for mucociliary clearance, or is in a particle that is too large to pass directly through tissues, it bioaccumulates in the lungs of smokers. It is important to determine the concentrations of chromium that are transported in mainstream smoke. Several reliable studies have resulted in reports of chromium concentrations in smoke particulate that were below limits of detection (LODs) for the instruments and methods employed. In this study, electrothermal vaporization-triple quad-inductively coupled plasma-mass spectrometry (ETV-QQQ-ICP-MS) was chosen for determination of chromium concentrations in mainstream smoke because of the high sensitivity of ETV combined with QQQ-ICP-MS. The smoke from five reference, quality control, and commercial cigarettes was analyzed using ETV-QQQ-ICP-MS with isotope dilution for quantitative determination of chromium. The method LOD was sufficiently low that chromium concentrations in mainstream smoke could indeed be determined. The chromium concentrations in the smoke particulate were between 0.60 and 1.03 ng/cigarette. The range of chromium concentrations was at or below previously reported LODs. Determination of the oxidation state of the chromium transported in mainstream smoke would also be important, in consideration of the fact that both chromium(III) and chromium(VI) oxidation states cause inhalation toxicity, but chromium(VI) is also a carcinogen. It was possible to separate the oxidation states using ETV-QQQ-ICP-MS. However, determination of individual species at the levels found in mainstream smoke particulate matter was not possible with the present method. Published by Oxford University Press 2017. This work is written by (a) US Government employee(s) and is in the public domain in the US.

  5. Speciation of the plutonium at trace levels by capillary electrophoresis-ICP-MS coupling

    International Nuclear Information System (INIS)

    Ambard, Ch.

    2007-01-01

    The CE-ICP-MS coupling allowed the development of new analytical methods for the study of plutonium (Pu) speciation at trace levels including complexation studies of this element by organic and inorganic ligands. First, a method, called dual detection, based on the simultaneous use of the UV-Visible spectrophotometer integrated in the capillary electrophoresis and the ICP-MS was developed and validated. It allows the unambiguous determination of electrophoretic mobilities for separated chemical species and gives a powerful tool for speciation studies. Then, the influence on Pu redox speciation of the buffer from the background electrolyte was evaluated. This study showed the implications of the electrolyte constituents' choice on Pu redox equilibrium in the sample. Furthermore, the CE-ICP-MS coupling was used for studying the Pu complexation at trace levels by some organic (NTA and DTPA) and inorganic ligands (carbonates). The behaviour of Pu valence +III, +IV and +VI was studied in the presence of buffer at near neutral pH. Different species of Pu were observed depending on the initial oxidation state of the plutonium. The study showed the potential of poly-amino-carboxylic acids, such as NTA and DTPA, for dissolving Pu precipitates, regardless its initial speciation. Finally, the carbonation of pentavalent neptunium, as an analogue of Pu(V), was achieved at very low concentration of Np (10 -8 mol.L -1 ). The formation of NpO 2 (CO 3 ) - at 25 C and 2,5*10 -2 mol.L -1 ionic strength was measured by CE-ICP-MS and found to consistent with literature data. (author)

  6. Analysis of radioactive corrosion test specimens by means of ICP-MS. Comparison with earlier methods

    International Nuclear Information System (INIS)

    Forsyth, Roy

    1997-07-01

    In June 1992, an ICP-MS instrument (Inductively Coupled Plasma-Mass Spectrometry) was commissioned for use with radioactive sample solutions at Studsvik Nuclear's Hot Cell Laboratory. For conventional environmental samples the instrument permits the simultaneous analysis of many trace elements, but the software used in evaluation of the mass spectra is based on a library of isotopic compositions relevant only for elements in the lithosphere. Fission products and actinides, however, have isotopic compositions which are significantly different from the natural elements, and which also vary with the burnup of the nuclear fuel specimen. Consequently, a spread-sheet had to be developed which could evaluate the mass spectra with these isotopic compositions. Following these preparations, a large number of samples (about 200) from SKB's experimental programme for the study of spent fuel corrosion have been analyzed by the ICP-MS technique. Many of these samples were archive solutions of samples which had been taken earlier in the programme. This report presents a comparison of the analytical results for uranium, plutonium, cesium, strontium and technetium by both the ICP-MS technique, and the previously used analytical methods. For three products, a satisfactory agreement between the results from the various methods was obtained, but for uranium and plutonium the ICP-MS method gave results which were 10-20% higher than the conventional methods. The comparison programme has also shown, not unexpectedly, that significant losses of plutonium from solution had occurred, by precipitation and/or absorption, in the archive solutions during storage. It can be expected that such losses also occur for the other actinides, and consequently, all the analytical results for actinides in older archive solutions must be treated with great caution. 9 refs

  7. Total Arsenic, Cadmium, and Lead Determination in Brazilian Rice Samples Using ICP-MS

    OpenAIRE

    Mataveli, Lidiane Raquel Verola; Buzzo, Márcia Liane; Arauz, Luciana Juncioni de; Carvalho, Maria de Fátima Henriques; Arakaki, Edna Emy Kumagai; Matsuzaki, Richard; Tiglea, Paulo

    2016-01-01

    This study is aimed at investigating a suitable method for rice sample preparation as well as validating and applying the method for monitoring the concentration of total arsenic, cadmium, and lead in rice by using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Various rice sample preparation procedures were evaluated. The analytical method was validated by measuring several parameters including limit of detection (LOD), limit of quantification (LOQ), linearity, relative bias, and rep...

  8. HPLC-ICP-MS compared with radiochemical detection for metabolite profiling of H-3-bromohexine in rat urine and faeces

    DEFF Research Database (Denmark)

    Jensen, B.P.; Gammelgaard, B.; Hansen, S.H.

    2005-01-01

    H-3-Bromohexine was dosed to rats as a model compound to allow comparison of HPLC-ICP-MS detection on bromine to radiochemical detection in an in vivo drug metabolism study. Metabolite profiles were obtained in urine and faeces extracts. No influence of the methanol gradient on the bromine response...... was observed in the range of 18 - 75% methanol. The sensitivity obtained by HPLC- ICP-MS was almost two orders of magnitude better than on-line H-3 radiochemical detection. For ICP- MS, the limit of detection was calculated to be 69 nM Br ( injection volume 100 mu l), corresponding to an absolute limit...

  9. Analysis of plutonium isotopes in marine samples by radiometric, ICP-MS and AMS techniques

    International Nuclear Information System (INIS)

    Lee, S.H.; Gastaud, J.; La Rosa, J.J.; Liong Wee Kwong, L.; Povinec, P.P.; Wyse, E.

    2001-01-01

    IAEA reference materials (radionuclides in the marine environment) collected in areas affected by nuclear reprocessing plants and nuclear weapons tests have been analysed by semiconductor alpha-spectrometry (SAS), liquid scintillation spectrometry (LSS) and mass spectrometric techniques (high resolution ICP-MS and AMS) with the aim of developing analytical procedures and to study the geochemical behavior of plutonium in the marine environment. The Pu results obtained by SAS, ICP-MS and AMS were in reasonably good agreement (R 2 = 0.99). The mean atom ratios of 240 Pu/ 239 Pu in IAEA reference materials, IAEA-134, 135 and 381 were (0.212±0.010), (0.211±0.004) and (0.242±0.004), respectively. IAEA-384 (Fangataufa Lagoon Sediment) gave a 240 Pu/ 239 Pu mean atom ratio of 0.051±0.001. The results of 241 Pu obtained buy ICP-MS and LSS also show reasonable agreement (R 2 = 0.91). Pu isotopic signatures were useful in tracing Pu origin and in interpreting biogeochemical processes involving Pu in the marine environment. (author)

  10. Measurement of technetium-99 in Marshall Islands soil samples by ICP-MS

    Science.gov (United States)

    Tagami; Uchida; Hamilton; Robison

    2000-07-01

    Extraction techniques for recovery of technetium-99 (99Tc) for Inductively Coupled Plasma Mass Spectrometry (ICP-MS) measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (MI) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for 99Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the 99Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The 99Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq g(-1) dry weight (dw). The limit of detection for 99Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq g(-1) dw under standard operating conditions.

  11. Quantification of pharmaceutical peptides in human plasma by LC-ICP-MS sulfur detection

    DEFF Research Database (Denmark)

    Møller, Laura Hyrup; Macherius, André; Hansen, Thomas Hesselhøj

    2016-01-01

    A method for quantification of a pharmaceutical peptide in human plasma was developed using gradient elution LC-ICP-MS. A membrane desolvation (MD) system was applied to remove organic solvents from the eluent prior to the detection as SO+ in the dynamic reaction cell (DRC) of the ICP-DRC-MS inst......A method for quantification of a pharmaceutical peptide in human plasma was developed using gradient elution LC-ICP-MS. A membrane desolvation (MD) system was applied to remove organic solvents from the eluent prior to the detection as SO+ in the dynamic reaction cell (DRC) of the ICP......-DRC-MS instrument and subsequent quantification by post-column isotope dilution (IDA). Plasma proteins were precipitated prior to analysis. Analytical figures of merit including linearity, precision, LOD, LOQ and accuracy were considered satisfactory for analysis of plasma samples. The selectivity of the developed...... method was demonstrated for five pharmaceutically relevant peptides: desmopressin, penetratin, substance P, PTH (1-34) and insulin. Preliminary experiments on an ICP-MS/MS system using oxygen to reduce the effect of organic solvents were also performed to compare sensitivity. The results of the study...

  12. Simultaneous Speciation of Arsenic, Selenium, and Chromium by HPLC-ICP-MS

    Science.gov (United States)

    Wolf, Ruth E.; Morman, Suzette A.; Morrison, Jean M.; Lamothe, Paul J.

    2008-01-01

    An adaptation of an analytical method developed for chromium speciation has been utilized for the simultaneous determination of As(III), As(V), Se(IV), Se(VI), Cr(III), and Cr(VI) species using high performance liquid chromatography (HPLC) separation with ICP-MS detection. Reduction of interferences for the determination of As, Se, and Cr by ICP-MS is a major consideration for this method. Toward this end, a Dynamic Reaction Cell (DRC) ICP-MS system was used to detect the species eluted from the chromatographic column. A variety of reaction cell gases and conditions may be utilized, and the advantages and limitations of the gases tested to date will be presented and discussed. The separation and detection of the As, Se, and Cr species of interest can be achieved using the same chromatographic conditions in less than 2 minutes by complexing the Cr(III) with EDTA prior to injection on the HPLC column. Practical aspects of simultaneous speciation analysis will be presented and discussed, including issues with HPLC sample vial contamination, standard and sample contamination, species stability, and considerations regarding sample collection and preservation methods. The results of testing to determine the method's robustness to common concomitant element and anion effects will also be discussed. Finally, results will be presented using the method for the analysis of a variety of environmental and geological samples including waters, soil leachates and simulated bio-fluid leachates.

  13. Measurement of technetium-99 in Marshall Islands soil samples by ICP-MS

    International Nuclear Information System (INIS)

    Tagami, K.; Uchida, S.; Hamilton, T.; Robison, W.

    2000-01-01

    Extraction techniques for recovery of technetium-99 ( 99 Tc) for Inductively Coupled Plasma Mass Spectrometry (ICP-MS) measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (M1) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for 99 Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the 99 Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The 99 Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq g -1 dry weight (dw). The limit of detection for 99 Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq g -1 dw under standard operating conditions

  14. Measurement of technetium-99 in Marshall Islands soil samples by ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Tagami, K. E-mail: k_tagami@nirs.go.jp; Uchida, S.; Hamilton, T.; Robison, W

    2000-07-15

    Extraction techniques for recovery of technetium-99 ({sup 99}Tc) for Inductively Coupled Plasma Mass Spectrometry (ICP-MS) measurements were evaluated using soil samples collected from the Marshall Islands. The results of three different extraction techniques were compared: (M1) acid leaching of Tc from ashed soil; (M2) acid leaching of Tc from raw dry soil; and (M3) Tc volatilization from ashed soil using a combustion apparatus. Total Tc recoveries varied considerably between the extraction techniques but each method yielded similar analytical results for {sup 99}Tc. Applications of these extraction techniques to a series of environmental samples and ICP-MS measurements have yielded first data on the {sup 99}Tc content of Marshall Islands soil samples contaminated with close-in radioactive fallout from nuclear weapons testing. The {sup 99}Tc activity concentration in the soil samples ranged between 0.1 and 1.1 mBq g{sup -1} dry weight (dw). The limit of detection for {sup 99}Tc by ICP-MS was 0.17 mBq per sample or 0.014 mBq g{sup -1} dw under standard operating conditions.

  15. A multifunctional probe for ICP-MS determination and multimodal imaging of cancer cells.

    Science.gov (United States)

    Yang, Bin; Zhang, Yuan; Chen, Beibei; He, Man; Yin, Xiao; Wang, Han; Li, Xiaoting; Hu, Bin

    2017-10-15

    Inductively coupled plasma-mass spectrometry (ICP-MS) based bioassay and multimodal imaging have attracted increasing attention in the current development of cancer research and theranostics. Herein, a sensitive, simple, timesaving, and reliable immunoassay for cancer cells counting and dual-modal imaging was proposed by using ICP-MS detection and down-conversion fluorescence (FL)/upconversion luminescence (UCL) with the aid of a multifunctional probe for the first time. The probe consisted of a recognition unit of goat anti-mouse IgG to label the anti-EpCAM antibody attached cells, a fluorescent dye (Cy3) moiety for FL imaging as well as upconversion nanoparticles (UCNPs) tag for both ICP-MS quantification and UCL imaging of cancer cells. Under the optimized conditions, an excellent linearity and sensitivity were achieved owing to the signal amplification effect of nanoparticles and low spectral interference. Accordingly, a limit of detection (3σ) of 1×10 2 HepG2 cells and a relative standard deviation of 7.1% for seven replicate determinations of 1×10 3 HepG2 cells were obtained. This work proposed a method to employ UCNPs with highly integrated functionalities enabling us not only to count but also to see the cancer cells, opening a promising avenue for biological research and clinical theranostics. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. LC coupled to ESI, MALDI and ICP MS - A multiple hyphenation for metalloproteomic studies.

    Science.gov (United States)

    Coufalíková, Kateřina; Benešová, Iva; Vaculovič, Tomáš; Kanický, Viktor; Preisler, Jan

    2017-05-22

    A new multiple detection arrangement for liquid chromatography (LC) that supplements conventional electrospray ionization (ESI) mass spectrometry (MS) detection with two complementary detection techniques, matrix-assisted laser desorption/ionization (MALDI) MS and substrate-assisted laser desorption inductively coupled plasma (SALD ICP) MS has been developed. The combination of the molecular and elemental detectors in a single separation run is accomplished by utilizing a commercial MALDI target made of conductive plastic. The proposed platform provides a number of benefits in today's metalloproteomic applications, which are demonstrated by analysis of a metallothionein mixture. To maintain metallothionein complexes, separation is carried out at a neutral pH. The effluent is split; a major portion is directed to ESI MS while the remaining 1.8% fraction is deposited onto a plastic MALDI target. Dried droplets are overlaid with MALDI matrix and analysed consecutively by MALDI MS and SALD ICP MS. In the ESI MS spectra, the MT isoform complexes with metals and their stoichiometry are determined; the apoforms are revealed in the MALDI MS spectra. Quantitative determination of metallothionein isoforms is performed via determination of metals in the complexes of the individual protein isoforms using SALD ICP MS. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Association of glass fragments by their trace elemental content using ICP-MS and LA-ICP-MS in the analysis scheme

    Science.gov (United States)

    Almirall, Jose R.; Montero, Shirly; Furton, Kenneth G.

    2002-08-01

    The importance of glass as evidence of association between a crime event and a suspect has been recognized for some time. Glass is a fragile material that is often found at the scenes of crimes such as burglaries, hit-and-run accidents and violent crime offenses. The physical and chemical properties of glass can be used to differentiate between possible sources and as evidence of association between two fragments of glass thought to originate from the same source. Refractive index (RI) comparisons have been used for this purpose but due to the improved control over glass manufacturing processes, RI values often cannot differentiate glasses, even if the glass originates from different sources. Elemental analysis methods such as NAA, XRF, ICP-AES, and Inductively Coupled Plasma Mass Spectrometry (ICP-MS) have also been used for the comparison of trace elemental compositions and these techniques have been shown to provide an improvement in the discrimination of glass fragments over RI comparisons alone. The multi-element capability and the sensitivity of ICP-MS combined with the simplified sample introduction of laser ablation prior to ion detection provides for an excellent and relatively non-destructive technique for elemental analysis of glass fragments. The methodology for solution analysis (digestion procedure) and solid sample analysis (laser ablation) of glass is reported and the analytical results are compared. An isotope dilution method is also reported as a high precision technique for elemental analysis of glass fragments. The optimum sampling parameters for laser ablation, for semi-quantitative analysis and element ratio comparisons are also presented. Finally, the results of a case involving the breaking of 15 vehicle windows in an airport parking lot and the association of a suspect to the breakings by the glass fragments found on his person are also presented.

  18. Single-cell analysis by ICP-MS/MS as a fast tool for cellular bioavailability studies of arsenite.

    Science.gov (United States)

    Meyer, S; López-Serrano, A; Mitze, H; Jakubowski, N; Schwerdtle, T

    2018-01-24

    Single-cell inductively coupled plasma mass spectrometry (SC-ICP-MS) has become a powerful and fast tool to evaluate the elemental composition at a single-cell level. In this study, the cellular bioavailability of arsenite (incubation of 25 and 50 μM for 0-48 h) has been successfully assessed by SC-ICP-MS/MS for the first time directly after re-suspending the cells in water. This procedure avoids the normally arising cell membrane permeabilization caused by cell fixation methods (e.g. methanol fixation). The reliability and feasibility of this SC-ICP-MS/MS approach with a limit of detection of 0.35 fg per cell was validated by conventional bulk ICP-MS/MS analysis after cell digestion and parallel measurement of sulfur and phosphorus.

  19. Post hoc interlaboratory comparison of single particle ICP-MS size measurements of NIST gold nanoparticle reference materials.

    Science.gov (United States)

    Montoro Bustos, Antonio R; Petersen, Elijah J; Possolo, Antonio; Winchester, Michael R

    2015-09-01

    Single particle inductively coupled plasma-mass spectrometry (spICP-MS) is an emerging technique that enables simultaneous measurement of nanoparticle size and number quantification of metal-containing nanoparticles at realistic environmental exposure concentrations. Such measurements are needed to understand the potential environmental and human health risks of nanoparticles. Before spICP-MS can be considered a mature methodology, additional work is needed to standardize this technique including an assessment of the reliability and variability of size distribution measurements and the transferability of the technique among laboratories. This paper presents the first post hoc interlaboratory comparison study of the spICP-MS technique. Measurement results provided by six expert laboratories for two National Institute of Standards and Technology (NIST) gold nanoparticle reference materials (RM 8012 and RM 8013) were employed. The general agreement in particle size between spICP-MS measurements and measurements by six reference techniques demonstrates the reliability of spICP-MS and validates its sizing capability. However, the precision of the spICP-MS measurement was better for the larger 60 nm gold nanoparticles and evaluation of spICP-MS precision indicates substantial variability among laboratories, with lower variability between operators within laboratories. Global particle number concentration and Au mass concentration recovery were quantitative for RM 8013 but significantly lower and with a greater variability for RM 8012. Statistical analysis did not suggest an optimal dwell time, because this parameter did not significantly affect either the measured mean particle size or the ability to count nanoparticles. Finally, the spICP-MS data were often best fit with several single non-Gaussian distributions or mixtures of Gaussian distributions, rather than the more frequently used normal or log-normal distributions.

  20. QEMSCAN+LA-ICP-MS: a 'big data' generator for sedimentary provenance analysis

    Science.gov (United States)

    Vermeesch, Pieter; Rittner, Martin; Garzanti, Eduardo

    2017-04-01

    Sedimentary provenance may be traced by 'fingerprinting' sediments with chemical, mineralogical or isotopic means. Normally, each of these provenance proxies is characterised on a separate aliquot of the same sample. For example, the chemical composition of the bulk sample may be analysed by X-ray fluorescence (XRF) on one aliquot, framework petrography on another, heavy mineral analysis on a density separate of a third split, and zircon U-Pb dating on a further density separate of the heavy mineral fraction. The labour intensity of this procedure holds back the widespread application of multi-method provenance studies. We here present a new method to solve this problem and avoid mineral separation by coupling a QEMSCAN electron microscope to an LA-ICP-MS instrument and thereby generate all four aforementioned provenance datasets as part of the same workflow. Given a polished hand specimen, a petrographic thin section, or a grain mount, the QEMSCAN+LA-ICP-MS method produces chemical and mineralogical maps from which the X-Y coordinates of the datable mineral are extracted. These coordinates are subsequently passed on to the laser ablation system for isotopic and, hence, geochronological analysis. In the process of finding all the zircons in a sediment grain mount, the QEMSCAN yields the compositional and mineralogical compositions as byproducts. We have applied the new QEMSCAN+LA-ICP-MS instrument suite to over 100 samples from three large sediment routing systems: (1) the Tigris-Euphrates river catchments and Rub' Al Khali desert in Arabia; (2) the Nile catchment in northeast Africa and (3) desert and beach sands between the Orange and Congo rivers in southwest Africa. These studies reveal (1) that Rub' Al Khali sand is predominantly derived from the Arabian Shield and not from Mesopotamia; (2) that the Blue Nile is the principal source of Nile sand; and (3) that Orange River sand is carried northward by longshore drift nearly 1,800km from South Africa to southern

  1. Speciation of the plutonium at trace levels by capillary electrophoresis-ICP-MS coupling

    International Nuclear Information System (INIS)

    Ambard, Ch.

    2007-01-01

    The CE-ICP-MS coupling allowed the development of new analytical methods for the study of plutonium speciation at trace levels including complexation studies of this element by organic and inorganic ligands. First, a method, called dual detection, based on the simultaneous use of the UV-Visible spectrophotometer integrated in the capillary electrophoresis and the ICPMS was developed and validated. It allows the unambiguous determination of electrophoretic mobilities for separated chemical species and gives a powerful tool for speciation studies. Then, the influence on plutonium redox speciation of the buffer from the background electrolyte was evaluated. This study showed the implications of the electrolyte constituents' choice on plutonium redox equilibrium in the sample. Furthermore, the CE-ICP-MS coupling was used for studying the plutonium complexation at trace levels by some organic (NTA and DTPA) and inorganic ligands (carbonates). The behaviour of plutonium valence +III, +IV and +VI was studied in the presence of buffer at near neutral pH. Different species of plutonium were observed depending on the initial oxidation state of the plutonium. This study showed the potential of poly-amino-carboxylic acids, such as NTA and DTPA, for dissolving plutonium precipitates, regardless its initial speciation. Finally, the carbonation of pentavalent neptunium, as an analogue of Pu(V), was achieved at very low concentration of Np (10 -8 mol.L -1 ). The formation constant of NpO 2 (CO 3 )- at 25 deg. C and 2,5 x 10 -2 mol.L -1 ionic strength was measured by CE-ICP-MS and found to be consistent with literature data. (author)

  2. Ultratrace analysis of {sup 129}I in sediments by ICP-MS with collision cell

    Energy Technology Data Exchange (ETDEWEB)

    Izmer, A.V.; Becker, J.S. [Research Center Juelich (Germany). Central Div. of Analytical Chemistry; Boulyga, S.F. [Mainz Univ. (Germany). Inst. for Inorganic Chemistry and Analytical Chemistry; Zoriy, M.V. [Research Center Juelich (Germany). Central Div. of Analytical Chemistry]|[Research Center Juelich (Germany). Dept. for Safety and Radiation Protection

    2004-07-01

    The aim of the work was the development of a rapid and high-sensitive analytical method using ICP-MS with hexapole collision cell (ICP-CC-MS) for the determination of low 129I+/127I+ isotope ratios in synthetic lab standards and environmental samples. A special direct sample introduction device for iodine extraction via the gas phase from solid environmental material coupled on-line to ICP-CC-QMS was developed. The detection limit for 129I+ determination in aqueous solution and soil samples via gas-phase extraction was determined to be of 0.8 pg/g and 30 pg/g, respectively. (orig.)

  3. Trace element analysis of mineral water samples by PIXE and ICP-MS

    International Nuclear Information System (INIS)

    Kennedy, V.John; Augusthy, A.; Varier, K. M.; Magudapathy, P.; Panchapakesan, S.; Nair, K.G.M.

    1998-01-01

    Trace elements present in bottled mineral water have been studied by PIXE and ICP-MS. Samples from ten different brands of brands of bottled mineral water were prepared by preconcentration techniques. Measurements were carried out using the 2 MeV proton beam obtained from 3 MV Tandem pelletron accelerator at the Institute of Physics, Bhubaneswar. Our results are compared with Indian standard packaged natural mineral water specifications, World Health Organisation (WHO) and European guidelines for drinking water standards. Concentration of aluminum was found to be more in one of the brands. In general, our results are comparable to the above standards. (author)

  4. Identification of target organs of copper nanoparticles with ICP-MS technique

    International Nuclear Information System (INIS)

    Zhen Chen; Huan Meng; Yun Wang; Chengcheng Zhang; Yuliang Zhao

    2007-01-01

    Nanosized copper particles are widely used in fields of lubricants, polymers/plastic, metallic coating and ink. Recently, we found that copper particles in different sizes can lead to different toxicological effects. To clarify the target organs of copper particles of different sizes, the inductively coupled plasma mass spectroscopy (ICP-MS) was employed to evaluate the distribution of copper in different organs of mice after a single dose oral exposure. The results suggest that the main target organs for copper nanoparticles are kidney, liver and blood. Liver is the main damaged organ. (author)

  5. Applications of a glove-box ICP-MS for the analysis of nuclear materials

    International Nuclear Information System (INIS)

    Garcia Alonso, J.I.; Babelot, J.F.; Glatz, J.P.; Cromboom, O.; Koch, L.

    1993-01-01

    The relatively new analytical technique, Inductively Coupled Plasma Mass Spectrometry (ICP-MS), has been used for the analysis of nuclear materials stemming from different parts of the nuclear fuel cycle. The original instrument has been modified in order to work with radioactive materials in a glove box. The plasma torch and vacuum interface are situated inside the glove box while the mass spectrometer and associated electronics are outside. Samples analysed include fresh nuclear fuels (natural impurities), spent fuels (fission products and actinides), reprocessing solutions (minor actinides) and leachates of spent fuel and high level waste glasses (natural elements, fission products and actinides). (orig.)

  6. Chemical Characterization of Bed Material Coatingsby LA-ICP-MS and SEM-EDS

    Science.gov (United States)

    Piispanen, M. H.; Mustonen, A. J.; Tiainen, M. S.; Laitinen, R. S.

    Bed material coatings and the consequent agglomeration of bed material are main ash-related problems in FB-boilers. The bed agglomeration is a particular problem when combusting biofuels and waste materials. Whereas SEM-EDS together with automated image processing has proven to be a convenient method to study compositional distribution in coating layers and agglomerates, it is a relatively expensive technique and is not necessarily widely available. In this contribution, we explore the suitability of LA-ICP-MS to provide analogous information of the bed.

  7. Experiences in the ICP-MS analysis of geological and environmental samples

    International Nuclear Information System (INIS)

    Kallio, E.

    1994-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) has been used at the Geological Survey of Finland since 1991. Applied to determination of trace and ultra trace elements in water, sediments, biological samples and rocks. The strength of the technique lies in the ability to determine isotope ratios, and elements that are difficult or expensive to determine by other techniques, e.g. platinum group elements (PGEs), rare earths elements (REEs) and toxic metals (As, Be, Cd, Hg, Pb, Tl, U). An important part of the analysis is the pretreatment of the samples before the measurement. This paper gives an overview of the methods used at the Geological Survey. (orig.). (5 refs.)

  8. Development of on-line electrochemical sample pretreatment methods for the analysis of thallium and uranium by ICP-MS

    International Nuclear Information System (INIS)

    Zhou, F.; Van Berkel, G.J.; Morton, S.J.; Duckworth, D.C.; Adeniyi, W.K.; Keller, J.M.

    1995-01-01

    Anodic and adsorptive stripping voltammetry (AWV and AdSV, respectively) were performed on-line with a mercury thin-film electrode (MTFE) to effect the selective accumulation and detection of thallium and uranium, respectively. ASV-ICP-MS experiments using thallium as the test element were performed to characterize the behavior of the on-line system for low level and quantitative determinations. Excellent linearity in response was demonstrated for thallium standards ranging from 0.25 ng/L to 50 microg/L. The 1.0 pg/L detection limit calculated from this data for thallium (3σ/sensitivity) was 400 times lower than that of conventional ICP-MS. The ability to overcome sample matrix effects in quantitative determinations was demonstrated by the analysis of an undiluted synthetic urine sample. AdSV-ICP-MS experiments were performed using uranium as the test element to demonstrate the utility of this method for the determination of radiologically important elements. A uranium(VI)-cupferron complex was used to effect adsorptive accumulation of uranium from a 10 microg/L standard solution onto the MTFE. The uranium was chemically stripped from the electrode for subsequent downstream detection by the ICP-MS. The quantitative nature of this method and a modest enhancement of signal levels (∼X10) over those levels obtained with conventional ICP-MS for samples in the microgram/liter concentration range were demonstrated. Modifications to the current system to provide low flow rate operation will allow further optimization of the ASV-ICP-MS and AdSV-ICP-MS combinations

  9. Study of Long-Lived Radionuclides in Environmental Samples by ICP-MS; Estudio de Radionucleidos de Vida Larga en Muestras Medioambientales por ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Conde, E.; Navarro, N.; Fernández, M.

    2015-07-01

    Thorium is considered as one of the highly radiotoxic elements, because following its decay a number of other α, β and/or γ emitting daughters are produced. Uranium mining and processing, as well as remediation of impacted soils, are one of the principal anthropogenic sources of thorium release to the air, soil and water. Measurement of Th isotopes requires the use of analytical techniques capable of reliably measure the content of Th isotopes at trace levels. 230Th determination has generally been performed by α-spectrometry. However, this method needs sample preparation of 3-4 days and counting times from days to up to two weeks. A way to face this difficulty is the use of inductively coupled plasma mass spectrometry (ICP-MS). This technique is adequate for the determination of 232Th and 238U, long-lived radionuclides, and it can be applied, successfully, in the determination of 230Th, particularly if it is associated with a pre-concentration stage. This work presents the development of a rapid and simple analytical procedure based on mass spectrometry for the determination of 230Th and the results obtained in the analysis of environmental filters.

  10. Evaluation of the inorganic selenium biotransformation in selenium-enriched yogurt by HPLC-ICP-MS.

    Science.gov (United States)

    Alzate, Adriana; Cañas, Benito; Pérez-Munguía, Sandra; Hernández-Mendoza, Hector; Pérez-Conde, Concepción; Gutiérrez, Ana Maria; Cámara, Carmen

    2007-11-28

    Selenium is an essential element in the human diet. Interestingly, there has been an increased consumption of dietary supplements containing this element in the form of either inorganic or organic compounds. The effect of using selenium as a dietary supplement in yogurt has been evaluated. For this purpose, different concentrations of inorganic Se (ranging from 0.2 to 5000 microg g(-1)) have been added to milk before the fermentation process. Biotransformation of inorganic Se into organic species has been carefully evaluated by ion-exchange, reversed-phase, or size-exclusion chromatography, coupled to inductively coupled plasma mass spectrometry (ICP-MS). Yogurt fermentation in the presence of up to 2 microg g(-1) of Se(IV) produces a complete incorporation of this element into proteins as has been demonstrated applying a dialysis procedure. Analysis by SEC-ICP-MS showed that most of them have a molecular mass in the range of 30-70 kDa. Species determination after enzymatic hydrolysis has allowed the identification of Se-cystine using two different chromatographic systems. The biotransformation process that takes place during yogurt fermentation is very attractive because yogurt can act as a source of selenium supplementation.

  11. Isotope ratio measurements of uranium by LA-HR-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Marin, Rafael C.; Sarkis, Jorge E.S., E-mail: rafael.marin@usp.b, E-mail: jesarkis@ipen.b [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-07-01

    This work describes the utilization of Laser Ablation High Resolution Inductively Mass Spectrometry (LA-HR-ICP-MS) technique for the determination of uranium isotope composition in a UO{sub 2} pellet (CRM -125A) supplied and certified by the New Brunswick Laboratory (NBL). To carry out the adjustments of the parameters was used a glass standard NIST 610, supplied and certified by National Institute of Standards and Technology (NIST). The precision of the measurements were improved by adjusting the following parameters: RF power, laser beam diameter, defocusing of laser beam, laser energy, laser energy-density, auxiliary gas and sample gas. The measurements were performed on a continuous ablation with low energy density and defocusing, which demonstrated to be the optimum to reach the best signal stability. Isotope ratios, {sup 234}U/{sup 238}U, {sup 235}U/{sup 238}U and {sup 236}U/{sup 238}U were measured, reaching relative standard deviations (RSD) from 1.55% to 7.60%. The parameters which caused the greatest impact in order to improve the signal stability were RF power, defocusing and laser beam diameter. The results presented by the measurements revealed that the Laser ablation ICP-MS technique offers a rapid and accurate way to perform uranium isotope ratios without any sample preparation, since it allows carrying out the measurements straight on the sample, besides to preserve the testimony that is very important for safeguards and nuclear forensics purposes. (author)

  12. [Determination of 27 elements in Maca nationality's medicine by microwave digestion ICP-MS].

    Science.gov (United States)

    Yu, Gui-fang; Zhong, Hai-jie; Hu, Jun-hua; Wang, Jing; Huang, Wen-zhe; Wang, Zhen-zhong; Xiao, Wei

    2015-12-01

    An analysis method has been established to test 27 elements (Li, Be, B, Mg, Al, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Sr, Mo, Cd, Sn, Sb, Ba, La, Hg, Pb, Bi) in Maca nationality's medicine with microwave digestion-ICP-MS. Sample solutions were analyzed by ICP-MS after microwave digestion, and the contents of elements were calculated according to their calibration curves, and internal standard method was adopted to reduce matrix effect and other interference effects. The experimental results showed that the linear relations of all the elements were very good; the correlation coefficient (r) was 0.9994-1.0000 (Hg was 0.9982) ; the limits of detection were 0.003-2.662 microg x L(-1); the relative standard deviations for all elements of reproducibility were lower than 5% (except the individual elements); the recovery rate were 78.5%-123.7% with RSD lower than 5% ( except the individual elements). The analytical results of standard material showed acceptable agreement with the certified values. This method was applicable to determinate the contents of multi-elements in Maca which had a high sensitivity, good specificity and good repeatability, and provide basis for the quality control of Maca.

  13. ICP-MS: suitable method to study the metals distribution in estuarine regions

    International Nuclear Information System (INIS)

    Vasconcelos, Danilo C.; Oliveira, Arno H.; Santos, Silvio J. dos; Brito, Veronica F.O.; Severo, Maria Isabel G.

    2005-01-01

    Anthropogenic inputs of pollutants such as heavy metals into the marine environment have increased their levels to large extents within past a few decades. These pollutants tend to accumulate in the bottom sediments. As a result, ecosystems such as seaports or other industrialized coastal areas that have chronic inputs of metals have highly contaminated sediments. This characteristic has led to concerns over the ecological effects that may be associated with sediment quality. Of particular concern are toxic effects and the potential for bioaccumulation of metals in biota exposed to the sediments. The bivalves Crassostrea rhizophorae, Lucina pectinata and Mytella falcata have been used as biomonitors of trace metal contamination in two estuaries from Ilheus city, Bahia state, in Brazil. Bivalves, sediment and water samples were collected in March 2004 in Acuipe and Rio do Engenho mangroves. The proposed technique to analyze the studied matrices was the inductively coupled plasma mass spectrometry (ICP-MS). The results suggested that the studied molluscs are bioaccumulators of metals and showed the Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) as an adequate technique to determine a large range of inorganic elements, because its high sensibility and low detection limits. (author)

  14. Lead isotope ratio analysis of bullet samples by using quadrupole ICP-MS

    International Nuclear Information System (INIS)

    Tamura, Shu-ichi; Hokura, Akiko; Nakai, Izumi; Oishi, Masahiro

    2006-01-01

    The measurement conditions for the precise analysis of the lead stable isotope ratio by using an ICP-MS equipped with a quadrupole mass spectrometer were studied in order to apply the technique to the forensic identification of bullet samples. The values of the relative standard deviation obtained for the ratio of 208 Pb/ 206 Pb, 207 Pb/ 206 Pb and 204 Pb/ 206 Pb were lower than 0.2% after optimization of the analytical conditions, including the optimum lead concentration of the sample solution to be about 70 ppb and an integration time for 1 m/s of 15 s. This method was applied to an analysis of lead in bullets for rifles and handguns; a stable isotope ratio of lead was found to be suitable for the identification of bullets. This study has demonstrated that the lead isotope ratio measured by using a quadrupole ICP-MS was useful for a practical analysis of bullet samples in forensic science. (author)

  15. Heavy metal elements in toiletries analyzed by INAA, ICP-MS and SEM-EDX

    International Nuclear Information System (INIS)

    Furuta, E.; Tagami, K.; Okada, Y.; Nakahara, H.

    2011-01-01

    Recently, many toiletries claiming inclusion of platinum (Pt), silver (Ag) and gold (Au) as additives are sold in ordinary cosmetics shops. However, their concentrations are not clearly indicated. In the present work, these toiletries were analyzed for heavy metal elements by instrumental neutron activation analysis (INAA) and inductively coupled plasma mass spectrometry (ICP-MS), and the particle sizes were observed by scanning electron microscope (SEM) and the constitutions of the small particles were analyzed by energy dispersive X-ray spectroscopy (EDX). The concentrations of Pt in the toiletries observed were from 1 to 80 ppm. The lower detection limit of Pt by INAA was about 1 ppm because of the presence of sodium in high concentrations for those samples. Consequently, some toiletries which should have had Pt according to the manufactures were found not to contain Pt probably because it was less than the detection limit. On the other hand, there were a few toiletries that were found to contain Ag although the addition of Ag was not mentioned by the manufactures. It is considered that these non-indicated Ag were included as impurities of the added Au. The concentrations of the non-indicated Ag were even higher than those of the indicated Ag. A very small amount of Sr, which was nominated in the negative list of Japan, was also detected in 2 out of 5 kinds of toiletries analyzed by ICP-MS. (orig.)

  16. Determination of 99Tc in fresh water using TRU resin by ICP-MS.

    Science.gov (United States)

    Guérin, Nicolas; Riopel, Remi; Kramer-Tremblay, Sheila; de Silva, Nimal; Cornett, Jack; Dai, Xiongxin

    2017-10-02

    Technetium-99 ( 99 Tc) determination at trace level by inductively coupled plasma mass spectrometry (ICP-MS) is challenging because there is no readily available appropriate Tc isotopic tracer. A new method using Re as a recovery tracer to determine 99 Tc in fresh water samples, which does not require any evaporation step, was developed. Tc(VII) and Re(VII) were pre-concentrated on a small anion exchange resin (AER) cartridge from one litre of water sample. They were then efficiently eluted from the AER using a potassium permanganate (KMnO 4 ) solution. After the reduction of KMnO 4 in 2 M sulfuric acid solution, the sample was passed through a small TRU resin cartridge. Tc(VII) and Re(VII) retained on the TRU resin were eluted using near boiling water, which can be directly used for the ICP-MS measurement. The results for method optimisation, validation and application were reported. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

  17. In Situ Carbon Isotope Analysis by Laser Ablation MC-ICP-MS.

    Science.gov (United States)

    Chen, Wei; Lu, Jue; Jiang, Shao-Yong; Zhao, Kui-Dong; Duan, Deng-Fei

    2017-12-19

    Carbon isotopes have been widely used in tracing a wide variety of geological and environmental processes. The carbon isotope composition of bulk rocks and minerals was conventionally analyzed by isotope ratio mass spectrometry (IRMS), and, more recently, secondary ionization mass spectrometry (SIMS) has been widely used to determine carbon isotope composition of carbon-bearing solid materials with good spatial resolution. Here, we present a new method that couples a RESOlution S155 193 nm laser ablation system with a Nu Plasma II MC-ICP-MS, with the aim of measuring carbon isotopes in situ in carbonate minerals (i.e., calcite and aragonite). Under routine operating conditions for δ 13 C analysis, instrumental bias generally drifts by 0.8‰-2.0‰ in a typical analytical session of 2-3 h. Using a magmatic calcite as the standard, the carbon isotopic composition was determined for a suite of calcite samples with δ 13 C values in the range of -6.94‰ to 1.48‰. The obtained δ 13 C data are comparable to IRMS values. The combined standard uncertainty for magmatic calcite is ICP-MS can serve as an appropriate method to analyze carbon isotopes of carbonate minerals in situ.

  18. Potential Health Benefits and Metabolomics of Camel Milk by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Raish, Mohammad; Ahmad, Ajaz; Shakeel, Faiyaz

    2017-02-01

    None of the research reports reveals the metabolomics and elemental studies on camel milk. Recent studies showed that camel milk possesses anticancer and anti-inflammatory activity. Metabolomics and elemental studies were carried out in camel milk which showed us the pathways and composition that are responsible for the key biological role of camel milk. Camel milk was dissolved in methanol and chloroform fraction and then vortexed and centrifuged. Both the fractions were derivatized by N,O-bis-(trimethylsilyl)trifluoroacetamide (BSTFA) and TMCS after nitrogen purging and analyzed by GC-MS. Camel milk was also analyzed by ICP-MS after microwave digestion. We found that higher alkanes and fatty acids are present in the chloroform fraction and amino acids, sugars and fatty acid derivatives are present in aqueous fractions. All the heavy metals like As, Pb, Cd, Co, Cu, and Ni were in the safe limits in terms of maximum daily intake of these elements. Na, K, Mg, and Ca were also present in the safe limits in terms of maximum daily intake of these elements. These results suggested that the camel milk drinking is safe and there is no health hazard. The present data of GC-MS and ICP-MS correlate the activities related to camel milk.

  19. Online preconcentration ICP-MS analysis of rare earth elements in seawater

    Science.gov (United States)

    Hathorne, Ed C.; Haley, Brian; Stichel, Torben; Grasse, Patricia; Zieringer, Moritz; Frank, Martin

    2012-01-01

    The rare earth elements (REEs) with their systematically varying properties are powerful tracers of continental inputs, particle scavenging intensity and the oxidation state of seawater. However, their generally low (˜pmol/kg) concentrations in seawater and fractionation potential during chemical treatment makes them difficult to measure. Here we report a technique using an automated preconcentration system, which efficiently separates seawater matrix elements and elutes the preconcentrated sample directly into the spray chamber of an ICP-MS instrument. The commercially available "seaFAST" system (Elemental Scientific Inc.) makes use of a resin with ethylenediaminetriacetic acid and iminodiacetic acid functional groups to preconcentrate REEs and other metals while anions and alkali and alkaline earth cations are washed out. Repeated measurements of seawater from 2000 m water depth in the Southern Ocean allows the external precision (2σ) of the technique to be estimated at mine water reference materials diluted with a NaCl matrix with recommended values in the literature. This makes the online preconcentration ICP-MS technique advantageous for the minimal sample preparation required and the relatively small sample volume consumed (7 mL) thus enabling large data sets for the REEs in seawater to be rapidly acquired.

  20. Reduction of Solvent Effect in Reverse Phase Gradient Elution LC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Sullivan, Patrick Allen [Iowa State Univ., Ames, IA (United States)

    2005-12-17

    Quantification in liquid chromatography (LC) is becoming very important as more researchers are using LC, not as an analytical tool itself, but as a sample introduction system for other analytical instruments. The ability of LC instrumentation to quickly separate a wide variety of compounds makes it ideal for analysis of complex mixtures. For elemental speciation, LC is joined with inductively coupled plasma mass spectrometry (ICP-MS) to separate and detect metal-containing, organic compounds in complex mixtures, such as biological samples. Often, the solvent gradients required to perform complex separations will cause matrix effects within the plasma. This limits the sensitivity of the ICP-MS and the quantification methods available for use in such analyses. Traditionally, isotope dilution has been the method of choice for LC-ICP-MS quantification. The use of naturally abundant isotopes of a single element in quantification corrects for most of the effects that LC solvent gradients produce within the plasma. However, not all elements of interest in speciation studies have multiple naturally occurring isotopes; and polyatomic interferences for a given isotope can develop within the plasma, depending on the solvent matrix. This is the case for reverse phase LC separations, where increasing amounts of organic solvent are required. For such separations, an alternative to isotope dilution for quantification would be is needed. To this end, a new method was developed using the Apex-Q desolvation system (ESI, Omaha, NE) to couple LC instrumentation with an ICP-MS device. The desolvation power of the system allowed greater concentrations of methanol to be introduced to the plasma prior to destabilization than with direct methanol injection into the plasma. Studies were performed, using simulated and actual linear methanol gradients, to find analyte-internal standard (AIS) pairs whose ratio remains consistent (deviations {+-} 10%) over methanol concentration ranges of 5

  1. Direct determination of halogens in powdered geological and environmental samples using isotope dilution laser ablation ICP-MS

    Science.gov (United States)

    Boulyga, Sergei F.; Heumann, Klaus G.

    2005-04-01

    Laser ablation inductively coupled plasma isotope dilution mass spectrometry (LA-ICP-IDMS) with a special laser ablation system for bulk analyses (LINA-Spark(TM)-Atomiser) was applied for direct determinations of chlorine, bromine, and iodine in rock and sediment samples. Special attention was focused on possible inter-halogen fractionations and analyte/spike isotope fractionations by using LA-ICP-MS and LA-ICP-IDMS, respectively. A variation of Br/Cl and I/Cl element intensity ratios by a factor of 1.3-3 was observed when changing the nebulizer gas flow rate in the range of 0.84-1.0 L min-1 and the laser power density in the range of 2-10 GW cm-2, respectively. When using an internal standard for halogen quantification in LA-ICP-MS, this inter-element fractionation can cause systematic errors, which can be avoided by applying the isotope dilution technique. However, at high laser power densities (>5.7 GW cm-2 for iodine and >4.0 GW cm-2 for bromine and chlorine) the corresponding measured isotope ratio of the isotope-diluted sample deviates significantly from the target value. Under optimised conditions concentrations in the range of 30 [mu]g g-1-16 × 103 [mu]g g-1 for chlorine, <2-140 [mu]g g-1 for bromine, and <0.1-31 [mu]g g-1 for iodine were determined by LA-ICP-IDMS in two sediment reference materials (SRM 1646, SRM 2704) and three rock reference samples (GS-N, Granite; BX-N, Bauxite; DT-N, Disthene), which have not been certified for these halogens. The sediment results agree well within the given uncertainties with indicative values by different methods and the results of the rock samples with those obtained by negative thermal ionisation isotope dilution mass spectrometry. The detection limits of LA-ICP-IDMS are 8 [mu]g g-1 for chlorine, 1.7 [mu]g g-1 for bromine, and 0.1 [mu]g g-1 for iodine.

  2. Measurement of very low amounts of arsenic in soils and waters: is ICP-MS the indispensable analytical tool?

    Science.gov (United States)

    López-García, Ignacio; Marín-Hernández, Juan Jose; Perez-Sirvent, Carmen; Hernandez-Cordoba, Manuel

    2017-04-01

    The toxicity of arsenic and its wide distribution in the nature needs nowadays not to be emphasized, and the convenience of reliable analytical tools for arsenic determination at very low levels is clear. Leaving aside atomic fluorescence spectrometers specifically designed for this purpose, the task is currently carried out by using inductively coupled plasma mass spectrometry (ICP-MS), a powerful but expensive technique that is not available in all laboratories. However, as the recent literature clearly shows, a similar or even better analytical performance for the determination of several elements can be achieved by replacing the ICP-MS instrument by an AAS spectrometer (which is commonly present in any laboratory and involves low acquisition and maintenance costs) provided that a simple microextraction step is used to preconcentrate the sample. This communication reports the optimization and results obtained with a new analytical procedure based on this idea and focused to the determination of very low concentrations of arsenic in waters and extracts from soils and sediments. The procedure is based on a micro-solid phase extraction process for the separation and preconcentration of arsenic that uses magnetic particles covered with silver nanoparticles functionalized with the sodium salt of 2-mercaptoethane-sulphonate (MESNa). This composite is obtained in an easy way in the laboratory. After the sample is treated with a low amount (only a few milligrams) of the magnetic material, the solid phase is separated by means of a magnetic field, and then introduced into an electrothermal atomizer (ETAAS) for arsenic determination. The preconcentration factor is close to 200 with a detection limit below 0.1 µg L-1 arsenic. Speciation of As(III) and As(V) can be achieved by means of two extractions carried out at different acidity. The results for total arsenic are verified using certified reference materials. The authors are grateful to the Comunidad Autonóma de la

  3. Concerns about Quadrupole ICP-MS Lead Isotopic Data and Interpretations in the Environment and Health Fields

    Directory of Open Access Journals (Sweden)

    Brian Gulson

    2018-04-01

    Full Text Available There has been a massive increase in recent years of the use of lead (Pb isotopes in attempts to better understand sources and pathways of Pb in the environment and in man or experimental animals. Unfortunately, there have been many cases where the quality of the isotopic data, especially that obtained by quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS, are questionable, resulting in questionable identification of potential sources, which, in turn, impacts study interpretation and conclusions. We present several cases where the isotopic data have compromised interpretation because of the use of only the major isotopes 208Pb/206Pb and 207Pb/206Pb, or their graphing in other combinations. We also present some examples comparing high precision data from thermal ionization (TIMS or multi-collector plasma mass spectrometry (MC-ICP-MS to illustrate the deficiency in the Q-ICP-MS data. In addition, we present cases where Pb isotopic ratios measured on Q-ICP-MS are virtually impossible for terrestrial samples. We also evaluate the Pb isotopic data for rat studies, which had concluded that Pb isotopic fractionation occurs between different organs and suggest that this notion of biological fractionation of Pb as an explanation for isotopic differences is not valid. Overall, the brief review of these case studies shows that Q-ICP-MS as commonly practiced is not a suitable technique for precise and accurate Pb isotopic analysis in the environment and health fields.

  4. Detection and characterisation of aluminium-containing nanoparticles in Chinese noodles by single particle ICP-MS.

    Science.gov (United States)

    Loeschner, Katrin; Correia, Manuel; López Chaves, Carlos; Rokkjær, Inge; Sloth, Jens J

    2018-01-01

    This study investigated Chinese noodles for the presence of aluminium-containing nanoparticles by using inductively coupled plasma mass spectrometry in single particle mode (spICP-MS) after enzymatic digestion by α-amylase. The aluminium concentrations in the noodle samples, determined by conventional ICP-MS without or with the use of hydrofluoric acid for digestion, were 5.4 ± 1.9 µg/g and 10.1 ± 2.2 µg/g (N = 21), respectively. Aluminium-containing nanoparticles were detected by spICP-MS in all 21 samples. Depending on the assumed particle composition, Al 2 O 3 or Al 2 O 3 ∙2SiO 2 ∙2H 2 O, the median particle diameters were either below or above 100 nm, respectively. The minimum detectable particle diameter by spICP-MS was between 54 and 83 nm. The mass recovery of aluminium in the form of particles was between 5% and 18%. The presented work reports for the first time the detection of Al-containing particles in food by spICP-MS.

  5. Concerns about Quadrupole ICP-MS Lead Isotopic Data and Interpretations in the Environment and Health Fields.

    Science.gov (United States)

    Gulson, Brian; Kamenov, George D; Manton, William; Rabinowitz, Michael

    2018-04-11

    There has been a massive increase in recent years of the use of lead (Pb) isotopes in attempts to better understand sources and pathways of Pb in the environment and in man or experimental animals. Unfortunately, there have been many cases where the quality of the isotopic data, especially that obtained by quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS), are questionable, resulting in questionable identification of potential sources, which, in turn, impacts study interpretation and conclusions. We present several cases where the isotopic data have compromised interpretation because of the use of only the major isotopes 208 Pb/ 206 Pb and 207 Pb/ 206 Pb, or their graphing in other combinations. We also present some examples comparing high precision data from thermal ionization (TIMS) or multi-collector plasma mass spectrometry (MC-ICP-MS) to illustrate the deficiency in the Q-ICP-MS data. In addition, we present cases where Pb isotopic ratios measured on Q-ICP-MS are virtually impossible for terrestrial samples. We also evaluate the Pb isotopic data for rat studies, which had concluded that Pb isotopic fractionation occurs between different organs and suggest that this notion of biological fractionation of Pb as an explanation for isotopic differences is not valid. Overall, the brief review of these case studies shows that Q-ICP-MS as commonly practiced is not a suitable technique for precise and accurate Pb isotopic analysis in the environment and health fields.

  6. Determination of trace Np and Pu by ICP-MS with extraction chromatography in emergency situations

    International Nuclear Information System (INIS)

    Yanqin, Ji; Qing, Tian; Baoming, Shen; Xianzhang, Shao

    2008-01-01

    Full text: An accurate determination of radioculides from various sources in the environmental samples is essential for assessment of the potential hazards and suitable countermeasures both in case of accidents, authorised release and routine surveillance. However, the concentrationof neptunium and plutonium is extremely low in environmental samples, and such samples have a complex matrix composition, which is to be taken into account for a proper analysis. Conventional radiochemical methods such as alpha spectrometry, neutron activation analysis, liquid, liquid scintillation system, fission track and gamma spectrometry for the quantitative determination of neptunium and plutonium often require complicated and time-consuming sample preparation and separation procedures. Due to the large amount of the complex and often unknown matrix, the analysis may also be covered by naturally occurring radionuclides. With the development of new analysis techniques, non-radioactive methods are increasingly used for the determination of trace or ultra-trace radionuclides in environmental samples. Inductively coupled plasma mass spectrometry (ICP-MS) is one of the most suitable analysis techniques for the measurement of the long-lived radionuclides with its high sensitivity, low detection limits, short analysis time, less chemical interferences and multi-elemental capability. The throughput is therefore very high (approx.100 samples a day). The main objective of the present study was to set up of a simple, fast separation procedure to measure Np and Pu in the environmental samples ICP-MS. An unique extraction chromatographic column (TOA: tri-n-octylamine on Teflon powder) with a two-stage sample loading was prepared to separate Np and Pu from the environmental matrix. Np and Pu were efficiently retained in 4 M HNO 3 medium on the column and easiy eluted with 0.02 M oxalic acid 0.16 M HNO 3 at 95 C degree. The separated solutions were free from most of the matrix elements and were

  7. External calibration strategy for trace element quantification in botanical samples by LA-ICP-MS using filter paper

    International Nuclear Information System (INIS)

    Nunes, Matheus A.G.; Voss, Mônica; Corazza, Gabriela; Flores, Erico M.M.; Dressler, Valderi L.

    2016-01-01

    The use of reference solutions dispersed on filter paper discs is proposed for the first time as an external calibration strategy for matrix matching and determination of As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sr, V and Zn in plants by laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS). The procedure is based on the use of filter paper discs as support for aqueous reference solutions, which are further evaporated, resulting in solid standards with concentrations up to 250 μg g −1 of each element. The use of filter paper for calibration is proposed as matrix matched standards due to the similarities of this material with botanical samples, regarding to carbon concentration and its distribution through both matrices. These characteristics allowed the use of 13 C as internal standard (IS) during the analysis by LA-ICP-MS. In this way, parameters as analyte signal normalization with 13 C, carrier gas flow rate, laser energy, spot size, and calibration range were monitored. The calibration procedure using solution deposition on filter paper discs resulted in precision improvement when 13 C was used as IS. The method precision was calculated by the analysis of a certified reference material (CRM) of botanical matrix, considering the RSD obtained for 5 line scans and was lower than 20%. Accuracy of LA-ICP-MS determinations were evaluated by analysis of four CRM pellets of botanical composition, as well as by comparison with results obtained by ICP-MS using solution nebulization after microwave assisted digestion. Plant samples of unknown elemental composition were analyzed by the proposed LA method and good agreement were obtained with results of solution analysis. Limits of detection (LOD) established for LA-ICP-MS were obtained by the ablation of 10 lines on the filter paper disc containing 40 μL of 5% HNO 3 (v v −1 ) as calibration blank. Values ranged from 0.05 to 0.81  μg g −1 . Overall, the use of filter paper as support for dried

  8. Determination of 241Pu in nuclear waste slurries: a comparative study using LSC and ICP-MS.

    Science.gov (United States)

    Jäggi, M; Röllin, S; Alvarado, J A Corcho; Eikenberg, J

    2012-02-01

    (241)Pu was determined in slurry samples from a nuclear reactor decommissioning project at the Paul Scherrer Institute (Switzerland). To validate the results, the (241)Pu activities of five samples were determined by LSC (TriCarb and Quantulus) and ICP-MS, with each instrument at a different laboratory. In lack of certified reference materials for (241)Pu, the methods were further validated using the (241)Pu information values of two reference sediments (IAEA-300 and IAEA-384). Excellent agreement with the results was found between LSC and ICP-MS in the nuclear waste slurries and the reference sediments. Copyright © 2011 Elsevier Ltd. All rights reserved.

  9. Impact of and correction for instrument sensitivity drift on nanoparticle size measurements by single-particle ICP-MS

    Science.gov (United States)

    El Hadri, Hind; Petersen, Elijah J.; Winchester, Michael R.

    2016-01-01

    The effect of ICP-MS instrument sensitivity drift on the accuracy of NP size measurements using single particle (sp)ICP-MS is investigated. Theoretical modeling and experimental measurements of the impact of instrument sensitivity drift are in agreement and indicate that drift can impact the measured size of spherical NPs by up to 25 %. Given this substantial bias in the measured size, a method was developed using an internal standard to correct for the impact of drift and was shown to accurately correct for a decrease in instrument sensitivity of up to 50 % for 30 nm and 60 nm gold nanoparticles. PMID:26894759

  10. Separation of selenium compounds by CE-ICP-MS in dynamically coated capillaries applied to selenized yeast samples

    DEFF Research Database (Denmark)

    Bendahl, Lars; Gammelgaard, Bente

    2004-01-01

    The selenium species in nutritional supplement tablets, based on selenized yeast, were separated by capillary zone electrophoresis using capillaries coated dynamically with poly(vinyl sulfonate) and detected by ICP-MS. Sample pre-treatment consisted of cold-water extraction by sonication and subs......The selenium species in nutritional supplement tablets, based on selenized yeast, were separated by capillary zone electrophoresis using capillaries coated dynamically with poly(vinyl sulfonate) and detected by ICP-MS. Sample pre-treatment consisted of cold-water extraction by sonication...

  11. External calibration strategy for trace element quantification in botanical samples by LA-ICP-MS using filter paper

    Energy Technology Data Exchange (ETDEWEB)

    Nunes, Matheus A.G.; Voss, Mônica; Corazza, Gabriela; Flores, Erico M.M.; Dressler, Valderi L., E-mail: vdressler@gmail.com

    2016-01-28

    The use of reference solutions dispersed on filter paper discs is proposed for the first time as an external calibration strategy for matrix matching and determination of As, Cd, Co, Cr, Cu, Mn, Ni, Pb, Sr, V and Zn in plants by laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS). The procedure is based on the use of filter paper discs as support for aqueous reference solutions, which are further evaporated, resulting in solid standards with concentrations up to 250 μg g{sup −1} of each element. The use of filter paper for calibration is proposed as matrix matched standards due to the similarities of this material with botanical samples, regarding to carbon concentration and its distribution through both matrices. These characteristics allowed the use of {sup 13}C as internal standard (IS) during the analysis by LA-ICP-MS. In this way, parameters as analyte signal normalization with {sup 13}C, carrier gas flow rate, laser energy, spot size, and calibration range were monitored. The calibration procedure using solution deposition on filter paper discs resulted in precision improvement when {sup 13}C was used as IS. The method precision was calculated by the analysis of a certified reference material (CRM) of botanical matrix, considering the RSD obtained for 5 line scans and was lower than 20%. Accuracy of LA-ICP-MS determinations were evaluated by analysis of four CRM pellets of botanical composition, as well as by comparison with results obtained by ICP-MS using solution nebulization after microwave assisted digestion. Plant samples of unknown elemental composition were analyzed by the proposed LA method and good agreement were obtained with results of solution analysis. Limits of detection (LOD) established for LA-ICP-MS were obtained by the ablation of 10 lines on the filter paper disc containing 40 μL of 5% HNO{sub 3} (v v{sup −1}) as calibration blank. Values ranged from 0.05 to 0.81  μg g{sup −1}. Overall, the use of filter

  12. Determination of {sup 126}Sn half-life from ICP-MS and gamma spectrometry measurements

    Energy Technology Data Exchange (ETDEWEB)

    Bienvenu, P.; Arnal, N.; Comte, J. [CEA Cadarache DEN/DEC/SA3C/LARC, Paul Lez Durance (France); Ferreux, L.; Lepy, M.C.; Be, M.M. [CEA Saclay LIST LNE/LNHB, Gif sur Yvette (France); Andreoletti, G. [AREVA Cogema SL/UP2-800, Beaumont Hague (France)

    2009-07-01

    A new value of {sup 126}Sn half-life was determined by combination of inductively coupled plasma-mass spectrometry (ICP-MS) and gamma spectrometry measurements on purified sample solutions collected from nuclear fuel reprocessing. {sup 126}Sn was isolated through dissolution of fission product precipitates and liquid-liquid extraction with N-benzoyl-N-phenyl-hydroxylamine (BPHA). The abundance of {sup 126}Sn atoms together with the absence of interfering species in the analysed solutions made it possible to measure both mass concentration and nuclide activity with high precision and accuracy. This led to a {sup 126}Sn half-life value of 1.980 (57) x 10{sup 5} a. (orig.)

  13. PIXE and ICP-MS Analysis of Andrographis Paniculata Medicinal Plant

    Science.gov (United States)

    Chandrasekhar Rao, J.; Naidu, B. G.; Sarita, P.; Srikanth, S.; Naga Raju, G. J.

    2017-08-01

    The concentrations of elements Li, Be, Al, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Ag, Cd, Ba, Pb and U in Andrographis Paniculata medicinal plant used in the treatment of Diabetes Mellitus were determined by using Particle Induced X-ray Emission (PIXE) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) techniques. This plant was collected from four different geographical locations in Andhra Pradesh, India in order to assess the regional variation of elemental concentrations. Appreciable levels of K, Ca, Cr, Mn, Cu and Zn determined in this plant can be correlated to the antidiabetic property of Andrographis Paniculata since these elements are known to regulate and potentiate insulin action. Presence of toxic elements As, Cd and Pb necessitates the adoption of precautionary measures while prescribing dosage of the herbal medicine prepared from this plant for the treatment diabetes mellitus.

  14. Elemental speciation in biomolecules by LC-ICP-MS with magnetic sector and collision cell instruments

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jin [Iowa State Univ., Ames, IA (United States)

    1999-11-08

    A methodology that can monitor and identify inorganic elements in biological and environmental systems was developed. Size exclusion chromatography (SEC) separates biomolecules, which are then nebulized by a microconcentric nebulizer. The resulting aerosol is desolved and introduced into either a high resolution ICP-MS device or a quadrupole device with a collision cell. Because of the high sensitivity and spectral resolution and high sample introduction efficiency, many unusual or difficult elements, such as Cr, Se, Cd and U, can be observed at ambient levels bound to proteins in human serum. These measurements are made in only a few minutes without preliminary isolation and preconcentration steps. Serum samples can be titrated with spikes of various elements to determine which proteins bind a given metal and oxidation state. Experiments concerning the effects of breaking disulfide linkages and denaturation on metal binding in proteins were also investigated. Elemental distribution in liver extract was also obtained.

  15. Elemental imaging of MRI contrast agents: benchmarking of LA-ICP-MS to MRI

    Energy Technology Data Exchange (ETDEWEB)

    Pugh, J.A.T. [University of Sheffield, Centre for Analytical Sciences, Sheffield (United Kingdom); University of Sheffield, Department of Chemical and Biological Engineering, Sheffield (United Kingdom); Cox, A.G.; McLeod, C.W. [University of Sheffield, Centre for Analytical Sciences, Sheffield (United Kingdom); Bunch, J. [University of Birmingham, School of Chemistry, Birmingham (United Kingdom); Writer, M.J.; Hart, S.L. [UCL Institute of Child Health, Wolfson Centre for Gene Therapy of Childhood Disease, London (United Kingdom); Bienemann, A.; White, E. [University of Bristol, School of Clinical Sciences, Southmead Hospital, Bristol (United Kingdom); Bell, J. [Hammersmith Hospital, Metabolic and Molecular Imaging Group, MRC Clinical Sciences Centre, Imperial College London, London (United Kingdom)

    2012-06-15

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been used to map the spatial distribution of magnetic resonance imaging (MRI) contrast agents (Gd-based) in histological sections in order to explore synergies with in vivo MRI. Images from respective techniques are presented for two separate studies namely (1) convection enhanced delivery of a Gd nanocomplex (developmental therapeutic) into rat brain and (2) convection enhanced delivery, with co-infusion of Magnevist (commercial Gd contrast agent) and Carboplatin (chemotherapy drug), into pig brain. The LA technique was shown to be a powerful compliment to MRI not only in offering improved sensitivity, spatial resolution and signal quantitation but also in giving added value regarding the fate of administered agents (Gd and Pt agents). Furthermore simultaneous measurement of Fe enabled assignment of an anomalous contrast enhancement region in rat brain to haemorrhage at the infusion site. (orig.)

  16. Elemental speciation in biomolecules by LC-ICP-MS with magnetic sector and collision cell instruments

    International Nuclear Information System (INIS)

    Wang, Jin

    1999-01-01

    A methodology that can monitor and identify inorganic elements in biological and environmental systems was developed. Size exclusion chromatography (SEC) separates biomolecules, which are then nebulized by a microconcentric nebulizer. The resulting aerosol is desolved and introduced into either a high resolution ICP-MS device or a quadrupole device with a collision cell. Because of the high sensitivity and spectral resolution and high sample introduction efficiency, many unusual or difficult elements, such as Cr, Se, Cd and U, can be observed at ambient levels bound to proteins in human serum. These measurements are made in only a few minutes without preliminary isolation and preconcentration steps. Serum samples can be titrated with spikes of various elements to determine which proteins bind a given metal and oxidation state. Experiments concerning the effects of breaking disulfide linkages and denaturation on metal binding in proteins were also investigated. Elemental distribution in liver extract was also obtained

  17. Simultaneous determination of arsenic, selenium and antimony species using HPLC/ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Lindemann, T.; Prange, A.; Neidhart, B. [GKSS-Forschungszentrum Geesthacht GmbH (Germany). Inst. fuer Physikalische und Chemische Analytik; Dannecker, W. [Univ. of Hamburg (Germany). Inst. for Inorganic and Applied Chemistry

    1999-07-01

    A new method for the simultaneous separation and determination of four arsenic species [As(III), As(V), monomethylarsonic acid and dimethylarsinic acid], three selenium species [Se(IV), Se(VI) and selenomethionine] as well as Sb(III) and Sb(V) is presented. The speciation was achieved by on-line coupling of anion exchange high-performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP-MS). Chromatographic parameters such as the composition and pH of the mobile phase were optimised. Limits of detection are below 4.5 {mu}g L{sup -1} (as element) for Sb(III) and the selenium species and below 0.5 {mu}g L{sup -1} for the other species. Precisions of retention times were better than 2% RSD and of peak areas better than 8% RSD for all the species investigated. (orig.) With 5 figs., 3 tabs., 41 refs.

  18. PIXE and ICP-MS analysis of fenugreek medicinal plant from different regions

    International Nuclear Information System (INIS)

    Chandrasekhar Rao, J.; Naidu, B.G.; Sarita, P.; Naga Raju, G.J.

    2017-01-01

    Elemental analysis of Fenugreek medicinal plant collected from different regions was carried out by Proton Induced X-ray Emission (PIXE) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) techniques. The elements Li, Be, Al, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Br, Rb, Sr, Ag, Cd, Ba, Pb and U were identified and their concentrations were estimated. These elements were found to be in widely varying concentrations in the analyzed Fenugreek medicinal plant collected from different regions. of the. The results of the present study provide a better understanding of the pharmacological action of Fenugreek medicinal plant and it can also be used to set new standards for prescribing the dosage of herbal drugs. (author)

  19. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Rosa, Mychelle M.L.; Maihara, Vera A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT. [Comissao Nacional de Energia Nuclear (LAPOC/CNEN-MG), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2015-07-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ({sup 234}U, {sup 235}U and {sup 238}U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  20. Characterisation of spent nuclear fuels by an on-line coupled HPLC-ICP-MS system

    International Nuclear Information System (INIS)

    Guenther-Leopold, I.; Gabler, F.; Wernli, B.; Kopajtic, Z.

    2000-01-01

    The determination of burn-up is one of the essential components of post-irradiation examination of nuclear fuel samples. In the framework of the ARIANE programme (Actinides Research in a Nuclear Element), at PSI the analysis of the isotopic vectors of uranium, plutonium, neodymium and some other fission and spallation products was carried out for the first time in the Hot Lab using high-performance liquid chromatography (HPLC), coupled on-line with an inductively coupled plasma mass spectrometer (ICP-MS). The results of these investigations, a comparison with the classical technique for burn-up determination, the advantages and limitations of the new method, the accuracy and precision of these types of analyses, the applicability of the technique to other samples and separation problems, and conclusions for further analyses of nuclear fuel samples, are here presented. (authors)

  1. Determination of rare earth elements in rice by INAA and ICP-MS

    International Nuclear Information System (INIS)

    Pham Thi Huynh, M.; Chu Pham Ngoc, S.; Carrot, F.; Revel, G.; Dang Vu, M.

    1997-01-01

    Irrigation of rice plants with a solution of rare earth elements increases both the production capacity and the resistance to disease. Assuming that the treated plants remain expendable, the different parts of plants, root stalk and grain, were analyzed by instrumental neutron activation analysis (INAA) and by mass spectrometry after plasma excitation (ICP-MS). About 40 elements were determined. The results showed that the contamination remained in the roots and was absent in rice grains. The analytical distribution of different elements in different parts of both treated and non-treated plants has given some information concerning the possible effect of the rare earth treatment. The performances of the two analytical methods have been compared. (author)

  2. Direct quantification of rare earth element concentrations in natural waters by ICP-MS

    International Nuclear Information System (INIS)

    Lawrence, Michael G.; Greig, Alan; Collerson, Kenneth D.; Kamber, Balz S.

    2006-01-01

    A direct quadrupole ICP-MS technique has been developed for the analysis of the rare earth elements and yttrium in natural waters. The method has been validated by comparison of the results obtained for the river water reference material SLRS-4 with literature values. The detection limit of the technique was investigated by analysis of serial dilutions of SLRS-4 and revealed that single elements can be quantified at single-digit fg/g concentrations. A coherent normalised rare earth pattern was retained at concentrations two orders of magnitude below natural concentrations for SLRS-4, demonstrating the excellent inter-element accuracy and precision of the method. The technique was applied to the analysis of a diluted mid-salinity estuarine sample, which also displayed a coherent normalised rare earth element pattern, yielding the expected distinctive marine characteristics

  3. Uranium isotopes determination in urine samples using alpha spectrometry and ICP-MS

    International Nuclear Information System (INIS)

    Rosa, Mychelle M.L.; Maihara, Vera A.; Tine, Fernanda D.; Santos, Sandra M.C.; Bonifacio, Rodrigo L.; Taddei, Maria HelenaT.

    2015-01-01

    The action of determining the concentration of uranium isotopes in biological samples, 'in vitro' bioassay, is an indirect method for evaluating the incorporation and quantification of these radionuclides internally deposited. When incorporated, these radionuclides tend to be disposed through excretion, with urine being the main source of data because it can be easily collected and analyzed. The most widely used methods for determination of uranium isotopes ( 234 U, 235 U and 238 U) are Alpha Spectrometry and ICP-MS. This work presents a comparative study for the determination of uranium isotopes using these two methodologies in real samples from occupationally exposed workers. In order to validate the methodology, a sample of the intercomparison exercise organized by PROCORAD (Association pour la Promotion du Controle de Qualite des Analyses de Biologie Medicale em Radiotoxicologie) was used, and the results were statistically compared applying the Student's t-test. (author)

  4. Profiling extractable and leachable inorganic impurities in ophthalmic drug containers by ICP-MS.

    Science.gov (United States)

    Solomon, Paige; Nelson, Jenny

    2018-03-01

    In this study, we investigated the elemental impurities present in the plastic material of ophthalmic eye drop bottles using inductively coupled plasma-mass spectrometry (ICP-MS). Metallic contaminations, especially localized within the small cavity of the eye, can significantly perturb the ocular metallome. The concern is two-fold: first certain elements, for example heavy metals, can be toxic to humans at even trace levels, and second, these contaminations can have adverse reactions with other medicines or enzymatic processes in the eye. The implication of redox-active metals in cataract formation is one such biological consequence. The analysis demonstrated the effect of aggressive storage and transportation conditions on elemental extractable and leachable contamination, and posits that release of these elemental impurities can disrupt metallome equilibrium in the ocular compartment, leading to toxicity and disease.

  5. Simultaneous speciation of endogenous and exogenous elements by HPLC/ICP-MS with enriched stable isotopes

    International Nuclear Information System (INIS)

    Suzuki, K.T.

    1996-01-01

    High performance liquid chromatography (HPLC)/inductively coupled argon plasma-mass spectrometry (ICP-MS) was introduced to investigate the distributions of selenium (Se) in biological fluids. The method was to determine both the natural abundance of Se and an enriched stable isotope of Se used as a tracer. The distributions of Se in plasma and in urine specimens were determined in Wistar rats on various Se diets with and without an intravenous injection of 82 Se-selenite. Although the distribution of natural abundance Se (endogenous Se) in the plasma was affected little by the nutritional status of Se, that in the urine gave a Se peak depending on the nutritional status of Se, and the peak was identified as methylselenol. When 82 Se-selenite was injected in excess into rats given three different Se diets (Se-deficient, Se-adequate, Se-excessive), three Se peaks occurred in the HPLC chromatogram of the urine samples, corresponding to selenite, methylselenol and trimethylselenonium ion in the order of elution, and the intensities of the tracer peaks reflected the nutritional status. These results indicate that the HPLC/ICP-MS method is a powerful analytical tool for specifying Se-containing biological constituents, both natural abundance and enriched stable isotopes. Methylselenol in urine is proposed to be a sensitive and Se-specific biological indicator for diagnosing the nutritional status of Se. Furthermore, it was shown that an enriched stable isotope such as 82 Se-selenite was shown to be used for the same purpose, and that 82 Se-methylselenol and 82 Se-trimethylselenonium ion in urine were more sensitive indicators of the Se status of the rats. (author)

  6. ICP-MS with hexapole collision cell for isotope ratio measurements of Ca, Fe, and Se.

    Science.gov (United States)

    Boulyga, S F; Becker, J S

    2001-07-01

    To avoid mass interferences on analyte ions caused by argon ions and argon molecular ions via reactions with collision gases, an rf hexapole filled with helium and hydrogen has been used in inductively coupled plasma mass spectrometry (ICP-MS), and its performance has been studied. Up to tenfold improvement in sensitivity was observed for heavy elements (m > 100 u), because of better ion transmission through the hexapole ion guide. A reduction of argon ions Ar+ and the molecular ions of argon ArX+ (X = O, Ar) by up to three orders of magnitude was achieved in a hexapole collision cell of an ICP-MS ("Platform ICP", Micromass, Manchester, UK) as a result of gas-phase reactions with hydrogen when the hexapole bias (HB) was set to 0 V; at an HB of 1.6 V argon, and argon-based ions of masses 40 u, 56 u, and 80 u, were reduced by approximately four, two, and five orders of magnitude, respectively. The signal-to-noise ratio 80Se/ 40Ar2+ was improved by more than five orders of magnitude under optimized experimental conditions. Dependence of mass discrimination on collision-cell properties was studied in the mass range 10 u (boron) to 238 u (uranium). Isotopic analysis of the elements affected by mass-spectrometric interference, Ca, Fe, and Se, was performed using a Meinhard nebulizer and an ultrasonic nebulizer (USN). The measured isotope ratios were comparable with tabulated values from IUPAC. Precision of 0.26%, 0.19%, and 0.12%, respectively, and accuracy of 0.13% 0.25%, and 0.92%, respectively, was achieved for isotope ratios 44Ca/ 40Ca and 56Fe/57Fe in 10 microg L(-1) solution nebulized by means of a USN and for 78Se/80Se in 100 microg L(-1) solution nebulized by means of a Meinhard nebulizer.

  7. New approach of a transient ICP-MS measurement method for samples with high salinity.

    Science.gov (United States)

    Hein, Christina; Sander, Jonas Michael; Kautenburger, Ralf

    2017-03-01

    In the near future it is necessary to establish a disposal for high level nuclear waste (HLW) in deep and stable geological formations. In Germany typical host rocks are salt or claystone. Suitable clay formations exist in the south and in the north of Germany. The geochemical conditions of these clay formations show a strong difference. In the northern ionic strengths of the pore water up to 5M are observed. The determination of parameters like K d values during sorption experiments of metal ions like uranium or europium as homologues for trivalent actinides onto clay stones are very important for long term safety analysis. The measurement of the low concentrated, not sorbed analytes commonly takes place by inductively coupled plasma mass spectrometry (ICP-MS). A direct measurement of high saline samples like seawater with more than 1% total dissolved salt content is not possible. Alternatives like sample clean up, preconcentration or strong dilution have more disadvantages than advantages for example more preparation steps or additional and expensive components. With a small modification of the ICP-MS sample introduction system and a home-made reprogramming of the autosampler a transient analysing method was developed which is suitable for measuring metal ions like europium and uranium in high saline sample matrices up to 5M (NaCl). Comparisons at low ionic strength between the default and the transient measurement show the latter performs similarly well to the default measurement. Additionally no time consuming sample clean-up or expensive online dilution or matrix removal systems are necessary and the analysation shows a high sensitivity due to the data processing based on the peak area. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Fingerprinting of ground water by ICP-MS. Progress report, January 1, 1995--March 31, 1995

    International Nuclear Information System (INIS)

    Stetzenbach, K.

    1995-01-01

    This report contains the results of the chemical analysis of water from springs in Ash Meadows National Wildlife Refuge, Nevada. Each spring was sampled two to five times between July, 1992 and March, 1994. Samples were collected and analyzed by the Harry Reid Center for Environmental Studies (HRC) Environmental/Analytical Laboratory, at the University of Nevada, Las Vegas. Chemical analyses included major cations and anions and trace elements. The analyses for the major anions were performed by atomic absorption (AA) spectrophotometry, the anions by ion chromatography (IC) and the trace elements by inductively coupled plasma - mass spectrometry (ICP-MS). The standard operating procedures (SOP) used for each method are included. The concentrations of the analytes range from the part per million (ppm) levels for the major cations and anions to the sub part per trillion (ppt) levels for a number of the trace elements. Approximately nine orders of magnitude are covered from the highest to the lowest concentrations. The formation of molecular species in the ICP-MS, plasma produces false positives for a number of elements. None of the elements reported here, that the HRC is aware of, are subject to these isobaric interferences, with the exception of europium (Eu). Europium values are reported for samplings four and five where the HRC used an extraction procedure that extracted Eu but not barium (Ba), whose oxides cause the interference. In order to overcome matrix effects in the samples from high concentrations of cations and other elements, the method of standard additions was instituted for the analysis of samplings four and five as an alternative to external standardization. It is believed that these data, and those for the Death Valley Spring reported in January, 1995 are the first efforts at such a comprehensive trace element analysis of ground waters. HRC has had to develop, test, and refine sampling and analysis procedures throughout the course of this study

  9. Behavior of the Pb–Li alloy impurities by ICP-MS

    International Nuclear Information System (INIS)

    Conde, E.; Barrado, A.I.; Pascual, L.; Fernández, M.; Salazar, J.M. Gómez de; Barrena, M.I.; Quiñones, J.

    2014-01-01

    Highlights: • In the new test blanket modules (TBM), Pb–Li alloy plays a key role in the new commercial fusion reactors functionality. • It is important to have a complete characterization to define their physicochemical properties and their regenerative function inside the blanket. • Methodology developed is a key tool that allows performing quality control procedures. • It is essential to determine concentrations of major and trace elements presents in Pb–Li alloy. It allows performing quality control procedures. • The inductively coupled plasma mass spectrometry (ICP-MS) is a highly sensitive technique, so enables very low detection limits. - Abstract: The ITER and DEMO projects are developing new test blanket modules (TBM), such as HCLL where the Li–Pb alloy plays a key role in the new commercial fusion reactors functionality. Lithium–lead eutectic alloy has no known uses outside of fusion technology, so the available databases of this material are currently incomplete. It is very important, within the material specifications, to have a complete characterization in order to define their chemical and physical properties, because any variation in the alloy composition has significant consequences in their behavior, and therefore in their regenerative function inside the blanket. This report provides a procedure to perform a wide material characterization, assessing the concentrations of major elements, as well as a review of trace level impurities that can be found both in the eutectic alloy as in starting materials. In this determination inductively coupled plasma mass spectrometry (ICP-MS) technique plays an important role, because as a highly sensitive technique it allows very low detection limits

  10. HPLC-ICP-MS speciation analysis of arsenic in urine of Japanese subjects without occupational exposure.

    Science.gov (United States)

    Hata, Akihisa; Endo, Yoko; Nakajima, Yoshiaki; Ikebe, Maiko; Ogawa, Masanori; Fujitani, Noboru; Endo, Ginji

    2007-05-01

    The toxicity and carcinogenicity of arsenic depend on its species. Individuals living in Japan consume much seafood that contains high levels of organoarsenics. Speciation analysis of urinary arsenic is required to clarify the health risks of arsenic intake. There has been no report of urinary arsenic analysis in Japan using high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). We performed speciation analysis of urinary arsenic for 210 Japanese male subjects without occupational exposure using HPLC-ICP-MS. The median values of urinary arsenics were as follows: sodium arsenite (AsIII), 3.5; sodium arsenate (AsV), 0.1; monomethylarsonic acid (MMA), 3.1; dimethylarsinic acid (DMA), 42.6; arsenobetaine (AsBe), 61.3; arsenocholine, trimethylarsine oxide, and unidentified arsenics (others), 5.2; and total arsenic (total As), 141.3 microgAs/l. The median creatinine-adjusted values were as follows: AsIII, 3.0; AsV, 0.1; MMA, 2.6; DMA, 35.9; AsBe, 52.1; others 3.5; and total As, 114.9 microgAs/g creatinine. Our findings indicate that DMA and AsBe levels in Japan are much higher than those found in Italian and American studies. It appears that the high levels of DMA and AsBe observed in Japan may be due in part to seafood intake. ACGIH and DFG set the BEI and BAT values for occupational arsenic exposure as 35 microgAs/l and 50 microgAs/l, respectively, using the sum of inorganic arsenic (iAs), MMA, and DMA. In the general Japanese population, the sums of these were above 50 microgAs/l in 115 (55%) samples. We therefore recommend excluding DMA concentration in monitoring of iAs exposure.

  11. Extraction techniques for arsenic species in rice flour and their speciation by HPLC-ICP-MS.

    Science.gov (United States)

    Narukawa, Tomohiro; Suzuki, Toshihiro; Inagaki, Kazumi; Hioki, Akiharu

    2014-12-01

    The extraction of arsenic (As) species present in rice flour samples was investigated using different extracting solvents, and the concentration of each species was determined by HPLC-ICP-MS after heat-assisted extraction. The extraction efficiencies for total arsenic species and especially for arsenite [As(III)] and arsenate [As(V)] were investigated. As(III), As(V) and dimethylarsinic acid (DMAA) were found in the samples, and the concentration of DMAA did not vary with treatment conditions. However, the concentrations of extracted total arsenic and those of As(III) and As(V) depended on the extracting solvents. When an extracting solvent was highly acidic, the concentrations of extracted total arsenic were in good agreement with the total arsenic concentration determined by ICP-MS after microwave-assisted digestion, though a part of the As(V) was reduced to As(III) during the highly acidic extraction process. Extraction under neutral conditions increased the extracted As(V), but extracted total arsenic was decreased because a part of the As(III) could not be extracted. Optimum conditions for the extraction of As(III) and As(V) from rice flour samples are discussed to allow the accurate determinations of As(III), As(V) and DMAA in the rice flour samples. Heat block extraction techniques using 0.05 mol L(-1) HClO4 and silver-containing 0.15 mol L(-1) HNO3 were also developed. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Determination of stable isotope ratio of lead in airborne particulate matter by ICP-MS

    International Nuclear Information System (INIS)

    Mukai, Hitoshi; Ambe, Yoshinari

    1990-01-01

    ICP-MS was applied to the measurement of stable isotope ratios of lead, which are used as an indicator of the source of lead in airborne particulate matter. For the measurement of lead isotopes ratios, the influences of machine conditions, lead concentration and matrix elements to the precision and accuracy of the measurements were studied. At a scanning mode, dwell time of 40∼160 μs gave the best precision to the isotope ratio measurements; about 0.3 % of R.S.D. for 206 Pb/ 207 Pb and 206 Pb/ 208 Pb, 0.6 % for 206 Pb/ 204 Pb. Precision of the measurement was better at a high concentration of lead in sample solution. The observed value of 206 Pb/ 207 Pb ratio was not affected by the lead concentration, but in the cases of 206 Pb/ 204 Pb and 206 Pb/ 208 Pb, about 1 % of the value changed in the observed ratios with the lead concentration of 100∼500 μg/l. Six matrix elements (Na, K, Ca, Mg, Al, Fe) did not affect the observed isotope ratios up to 200 mg/l. The lead isotope ratios of reference materials {Urban Particulates (NIST) and Vehicle Exhausted Particulates (NIES)} were measured by using two kinds of sample; crude sample and lead-isolated sample from matrix elements by anodic deposition. Both cases gave the same isotope ratio values, therefore, lead isotope ratios in airborne particulate samples can be measured by ICP-MS without any separation of lead from matrix elements. (author)

  13. Comparison of GC-ICP-MS and HPLC-ICP-MS for species-specific isotope dilution analysis of tributyltin in sediment after accelerated solvent extraction

    International Nuclear Information System (INIS)

    Wahlen, Raimund; Wolff-Briche, Celine

    2003-01-01

    This study describes a direct comparison of GC and HPLC hyphenated to ICP-MS determination of tributyltin (TBT) in sediment by species-specific isotope dilution analysis (SS-IDMS). The certified reference sediment PACS-2 (NRC, Canada) and a candidate reference sediment (P-18/HIPA-1) were extracted using an accelerated solvent extraction (ASE) procedure. For comparison of GC and LC methods an older bottle of PACS-2 was used, whilst a fresh bottle was taken for demonstration of the accuracy of the methods. The data obtained show good agreement between both methods for both the PACS-2 sediment (LC-ICP-IDMS 828±87 ng g -1 TBT as Sn, GC-ICP-IDMS 848±39 ng g -1 TBT as Sn) and the P-18/ HIPA-1 sediment (LC-ICP-IDMS 78.0±9.7 ng g -1 TBT as Sn, GC-ICP-IDMS 79.2±3.8 ng g -1 TBT as Sn). The analysis by GC-ICP-IDMS offers a greater signal-to-noise ratio and hence a superior detection limit of 0.03 pg TBT as Sn, in the sediment extracts compared to HPLC-ICP-IDMS (3 pg TBT as Sn). A comparison of the uncertainties associated with both methods indicates superior precision of the GC approach. This is related to the better reproducibility of the peak integration, which affects the isotope ratio measurements used for IDMS. The accuracy of the ASE method combined with HPLC-ICP-IDMS was demonstrated during the international interlaboratory comparison P-18 organised by the Comite Consultatif pour la Quantite de Matiere (CCQM). The results obtained by GC-ICP-IDMS for a newly opened bottle of PACS-2 were 1087±77 ng g -1 Sn for DBT and 876±51 ng g -1 Sn for TBT (expanded uncertainties with a coverage factor of 2), which are in good agreement with the certified values of 1090±150 ng g -1 Sn and 980±130 ng g -1 Sn, respectively. (orig.)

  14. Toepassing van DIN-ICP-MS en scanning-scouting van B en Mo in grondwater, drinkwater en regenwater

    NARCIS (Netherlands)

    van den Velde-Koerts T; LAC

    1998-01-01

    Doel van dit onderzoek was het ontwikkelen van een bepalingsmethode voor boor (B) en molybdeen (Mo) met ICP-MS om een indruk te krijgen van de concentraties in grond-, drink- en regenwater van Nederland. Omdat B adsorbeert aan de wand van de meeste verstuiverkamers (memory-effect) werd een directe

  15. Forensic identification of trunk mat by trace element analysis of single fiber with laser ablation ICP-MS

    International Nuclear Information System (INIS)

    Hiroma, Yuki; Nakai, Izumi; Hokura, Akiko

    2010-01-01

    The application of LA-ICP-MS (laser ablation inductively coupled plasma mass spectrometry) to the chemical characterization of single trunk mat fibers made of PET was investigated in order to establish a forensic analytical method for the discrimination of samples of different origins. The analytical conditions of LA-ICP-MS equipped with a 213 nm Nd : YAG laser were optimized to analyze trace elements, such as Cu, Sb, and Ba at ppm levels. A total of 31 samples produced by 7 car manufactures in Japan were used for analysis. The concentrations of Li, Mg, Al, P, Ca, Ti, Co, Cu, Ge, Nb, Sb, Ta, and Pb were successfully measured from a single fiber sample with a diameter of ca. 20 μm. It was possible to discriminate all 31 samples based on the analytical results of a single fiber by LA-ICP-MS combined with those of FT-IR and SEM-EDS. LA-ICP-MS has good analytical sensitivity, and requires a much shorter preparation time and a smaller sample size than any other conventional element analysis methods. This paper demonstrates for the first time that this method is practically useful as a powerful tool for the forensic identification of a single trunk mat fiber. (author)

  16. Determination of bismuth in environmental samples by ICP-MS and basic examination of cell toxicity for their compounds

    International Nuclear Information System (INIS)

    Kobayashi, Jun; Matsukawa, Takehisa; Chiba, Momoko; Yokoyama, Kazuhito; Terada, Hiroshi; Sugiyama, Hideo

    2011-01-01

    We examined both bismuth content levels in some environmental water samples (tapwater, bottled drinking water and slag obtained by sewage disposal) by inductively coupled plasma mass spectrometry (ICP-MS) and cultured cell toxicity of their compounds by the MTT assay. For ICP-MS, the conditions examined were addition of internal standard (IS), apparatus condition, and determination range, etc. When we examined an IS, the advantage was not clear that the ICP-MS response of the IS candidate elements was very variable. However, the sample induction rate into ICP-MS is more changeable at any time. Since the correction of analytical results was enabled by the addition of IS, Tl-203 was selected for IS, and was used in this study. The determination lower limit was 11 ppt by using 10 ppb Tl. Bi was detected in a few environmental water samples at 20.4 ppt - 6.8 ppb (0.07-6.83 μg/g original slags), but Bi concentrations of most samples were lower than the determination limit. On the other hand, concerning cell toxicity, the subgallate and free gallic acid affected the lives of cultured cells. Especially, the toxicity of free gallic acid was higher. It has been understood that the toxicity is weakly adjusted by chelating with Bi. (author)

  17. Determination of inorganic arsenic in white fish using microwave-assisted alkaline alcoholic sample dissolution and HPLC-ICP-MS

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Engman, Joakim; Sloth, Jens Jørgen

    2005-01-01

    An analytical method for the determination of inorganic arsenic in fish samples using HPLC-ICP-MS has been developed. The fresh homogenised sample was subjected to microwave-assisted dissolution by sodium hydroxide in ethanol, which dissolved the sample and quantitatively oxidised arsenite (As...

  18. Application of ICP-MS radionuclide analysis to 'Real World' samples of Department of Energy radioactive waste

    International Nuclear Information System (INIS)

    Meeks, A.M.; Giaquinto, J.M.; Keller, J.M.

    1998-01-01

    Disposal of Department of Energy (DOE) radioactive waste into repositories such as the Waste Isolation Pilot Plant (WIPP) and the Nevada Test Site (NTS) requires characterization to ensure regulatory and transportation requirements are met and to collect information regarding chemistry of the waste for processing concerns. Recent addition of an inductively coupled plasma quadrupole mass spectrometer in a radioactive contaminated laboratory at the Oak Ridge National Laboratory (ORNL) has allowed the evaluation of advantages of using ICP-MS over traditional techniques for some of these characterization needs. The measurement of long-lived beta nuclides (i.e. 99 Tc) by ICP-MS has resulted in improved detection limits and accuracy than the traditional counting techniques as well as reducing the need for separation/purification techniques which increase personnel exposure to radiation. Using ICP-MS for the measurement of U isotopes versus the traditional Thermal Ionization Mass Spectrometer (TIMS) technique has reduced cost and time by more than half while still maintaining the needed accuracy to determine risk assessment of the waste tanks. In addition, the application of ICP-MS to ORNL waste tank characterization has provided the opportunity to estimate non-routine radionuclides (i.e. 135 Cs and 151 Sm) and non-routine metals (i.e. Li, Ti, rare earths, etc.) using a rapid low cost screening method. These application methodologies and proficiencies on ORNL waste samples are summarized throughout the paper. (author)

  19. U-Pb zircon in situ dating with LA-MC-ICP-MS using a mixed detector configuration

    Energy Technology Data Exchange (ETDEWEB)

    Chemale Junior, Farid, E-mail: fchemale@unb.br [Universidade de Brasilia (UnB), DF (Brazil). Inst. de Geociencias; Kawashita, Koji; Dussin, Ivo A. [Universidade de Sao Paulo (USP), SP (Brazil). Centro de Pesquisas Geocronologicas; Avila, Janaina N. [Australian National University, Canberra, (Australia). Research School of Earth Sciences; Justino, Dayvisson; Bertotti, Anelise [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Curso de Pos-Graduacao em Geociencias

    2012-06-15

    The LA-MC-ICP-MS method applied to U-Pb in situ dating is still rapidly evolving due to improvements in both lasers and ICP-MS. To test the validity and reproducibility of the method, 5 different zircon samples, including the standard Temora-2, ranging in age between 2.2 Ga and 246 Ma, were dated using both LA-MC-ICP-MS and SHRIMP. The selected zircons were dated by SHRIMP and, after gentle polishing, the laser spot was driven to the same site or on the same zircon phase with a 213 nm laser microprobe coupled to a multi-collector mixed system. The data were collected with a routine spot size of 25 {mu}m and, in some cases, of 15 and 40 {mu}m. A careful cross-calibration using a diluted U-Th-Pb solution to calculate the Faraday reading to counting rate conversion factors and the highly suitable GJ-1 standard zircon for external calibrations were of paramount importance for obtaining reliable results. All age results were concordant within the experimental errors. The assigned age errors using the LA-MC-ICP-MS technique were, in most cases, higher than those obtained by SHRIMP, but if we are not faced with a high resolution stratigraphy, the laser technique has certain advantages. (author)

  20. Metabolite profiling with HPLC-ICP-MS as a tool for in vivo characterization of imaging probes.

    Science.gov (United States)

    Boros, Eszter; Pinkhasov, Omar R; Caravan, Peter

    2018-01-01

    Current analytical methods for characterizing pharmacokinetic and metabolic properties of positron emission tomography (PET) and single photon emission computed tomography (SPECT) probes are limited. Alternative methods to study tracer metabolism are needed. The study objective was to assess the potential of high performance liquid chromatography - inductively coupled plasma - mass spectrometry (HPLC-ICP-MS) for quantification of molecular probe metabolism and pharmacokinetics using stable isotopes. Two known peptide-DOTA conjugates were chelated with nat Ga and nat In. Limit of detection of HPLC-ICP-MS for 69 Ga and 115 In was determined. Rats were administered 50-150 nmol of Ga- and/or In-labeled probes, blood was serially sampled, and plasma analyzed by HPLC-ICP-MS using both reverse phase and size exclusion chromatography. The limits of detection were 0.16 pmol for 115 In and 0.53 pmol for 69 Ga. Metabolites as low as 0.001 %ID/g could be detected and transchelation products identified. Simultaneous administration of Ga- and In-labeled probes allowed the determination of pharmacokinetics and metabolism of both probes in a single animal. HPLC-ICP-MS is a robust, sensitive and radiation-free technique to characterize the pharmacokinetics and metabolism of imaging probes.

  1. Selenium speciation analysis of Misgurnus anguillicaudatus selenoprotein by HPLC-ICP-MS and HPLC-ESI-MS/MS

    Science.gov (United States)

    Analytical methods for selenium (Se) speciation were developed using high performance liquid chromatography (HPLC) coupled to either inductively coupled plasma mass spectrometry (ICP-MS) or electrospray ionization tandem mass spectrometry (ESI-MS/MS). Separations of selenomethionine (Se-Met) and sel...

  2. Separation and quantitation of radionuclides in Hanford environmental and waste tank samples using IC-ICP/MS techniques

    International Nuclear Information System (INIS)

    Farmer, O.T. III; Smith, M.R.; Wyse, E.J.; Barinage, C.J.; Koppenaal, D.W.

    1996-01-01

    The use of shielded ICP/MS instrumentation to characterize radioactive material has seen marked growth over the past few years. With a lower limit detection now in the fg/mL range for newer units, ICP/MS has become the method of choice for many studies requiring rapid, isotopic analysis of both stable elements and radionuclides with half-lives greater than 102-103 years. However, despite its sensitivity and versatility, ICP/MS has heretofore had some notable limitations in certain radiological applications. For example, Hanford waste tank samples contain a variety of nuclides with altered isotopic abundances, which complicate identification of these nuclides. Even if a nuclide can be identified, conventional quantitation using vendor-supplied software assumes natural, or knowledge of, isotopic abundance. Difficult sample matrices like those obtained from the Hanford tanks can further complicate interpretation and quantitation. On-line ion chromatography (IC) has been recently employed to mitigate some these problems. By sequentially separating elements, isobars can be resolved, thereby permitting the unequivocal determination of isotopic abundances. But even though the technique resolves isobaric interferences and is effective in reducing matrix problems, IC does not easily lend itself to quantitation. Internal standards, which are crucial for quantitation during a prolonged ICP/MS analysis with varying eluant matrices, are separated or affected as any indigenous element is using standard IC methodology

  3. Single particle ICP-MS combined with a data evaluastion tool as a routine techique for the analysis of nanoparticles in complex matrices

    NARCIS (Netherlands)

    Peters, R.J.B.; Herrera-Rivera, Z.; Undas, A.K.; Lee, van der M.K.; Marvin, H.J.P.; Bouwmeester, H.; Weigel, S.

    2015-01-01

    Detection and characterization of nanoparticles (NPs) in complex media as consumer products, food and toxicological test media is an essential part of understanding the potential benefits and risks of the application of nanoparticles. Single particle ICP-MS (spICP-MS) was studied as a screening tool

  4. Measurement of elemental speciation by liquid chromatography -- inductively coupled plasma mass spectrometry (LC-ICP-MS) with the direct injection nebulizer (DIN)

    Energy Technology Data Exchange (ETDEWEB)

    Shum, Sam [Iowa State Univ., Ames, IA (United States)

    1993-05-01

    This thesis is divided into 4 parts: elemental speciation, speciation of mercury and lead compounds by microbore column LC-ICP-MS with direct injection nebulization, spatially resolved measurements of size and velocity distributions of aerosol droplets from a direct injection nebulizer, and elemental speciation by anion exchange and size exclusion chromatography with detection by ICP-MS with direct injection nebulization.

  5. Development of analytical methods for the determination of trace elements in sediment with Neutron ActivAtion method (NAA) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Nam, Sang Ho; Kim, Jae Jin; Chung, Yong Sam; Kim, Sun Ha

    2005-01-01

    The analytical methods for the determination of major elements (Al, Ca, K, Fe, Mg) in sediment have been investigated with ICP-MS. The analytical results of major elements with Cool ICP-MS were much better than those with normal ICP-MS. The analytical results were compared with those of NAA. NAA were a little superior to ICP-MS for the determination of major elements in sediment, and NAA is a non-destructive analytical method. The analytical methods for the determination of minor elements (Cr, Ce, U, Co, Pb, As, Se) in sediment have been also studied with ICP-MS. The analytical results by standard calibration with ICP-MS were not accurate due to matrix interferences. Thus, internal standard method was applied, then the analytical results for minor element with ICP-MS were greatly improved. The analytical results obtained by ICP-MS were compared with those obtained by NAA. It showed that the two analytical methods have great capabilities for the determination of minor elements in sediments

  6. Quantification and speciation of technetium-99 in samples at low levels: contributions of capillary electrophoresis / ICP-MS system

    International Nuclear Information System (INIS)

    Kasprzak, L.M.

    2007-01-01

    Given the low levels of 99 Tc (long half-lived artificial radionuclide) in the environment (10 -8 M to 10 -12 M), its determination currently necessitates an enrichment and separation from the sample matrix prior to instrumental measurement. Therefore, nuclear safety monitoring requires the knowledge of the redox and chemical properties of this element in order to predict its behaviour and transfer in the environment. So, a separative and very sensitive measurement technique must thus be employed. We have developed a new environmental measurement method applied to the quantification and speciation of 99 Tc in sample at environmental concentrations. Indeed, we have combined a Capillary Electrophoresis (CE) with an Inductively Coupled Plasma Mass Spectrometer (ICP-MS). The limit of detection of 99 Tc is about 2.10 -8 M by CE/ICP-MS system equipped with a PFA-50 nebuliser. In addition to the detection and measurement of technetium, we can separate online 99 Tc(VII) of its interfering radionuclides like molybdenum and ruthenium by CE/ICP-MS. Indeed, due do the different migration time of each anions, it's possible to determinate a signal at m/z= 99 which is only given to 99 Tc. Results obtained by this method have been compared to an usual radiochemical technique, extraction of Tc(VII) by a TEVA resin followed by ICP-MS measurement. Within the framework of storage of spent fuel, studies on the speciation of Tc(VII) by CE / ICP-MS iron-sulphide soils in anoxic conditions have shown that technetium VII is reduced by sulphured suspensions. (author)

  7. Feasibility of asymmetric flow field-flow fractionation coupled to ICP-MS for the characterization of wear metal particles and metalloproteins in biofluids from hip replacement patients

    DEFF Research Database (Denmark)

    Löschner, Katrin; Harrington, Chris F.; Kearney, Jacque-Lucca

    2015-01-01

    or other elements, but the current analytical methods used to investigate the processes involved do not provide sufficient information to understand the size or composition of the wear particles generated in vivo. In this qualitative feasibility study, asymmetric flow field-flow fractionation (AF4) coupled...... to ICP-MS was used to confirm the metal–protein associations in the serum samples. Off-line single particle ICP-MS (spICP-MS) analysis was used to confirm the approximate size distribution indicated by AF4 of the wear particles in hip aspirates. In the serum samples, AF4–ICP-MS suggested that Cr...... unidentified compounds; AEC analysis confirmed the Cr results and the association of Co with Alb and a second compound. Enzymatic digestion of the hip aspirate sample, followed by separation using AF4 with detection by UV absorption (280 nm), multi-angle light scattering and ICP-MS, suggested that the sizes...

  8. ICP-MS with hexapole collision cell for isotope ratio measurements of Ca, Fe, and Se

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, S.F. [Radiation Physics and Chemistry Problems Inst., Minsk (Belarus); Becker, J.S. [Central Department for Analytical Chemistry, Research Centre Juelich (Germany)

    2001-07-01

    To avoid mass interferences on analyte ions caused by argon ions and argon molecular ions via reactions with collision gases, an rf hexapole filled with helium and hydrogen has been used in inductively coupled plasma mass spectrometry (ICP-MS), and its performance has been studied. Up to tenfold improvement in sensitivity was observed for heavy elements (m > 100 u), because of better ion transmission through the hexapole ion guide. A reduction of argon ions Ar{sup +} and the molecular ions of argon ArX{sup +} (X = O, Ar) by up to three orders of magnitude was achieved in a hexapole collision cell of an ICP-MS (''Platform ICP'', Micromass, Manchester, UK) as a result of gas-phase reactions with hydrogen when the hexapole bias (HB) was set to 0 V; at an HB of 1.6 V argon, and argon-based ions of masses 40 u, 56 u, and 80 u, were reduced by approximately four, two, and five orders of magnitude, respectively. The signal-to-noise ratio {sup 80}Se/ {sup 40}Ar{sub 2}{sup +} was improved by more than five orders of magnitude under optimized experimental conditions. Dependence of mass discrimination on collision-cell properties was studied in the mass range 10 u (boron) to 238 u (uranium). Isotopic analysis of the elements affected by mass-spectrometric interference, Ca, Fe, and Se, was performed using a Meinhard nebulizer and an ultrasonic nebulizer (USN). The measured isotope ratios were comparable with tabulated values from IUPAC. Precision of 0.26%, 0.19%, and 0.12%, respectively, and accuracy of 0.13% 0.25%, and 0.92%, respectively, was achieved for isotope ratios {sup 44}Ca/ {sup 40}Ca and {sup 56}Fe/{sup 57}Fe in 10 {mu}g L{sup -1} solution nebulized by means of a USN and for {sup 78}Se/{sup 80}Se in 100 {mu}g L{sup -1} solution nebulized by means of a Meinhard nebulizer. (orig.)

  9. Determination of arsenenic compounds in environmental and biological samples with LAMMA and HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Goessler, W.

    1997-07-01

    Different arsonium salts and alkyl- or aryl arsine sulfides were analyzed with a Laser-Microprobe-Mass-Analyzer (LAMMA-500). The positive-ion spectra of the arsonium salts showed clear signals for the (CH 3 ) 3 AsR + fragment. In the positive-ion spectra of alkyl- or arylarsine sulfides these arsenic compounds the molecular ions R 3 AsS + were never observed, but in most of the spectra the protonated parent compounds R 3 AsSH2 + were present. The negative-ion spectra showed mainly fragments S-n (n = 1, 2, 3, 4) and AsS n (n = 1, 2, 3). Chlorella vulgaris Beijerinck var. vulgaris with a concentration of 13,000 mg As/kg dry mass were analyzed with the LAMMA-500 to identify arsenic compounds. Surprisingly, arsenic could not be detected by the LAMMA technique at these high arsenic concentrations. Electron microscopy of Chlorella cells reveals, that particles adhered at the surface of the cells. Scanning transmission electron microscopy showed a high correlation between the arsenic concentration and the iron concentration in these particles. Algae may protect themselves from high arsenic concentrations, by precipitating FeAsO 4 at the cell surface. Different Chlorella sp. were grown to investigate the arsenic tolerance of Chlorella strains. Chlorella Boehm and Chlorella Kessleri grew better in arsenic-containing than in arsenic-free media. The growth of Chlorella 108 was depressed in high-arsenic media. After harvesting, the algal biomass was extracted and arsenic compounds determined in the extracts with HPLC-ICP-MS. Approximately 98 % of the total arsenic were present as arsenic acid. A method for the simultaneous identification and quantification of arsenocholine, arsenous acid, dimethylarsinic acid, arsenobetaine, methylarsonic acid, and arsenic acid at concentrations below 1 μg/L was developed. The developed HPLC-MPN-ICP-MS system allows the determination of arsenic compounds in urine sample at concentrations of 0.5 μg As/L with a relative standard deviation of

  10. Quantitating Iron in Serum Ferritin by Use of ICP-MS

    Science.gov (United States)

    Smith, Scott M.; Gillman, Patricia L.

    2003-01-01

    A laboratory method has been devised to enable measurement of the concentration of iron bound in ferritin from small samples of blood (serum). Derived partly from a prior method that depends on large samples of blood, this method involves the use of an inductively-coupled-plasma mass spectrometer (ICP-MS). Ferritin is a complex of iron with the protein apoferritin. Heretofore, measurements of the concentration of serum ferritin (as distinguished from direct measurements of the concentration of iron in serum ferritin) have been used to assess iron stores in humans. Low levels of serum ferritin could indicate the first stage of iron depletion. High levels of serum ferritin could indicate high levels of iron (for example, in connection with hereditary hemochromatosis an iron-overload illness that is characterized by progressive organ damage and can be fatal). However, the picture is complicated: A high level of serum ferritin could also indicate stress and/or inflammation instead of (or in addition to) iron overload, and low serum iron concentration could indicate inflammation rather than iron deficiency. Only when concentrations of both serum iron and serum ferritin increase and decrease together can the patient s iron status be assessed accurately. Hence, in enabling accurate measurement of the iron content of serum ferritin, the present method can improve the diagnosis of the patient s iron status. The prior method of measuring the concentration of iron involves the use of an atomic-absorption spectrophotometer with a graphite furnace. The present method incorporates a modified version of the sample- preparation process of the prior method. First, ferritin is isolated; more specifically, it is immobilized by immunoprecipitation with rabbit antihuman polyclonal antibody bound to agarose beads. The ferritin is then separated from other iron-containing proteins and free iron by a series of centrifugation and wash steps. Next, the ferritin is digested with nitric acid

  11. Development of a chromatographic separation method hyphenated to electro-spray ionization mass spectrometry (ESI-MS) and inductively coupled plasma mass spectrometry (ICP-MS): application to the lanthanides speciation analysis

    International Nuclear Information System (INIS)

    Beuvier, Ludovic

    2015-01-01

    This work focuses on the development of a chromatographic separation method coupled to both ESI-MS and ICP-MS in order to achieve the comprehensive speciation analysis of lanthanides in aqueous phase representative of back-extraction phases of advanced spent nuclear fuel treatment processes. This analytical method allowed the separation, the characterization and the quantitation of lanthanides complexes holding poly-aminocarboxylic ligands, such as DTPA and EDTA, used as complexing agents in these processes. A HILIC separation method of lanthanides complexes has been developed with an amide bonded stationary phase. A screening of a wide range of mobile phase compositions demonstrated that the adsorption mechanism was predominant. This screening allowed also obtaining optimized separation conditions. Faster analysis conditions with shorter amide column packed with sub 2 μm particles reduced analysis time by 2.5 and 25% solvent consumption. Isotopic and structural characterization by HILIC ESI-MS was performed as well as the development of external calibration quantitation method. Analytical performances of quantitation method were determined. Finally, the development of the HILIC coupling to ESI-MS and ICP-MS was achieved. A simultaneous quantitation method by ESI-MS and ICP-MS was performed to determine the species quantitative distribution in solution. Analytical performances of quantitation method were also determined. (author) [fr

  12. Off-line separation and determination of rare earth elements associated with chloroplast pigments of hyperaccumulator Dicranopteris dichotoma by normal-phase liquid chromatography and ICP-MS.

    Science.gov (United States)

    Wei, Z G; Hong, F S; Yin, M; Li, H X; Hu, F; Zhao, G W; Wong, J W C

    2004-10-01

    An off-line normal-phase liquid chromatography-ICP-MS method has been used for separation and determination of the rare earth elements (REE) associated with chloroplast pigments of Dicranopteris dichotoma. The stability of REE-bound pigments was tested, and almost no destruction of REE-bound pigments occurred during the so-called normal-phase liquid chromatography. The accumulated free REE ions on the microcrystalline cellulose column were cleaned by elution with 5 mmol L(-1) 2-ethylhexyl hydrogen 2-ethylhexylphosphonate (P507), to avoid exchange of these free ions with metals from the pigments. When these precautions were taken, the method was applied to the study of REE-bound pigments in D. dichotoma. ICP-MS results showed REE were present in chlorophylls and lutein, although REE concentrations in carotene and pheophytin were both below procedural blank levels. By careful analysis of the eluate fractions containing chlorophyll a it was found that REE-bound chlorophyll a in D. dichotoma was slightly enriched in the fractions with relatively short retention time. Results indicated that the retention time of REE-bound chlorophyll a might be slightly less than that of magnesium chlorophyll a, and REE-bound chlorophylls might be of relatively low polarity in comparison with magnesium bound chlorophylls. This phenomenon could be explained by the special double-decker sandwich-structure of REE-bound chlorophylls, as was reported by us and other authors. On the basis of these results we preferred to consider that REE can replace magnesium in chlorophyll a of D. dichotoma, and that the role of REE-bound chlorophylls in photosynthesis cannot be neglected. These data might be useful for understanding of both the properties of REE-bound pigments and the effect of REE on plant photosynthesis.

  13. Elemental analysis of soils using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and laser-induced breakdown spectroscopy (LIBS) with multivariate discrimination: tape mounting as an alternative to pellets for small forensic transfer specimens.

    Science.gov (United States)

    Jantzi, Sarah C; Almirall, José R

    2014-01-01

    Elemental analysis of soil is a useful application of both laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and laser-induced breakdown spectroscopy (LIBS) in geological, agricultural, environmental, archeological, planetary, and forensic sciences. In forensic science, the question to be answered is often whether soil specimens found on objects (e.g., shoes, tires, or tools) originated from the crime scene or other location of interest. Elemental analysis of the soil from the object and the locations of interest results in a characteristic elemental profile of each specimen, consisting of the amount of each element present. Because multiple elements are measured, multivariate statistics can be used to compare the elemental profiles in order to determine whether the specimen from the object is similar to one of the locations of interest. Previous work involved milling and pressing 0.5 g of soil into pellets before analysis using LA-ICP-MS and LIBS. However, forensic examiners prefer techniques that require smaller samples, are less time consuming, and are less destructive, allowing for future analysis by other techniques. An alternative sample introduction method was developed to meet these needs while still providing quantitative results suitable for multivariate comparisons. The tape-mounting method involved deposition of a thin layer of soil onto double-sided adhesive tape. A comparison of tape-mounting and pellet method performance is reported for both LA-ICP-MS and LIBS. Calibration standards and reference materials, prepared using the tape method, were analyzed by LA-ICP-MS and LIBS. As with the pellet method, linear calibration curves were achieved with the tape method, as well as good precision and low bias. Soil specimens from Miami-Dade County were prepared by both the pellet and tape methods and analyzed by LA-ICP-MS and LIBS. Principal components analysis and linear discriminant analysis were applied to the multivariate data

  14. In-situ Strontium Isotopes Analysis on Single Conodont Apatite by LA-MC-ICP-MS

    Science.gov (United States)

    Zhao, L.; Zhang, L.; Chen, Z. Q.; Ma, D.; Qiu, H.; Lv, Z.; Hu, Z.; Wang, F.

    2014-12-01

    Strontium isotope played an important role in stratigraphic chronology and sedimentary geochemistry research (McArthur et al., 2001). Conodonts is a kind of extinct species of marine animals and widely distributed in marine sediments all over the world. Rich in radiogenic Sr contents and difficulty to be affected during diagenesis alteration makes conodonts a good choice in seawater Sr isotope composition studies (John et al., 2008). Conodont samples were collected from 24th to 39th layer across Permian-Triassic boundary at Meishan D section (GSSP), Zhejiang Province, South China (Yin et al., 2001). Conodonts was originated from fresh limestone and only conodont elements with CAIextinction events during the Permian-Triassic transition. Our study also makes is possible for high resolution 87Sr/ 86Sr ratio testing on the single conodont apatite and riched the in-situ studies on the conodont apatite, which of great significance for the future conodont Sr isotope research (Zhao et al., 2009; Zhao et al., 2013). Keywords: Conodonts, Strontium isotope, LA-MC-ICP-MS, Permian-Triassic transition, Meishan D section [1] John et al., 2008 3P[2] McArthur et al., 2001 J. of Geology [3] Yin et al., 2001 Episodes [4] Zhao et al., 2009 Earth Science J. of CUG [5] Zhao et al., 2013 GPC.

  15. The Effect of Aqueous Alteration in Antarctic Carbonaceous Chondrites from Comparative ICP-MS Bulk Chemistry

    Science.gov (United States)

    Alonso-Azcarate, J.; Trigo-Rodriguez, J. M.; Moyano-Cambero, C. E.; Zolensky, M.

    2014-01-01

    Terrestrial ages of Antarctic carbonaceous chondrites (CC) indicate that these meteorites have been preserved in or on ice for, at least, tens of thousands of years. Due to the porous structure of these chondrites formed by the aggregation of silicate-rich chondrules, refractory inclusions, metal grains, and fine-grained matrix materials, the effect of pervasive terrestrial water is relevant. Our community defends that pristine CC matrices are representing samples of scarcely processed protoplanetary disk materials as they contain stellar grains, but they might also trace parent body processes. It is important to study the effects of terrestrial aqueous alteration in promoting bulk chemistry changes, and creating distinctive alteration minerals. Particularly because it is thought that aqueous alteration has particularly played a key role in some CC groups in modifying primordial bulk chemistry, and homogenizing the isotopic content of fine-grained matrix materials. Fortunately, the mineralogy produced by parent-body and terrestrial aqueous alteration processes is distinctive. With the goal to learn more about terrestrial alteration in Antarctica we are obtaining reflectance spectra of CCs, but also performing ICP-MS bulk chemistry of the different CC groups. A direct comparison with the mean bulk elemental composition of recovered falls might inform us on the effects of terrestrial alteration in finds. With such a goal, in the current work we have analyzed some members representative of CO and CM chondrite groups.

  16. Monitoring of metallic contaminants in energy drinks using ICP-MS.

    Science.gov (United States)

    Kilic, Serpil; Cengiz, Mehmet Fatih; Kilic, Murat

    2018-03-09

    In this study, an improved method was validated for the determination of some metallic contaminants (arsenic (As), chromium (Cr), cadmium (Cd), lead (Pb), iron (Fe), nickel (Ni), copper (Cu), Mn, and antimony (Sb)) in energy drinks using inductive coupled plasma mass spectrometry (ICP-MS). The validation procedure was applied for the evaluation of linearity, repeatability, recovery, limit of detection, and quantification. In addition, to verify the trueness of the method, it was participated in an interlaboratory proficiency test for heavy metals in soft drink organized by the LGC (Laboratory of the Government Chemist) Standard. Validated method was used to monitor for the determination of metallic contaminants in commercial energy drink samples. Concentrations of As, Cr, Cd, Pb, Fe, Ni, Cu, Mn, and Sb in the samples were found in the ranges of 0.76-6.73, 13.25-100.96, 0.16-2.11, 9.33-28.96, 334.77-937.12, 35.98-303.97, 23.67-60.48, 5.45-489.93, and 0.01-0.42 μg L -1 , respectively. The results were compared with the provisional guideline or parametric values of the elements for drinking waters set by the WHO (World Health Organization) and EC (European Commission). As, Cd, Cu, and Sb did not exceed the WHO and EC provisional guideline or parametric values. However, the other elements (Cr, Pb, Fe, Ni, and Mn) were found to be higher than their relevant limits at various levels.

  17. 99Tc atom counting by quadrupole ICP-MS. Optimisation of the instrumental response

    International Nuclear Information System (INIS)

    Mas, Jose L.; Garcia-Leon, Manuel; Bolivar, Juan P.

    2002-01-01

    In this paper, an extensive work is done on the specific tune of a conventional ICP-MS for 99 Tc atom counting. For this, two methods have been used and compared: the partial variable control method and the 5D Simplex method. Instrumental limits of detection of 0.2 and 0.8 ppt, respectively, were obtained. They are noticeably lower than that found with the automatic tune method of the spectrometer, 47 ppt, which shows the need of a specific tune when very low levels of 99 Tc have to be determined. A study is presented on the mass interferences for 99 Tc. Our experiments show that the formation of polyatomic atoms or refractory oxides as well as 98 Mo hydrides seem to be irrelevant for 99 Tc atom counting. The opposite occurs with the presence of isobaric interferences, i.e. 99 Ru, and the effect of abundance sensitivity, or low-mass resolution, which can modify the response at m/z=99 to a non-negligible extent

  18. Determination of 210Pb at ultra-trace levels in water by ICP-MS

    International Nuclear Information System (INIS)

    Lariviere, D.; Reiber, K.M.; Evans, R.D.; Cornett, R.J.

    2005-01-01

    210 Pb (t 1/2 = 22.26 years) is one of the most difficult naturally occurring radionuclides to analyze directly via radiometric measurement due to its low-energy radioactive decay. In this work, inductively coupled plasma mass spectrometry (ICP-MS) was investigated as a possible alternative to radiometric counting for the determination of 210 Pb. The formation of isobaric and polyatomic (molecular) interferences was studied and various strategies (i.e. co-precipitation, extraction chromatography, and derivatization) were tested to assess their usefulness in reducing these interferences. In addition, the potential of these strategies as pre-concentration methods was demonstrated. A 210 Pb pre-concentration of >300-fold and recoveries of 63-73% were obtained using a combined co-precipitation and extraction chromatography protocol followed by derivatization using an ethylating reagent. The abundance sensitivity at m/z = 210 in the presence of stable Pb was also investigated for three types of mass spectrometers (sector-field (ICP-SFMS), quadrupole-based (ICP-QMS), and quadrupole-based with a dynamic reaction cell (ICP-QMS (DRC))). Finally, the method was applied to determine 210 Pb in water samples and a detection limit of 90 mBq L -1 (10 pg L -1 ) was obtained

  19. Study of Long-Lived Radionuclides in Environmental Samples by ICP-MS

    International Nuclear Information System (INIS)

    Conde, E.; Navarro, N.; Fernández, M.

    2015-01-01

    Thorium is considered as one of the highly radiotoxic elements, because following its decay a number of other α, β and/or γ emitting daughters are produced. Uranium mining and processing, as well as remediation of impacted soils, are one of the principal anthropogenic sources of thorium release to the air, soil and water. Measurement of Th isotopes requires the use of analytical techniques capable of reliably measure the content of Th isotopes at trace levels. 230Th determination has generally been performed by α-spectrometry. However, this method needs sample preparation of 3-4 days and counting times from days to up to two weeks. A way to face this difficulty is the use of inductively coupled plasma mass spectrometry (ICP-MS). This technique is adequate for the determination of 232Th and 238U, long-lived radionuclides, and it can be applied, successfully, in the determination of 230Th, particularly if it is associated with a pre-concentration stage. This work presents the development of a rapid and simple analytical procedure based on mass spectrometry for the determination of 230Th and the results obtained in the analysis of environmental filters.

  20. Separation of organic and inorganic arsenic species by HPLC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Londesborough, S. [University of Helsinki, Department of Chemistry (Finland); Mattusch, J.; Wennrich, R. [UFZ-Centre for Environmental Research Leipzig-Halle, Department of Analytical Chemistry, Leipzig (Germany)

    1999-03-01

    The HPLC separation of eight anionic, cationic or neutral arsenic species (arsenite, arsenate, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine, arsenocholine, trimethylarsine oxide and tetramethylarsonium ion) on a high-capacity, anion-exchange column (Ion Pac AS 7, Dionex) was studied. The separation was performed during one run with a nitric acid gradient ranging from pH 4-1.3. The influence of sodium dodecyl sulfate (SDS), sodium octyl sulfate (SOS) and 1,2-benzenedisulfonic acid (BDSA) as ion pairing eluent modifiers was investigated. In addition the effect of elevated temperatures (30 to 40 C) was studied. The best results were obtained at room temperature of 20 C with 0.05 mM benzenedisulfonic acid as the eluent modifier. The chromatograph was connected to an ICP-MS via a cross-flow nebulizer. Detection limits obtained with the optimized chromatographic separation were 0.16-0.60 {mu}g As L{sup -1} for different species. The proposed speciation method was applied to the determination of arsenic species in the DORM-2 reference material (Dogfish Muscle) and in aqueous extracts of mushrooms collected on arsenic contaminated ground. (orig.) With 7 figs., 4 tabs., 17 refs.

  1. ICP-MS determination of boron: method optimization during preparation of graphite reference material for boron

    International Nuclear Information System (INIS)

    Granthali, S.K.; Shailaja, P.P.; Mainsha, V.; Venkatesh, K.; Kallola, K.S.; Sanjukta, A.K.

    2017-01-01

    Graphite finds widespread use in nuclear reactors as moderator, reflector, and fuel fabricating components because of its thermal stability and integrity. The manufacturing process consists of various mixing, moulding and baking operations followed by heat-treatment between 2500 °C and 3000 °C. The high temperature treatment is required to drive the amorphous carbon-to-graphite phase transformation. Since synthetic graphite is processed at high temperature, impurity concentrations in the precursor carbon get significantly reduced due to volatilization. However boron may might partly gets converted into boron carbide at high temperatures in the carbon environment of graphite and remains stable (B_4C: boiling point 3500 °C) in the matrix. Literature survey reveals the use of various methods for determination of boron. Previously we have developed a method for determination of boron in graphite electrodes using inductively coupled plasma mass spectrometry (ICP-MS). The method involves removal of graphite matrix by ignition of the sample at 800°C in presence of saturated barium hydroxide solution to prevent the loss of boron. Here we are reporting a modification in the method by using calcium carbonate in place of barium hydroxide and using beryllium (Be) as an internal standard, which resulted in a better precession. The method was validated by spike recovery experiments as well as using another technique viz. Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The modified method was applied in evaluation of boron concentration in the graphite reference material prepared

  2. Risk assessment using ICP-MS of heavy metals in groundwater in Upper Egypt

    Directory of Open Access Journals (Sweden)

    Ghada Bassioni

    2015-09-01

    Full Text Available It is of great importance to assess the pollution of groundwater as it makes up about twenty percent of the world’s freshwater supply. Environmental laws in Egypt are correlated with protecting water resources from contamination and generally set the maximum limits for the concentration of different hazardous components in wastewater before it is discharged to sea water, rivers, groundwater and the public sewer system. Groundwater from Samalout, Al Minya governorate, Egypt, is studied by analysing its heavy metal content using Inductively Coupled Plasma Mass Spectrometry (ICP-MS. Furthermore, the obtained heavy metal concentrations are compared with permissible limits set by environmental organizations such as the World Health Organization (WHO and the United States Environmental Protection Agency (US-EPA. Comparing the heavy metal concentrations with the groundwater in question clearly demonstrated that the water in this resource should not be directly used for drinking and requires some degree of treatment before usage. For example, concentrations of chromium and lead are far above the maximum permissible limit. The consequent health risks due to the usage of contaminated water are identified in this study as well.

  3. Biomonitoring of selenoprotein P in human serum by fast affinity chromatography coupled to ICP-MS.

    Science.gov (United States)

    Heitland, Peter; Köster, Helmut D

    2018-04-01

    Most of the Se in human serum is bound to selenoprotein P (SEPP1) in which Se is present in form of selenocysteine. The SEPP1 is a new possible biomarker for the Se status and for this reason we developed a fast, simple and reliable method for the quantitative determination of SEPP1 in serum by affinity chromatography coupled to ICP-MS. It is possible to separate SEPP1 from other selenoproteins in serum in only 5 min, which allows high sample throughput in clinical laboratories. Measured and certified concentrations of total Se and Se(SEPP1) are in good agreement for the reference material SRM 1950. The SEPP1 concentration was stable in serum samples of 3 persons for a minimum of 2 weeks. Further results of method validation were described including internal and external quality assurance. The analytical method was applied for a biomonitoring study of the SEPP1 and total Se concentration in human serum of 50 occupationally non-exposed persons living in northern Germany. Concentration ranges and mean concentrations for Se(SEPP1) are 31.1-59.7 and 46.2 μg/L, respectively. The corresponding values for total Se are 62-120 and 83.5 μg/L. The mean percentage of total Se in serum present as SEPP1 is 58%. Copyright © 2018 Elsevier GmbH. All rights reserved.

  4. Estimation of differences in trace element composition of Bulgarian summer fruits using ICP-MS

    Directory of Open Access Journals (Sweden)

    G. Toncheva

    2016-06-01

    Full Text Available Abstract. The content of potentially essential and toxic elements: chromium, manganese, iron, copper, nickel, cadmium and arsenic in Bulgarian fruits such as aronia, morello, cherry, raspberry, nectarine peach, apple type „akane” and pear type „early gold” were investigated. By using the ICP-MS we found that -1 -1 -1 raspberry has the highest content of iron (4635.9 ± 53.2 μg kg , manganese (5690.9 ± 31.7 μg kg and chromium (150.2 ± 2.5 μg kg , while the richest in -1 copper is the nectarine (887.5 ± 31.19 μg kg . The content of toxic elements (nickel, cadmium and arsenic is in amount significantly below the permissible standards. Single ANOVA and subsequent Dunkan's test were used to define the fruit and to estimate the significance of chemical elements. The test for multidirectional comparisons indicated that for five of the investigated seven elements: iron, copper, nickel, cadmium, and arsenic the fruits are statistically distinguishable According to hierarchical cluster analysis the fruits are into one cluster.

  5. Improved analytical techniques of sulfur isotopic composition in nanomole quantities by MC-ICP-MS.

    Science.gov (United States)

    Yu, Tsai-Luen; Wang, Bo-Shian; Shen, Chuan-Chou; Wang, Pei-Ling; Yang, Tsanyao Frank; Burr, George S; Chen, Yue-Gau

    2017-10-02

    We propose an improved method for precise sulfur isotopic measurements by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) in conjunction with a membrane desolvation nebulization system. The problems of sulfur loss through the membrane desolvation apparatus are carefully quantified and resolved. The method overcomes low intrinsic sulfur transmission through the instrument, which was initially 1% when operating at a desolvation temperature of 160 °C. Sulfur loss through the membrane desolvation apparatus was resolved by doping with sodium. A Na/S ratio of 2 mol mol -1 produced sulfur transmissions with 98% recovery. Samples of 3 nmol (100 ng) sulfur achieved an external precision of ±0.18‰ (2 SD) for δ 34 S and ±0.10‰ (2 SD) for Δ 33 S (uppercase delta expresses the extent of mass-independent isotopic fractionation). Measurements made on certified reference materials and in-house standards demonstrate analytical accuracy and reproducibility. We applied the method to examine microbial-induced sulfur transformation in marine sediment pore waters from the sulfate-methane transition zone. The technique is quite versatile, and can be applied to a range of materials, including natural waters and minerals. Copyright © 2017 Elsevier B.V. All rights reserved.

  6. Determination of rare earth elements in red mud by ICP-MS

    International Nuclear Information System (INIS)

    Kumar, Sanjukta A.; Suvarna, S.; Kiran Kumar, G.

    2017-01-01

    Red mud or red sludge is a highly alkaline waste product composed mainly of iron oxide that is generated in the industrial production of aluminum from bauxite. With about 77 million tons of this hazardous material being produced annually, red mud poses a serious disposal problem in the mining industry. Discharge of red mud is hazardous environmentally because of its alkalinity. Many studies have been conducted to develop uses of red mud. An estimated 2 to 3 million tones are used annually in the production of cement, road construction and as a source for iron. Potential applications include the production of low cost concrete, application to sandy soils to improve phosphorus cycling, amelioration of soil acidity, landfill capping and carbon sequestration. Red mud contains a large amount of iron along with appreciable concentrations of many strategic elements such as rare earth elements and therefore can be a source of valuable secondary raw material. This necessitates the elemental characterization of red mud. This paper presents an effective dissolution procedure using a mixture of phosphoric acid and nitric acid for red mud followed by determination of rare earth elements by ICP-MS. The method was validated by spike recovery experiments. The recoveries were found within 98 to 102 %. The relative standard deviation (RSD) of the method was found to be within 5 %

  7. Depth Profiling (ICP-MS Study of Toxic Metal Buildup in Concrete Matrices: Potential Environmental Impact

    Directory of Open Access Journals (Sweden)

    Ghada Bassioni

    2010-10-01

    Full Text Available This paper explores the potential of concrete material to accumulate toxic trace elements using ablative laser technology (ICP-MS. Concrete existing in offshore structures submerged in seawater acts as a sink for hazardous metals, which could be gradually released into the ocean creating pollution and anoxic conditions for marine life. Ablative laser technology is a valuable tool for depth profiling concrete to evaluate the distribution of toxic metals and locate internal areas where such metals accumulate. Upon rapid degradation of concrete these “hotspots” could be suddenly released, thus posing a distinct threat to aquatic life. Our work simulated offshore drilling conditions by immersing concrete blocks in seawater and investigating accumulated toxic trace metals (As, Be, Cd, Hg, Os, Pb in cored samples by laser ablation. The experimental results showed distinct inhomogeneity in metal distribution. The data suggest that conditions within the concrete structure are favorable for random metal accumulation at certain points. The exact mechanism for this behavior is not clear at this stage and has considerable scope for extended research including modeling and remedial studies.

  8. Reversed Phase Column HPLC-ICP-MS Conditions for Arsenic Speciation Analysis of Rice Flour.

    Science.gov (United States)

    Narukawa, Tomohiro; Matsumoto, Eri; Nishimura, Tsutomu; Hioki, Akiharu

    2015-01-01

    New measurement conditions for arsenic speciation analysis of rice flour were developed using HPLC-ICP-MS equipped with a reversed phase ODS column. Eight arsenic species, namely, arsenite [As(III)], arsenate [As(V)], monomethylarsonic acid (MMAA), dimethylarsinic acid (DMAA), trimethylarsine oxide (TMAO), tetramethylarsonium (TeMA), arsenobetaine (AsB) and arsenocholine (AsC), were separated and determined under the proposed conditions. In particular, As(III) and MMAA and DMAA and AsB were completely separated using a newly proposed eluent containing ammonium dihydrogen phosphate. Importantly, the sensitivity changes, in particular those of As(V) and As(III) caused by coexisting elements and by complex matrix composition, which had been problematical in previously reported methods, were eliminated. The new eluent can be applied to C8, C18 and C30 ODS columns with the same effectiveness and with excellent repeatability. The proposed analytical method was successfully applied to extracts of rice flour certified reference materials.

  9. Total Arsenic, Cadmium, and Lead Determination in Brazilian Rice Samples Using ICP-MS.

    Science.gov (United States)

    Mataveli, Lidiane Raquel Verola; Buzzo, Márcia Liane; de Arauz, Luciana Juncioni; Carvalho, Maria de Fátima Henriques; Arakaki, Edna Emy Kumagai; Matsuzaki, Richard; Tiglea, Paulo

    2016-01-01

    This study is aimed at investigating a suitable method for rice sample preparation as well as validating and applying the method for monitoring the concentration of total arsenic, cadmium, and lead in rice by using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Various rice sample preparation procedures were evaluated. The analytical method was validated by measuring several parameters including limit of detection (LOD), limit of quantification (LOQ), linearity, relative bias, and repeatability. Regarding the sample preparation, recoveries of spiked samples were within the acceptable range from 89.3 to 98.2% for muffle furnace, 94.2 to 103.3% for heating block, 81.0 to 115.0% for hot plate, and 92.8 to 108.2% for microwave. Validation parameters showed that the method fits for its purpose, being the total arsenic, cadmium, and lead within the Brazilian Legislation limits. The method was applied for analyzing 37 rice samples (including polished, brown, and parboiled), consumed by the Brazilian population. The total arsenic, cadmium, and lead contents were lower than the established legislative values, except for total arsenic in one brown rice sample. This study indicated the need to establish monitoring programs for emphasizing the study on this type of cereal, aiming at promoting the Public Health.

  10. Total Arsenic, Cadmium, and Lead Determination in Brazilian Rice Samples Using ICP-MS

    Directory of Open Access Journals (Sweden)

    Lidiane Raquel Verola Mataveli

    2016-01-01

    Full Text Available This study is aimed at investigating a suitable method for rice sample preparation as well as validating and applying the method for monitoring the concentration of total arsenic, cadmium, and lead in rice by using Inductively Coupled Plasma Mass Spectrometry (ICP-MS. Various rice sample preparation procedures were evaluated. The analytical method was validated by measuring several parameters including limit of detection (LOD, limit of quantification (LOQ, linearity, relative bias, and repeatability. Regarding the sample preparation, recoveries of spiked samples were within the acceptable range from 89.3 to 98.2% for muffle furnace, 94.2 to 103.3% for heating block, 81.0 to 115.0% for hot plate, and 92.8 to 108.2% for microwave. Validation parameters showed that the method fits for its purpose, being the total arsenic, cadmium, and lead within the Brazilian Legislation limits. The method was applied for analyzing 37 rice samples (including polished, brown, and parboiled, consumed by the Brazilian population. The total arsenic, cadmium, and lead contents were lower than the established legislative values, except for total arsenic in one brown rice sample. This study indicated the need to establish monitoring programs for emphasizing the study on this type of cereal, aiming at promoting the Public Health.

  11. Identification and quantification of metallothionein isoforms and superoxide dismutase in spiked liver extracts using HPLC-ESI-MS offline coupling and HPLC-ICP-MS online coupling.

    Science.gov (United States)

    Nischwitz, V; Michalke, B; Kettrup, A

    2003-01-01

    A two-dimensional chromatographic method for the characterization of metallothionein isoforms (MT) and superoxide dismutase (SOD) in spiked liver extracts was developed for the optimization of extraction procedures from liver samples. Element-specific detection (ICP-MS) and molecule-specific detection (ESI-MS) were applied for maximum species information. A special focus was laid on the quantitative data evaluation (species stoichiometry, calibration with and without matrix, recovery), which is neglected in most MT/SOD publications with hyphenated techniques. Linearity, precision (residual standard deviation of calibration curves <10%), and detection limits (<0.6 mg L(-1) for MT isoforms and 13 mg L(-1) for SOD) prove the suitability of the method for quantification. An alternative quantification is proposed for the extension towards other lesser or even unknown trace element species, especially the native porcine MT and SOD.

  12. Single particle analysis of TiO2 in candy products using triple quadrupole ICP-MS.

    Science.gov (United States)

    Candás-Zapico, S; Kutscher, D J; Montes-Bayón, M; Bettmer, J

    2018-04-01

    Titanium dioxide (TiO 2 ) belongs to the materials that have gained great importance in many applications. In its particulate form (micro- or nanoparticles), it has entered a huge number of consumer products and food-grade TiO 2 , better known as E171 within the European Union, represents an important food additive. Thus, there is an increasing need for analytical methods able to detect and quantify such particles. In this regard, inductively coupled-mass spectrometry (ICP-MS), in particular single particle ICP-MS (spICP-MS), has gained importance due to its simplicity and ease of use. Nevertheless, the number of applications for Ti nanoparticles is rather limited. In this study, we have applied the spICP-MS strategy by comparing different measuring modes available in triple quadrupole ICP-MS. First, single quadrupole mode using the collision/reaction cell system was selected for monitoring the isotope 47 Ti. Different cell gases like He, O 2 and NH 3 were tested under optimised conditions for its applicability in spICP-MS of standard suspensions of TiO 2 . The determined analytical figures of merit were compared to those obtained by triple quadrupole mode using the 47 Ti or 48 Ti reaction products using O 2 and NH 3 as reaction gases. This comparison demonstrated that the triple quadrupole mode (TQ mode) was superior in terms of sensitivity due to the more efficient removal of spectral interferences. Particle size detection limits down to 26nm were obtained using the best instrumental conditions for TiO 2 particles at a dwell time of 10ms. Finally, the different measuring modes were applied to the analysis of chewing gum samples after a simple extraction procedure using an ultrasonic bath. The obtained results showed a good agreement for the detected particle size range using the different TQ modes. The size range of TiO 2 particles was determined to be between approximately 30 and 200nm, whereas roughly 40% of the particles were smaller than 100nm. For the

  13. Characterization of Nanomaterials Using Field Flow Fractionation and Single Particle Inductively Coupled Plasma Mass Spectrometery (FFF-ICP-MS and SP-ICP-MS): Scientific Operating Procedure SOP-C

    Science.gov (United States)

    2015-04-01

    constituents of Cadmium Selenide/Zinc Sulfide core-shell quantum dots, silver nanoparticles with gold seed cores, and gold nanoparticles. Additionally...nanoparticles from tissues is possible using tetramethylammonium hydroxide (TMAH). Though any analysis described above is possible, only SP-ICP-MS has been...ENPs), through the various separation and detection techniques described above. These analytical tools were tested on a variety of gold and silver

  14. Methodology for determination of trace elements in mineral phases of iron banded formation by LA-ICP-MS; Metodologia de determinacao de elementos-traco em fases minerais de formacoes ferriferas bandadas por LA-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Sousa, Denise V.M. de; Nalini Junior, Herminio A.; Sampaio, Geraldo M.S.; Abreu, Adriana T. de; Lana, Cristiano de C., E-mail: deniseversiane2@yahoo.com.br, E-mail: nalini@degeo.ufop.br, E-mail: geraldomssampaio@gmail.com, E-mail: adrianatropia@gmail.com, E-mail: cristianodeclana@gmail.com [Universidade Federal de Ouro Preto (DEGEO/UFOP), Ouro Preto, MG (Brazil). Departamento de Geologia

    2015-07-01

    The study of the chemical composition of mineral phases of iron formation (FF), especially of trace elements, is an important tool in the understanding of the genesis of these rocks and the contribution of the phases in the composition of whole rock. Low mass fraction of such elements in the mineral phases present in this rock type requires a suitable analytical procedure. The laser ablation technique coupled with ICP-MS (LA-ICP-MS) has been widely used for determination of trace elements in geological samples. Thus, the aim of this study is to develop calibration curves for determination of trace elements (Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in mineral phases of banded iron formations by LA-ICP-MS. Several certified reference materials (CRM) were used for calibrate the equipment. The analytical conditions were checked by CRM NIST SRM 614. The results were satisfactory, since the curves showed good linearity coefficients, good accuracy and precision of results. (author)

  15. Comparison of standard and reaction cell inductively coupled plasma mass spectrometry in the determination of chromium and selenium species by HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Bednar, A.J.; Kirgan, R.A.; Jones, W.T.

    2009-01-01

    Elemental speciation is becoming a common analytical procedure for geochemical investigations. The various redox species of environmentally relevant metals can have vastly different biogeochemical properties, including sorption, solubility, bioavailability, and toxicity. The use of high performance liquid chromatography (HPLC) coupled to elemental specific detectors, such as inductively coupled plasma mass spectrometry (ICP-MS), has become one of the most important speciation methods employed. This is due to the separation versatility of HPLC and the sensitive and selective detection capabilities of ICP-MS. The current study compares standard mode ICP-MS to recently developed reaction cell (RC) ICP-MS, which has the ability to remove or reduce many common polyatomic interferences that can limit the ability of ICP-MS to quantitate certain analytes in complex matrices. Determination of chromium and selenium redox species is achieved using ion-exchange chromatography with elemental detection by standard and RC-ICP-MS, using various chromium and selenium isotopes. In this study, method performance and detection limits for the various permutations of the method (isotope monitored or ICP-MS detection mode) were found to be comparable and generally less than 1 μg L -1 . The method was tested on synthetic laboratory samples, surface water, groundwater, and municipal tap water matrices

  16. Analysis of marine samples by neutron-induced prompt gamma-ray technique and ICP-MS

    International Nuclear Information System (INIS)

    Yonezawa, C.; Matsue, H.; McKay, K.; Povinec, P.

    2001-01-01

    Multi-element and isotopic analyses of oils and marine environmental samples were carried out to estimate a contamination source using a 'finger printing' method. Elemental analyses were carried out using neutron-induced prompt gamma-ray analysis (PGA), instrumental neutron activation analysis (INAA) at the Japan Atomic Institute, Tokai-mura, Japan (JAERI) and ICP-MS in the IAEA Marine Environment Laboratory, Monaco (MEL). Fifteen elements including light elements, H, B, N, Si and Ca, which cannot be determined by INAA and ICP-MS, were determined by PGA. A total of 47 elements were determined in the present study. The potential of PGA for the determination of isotopic ratios was tested by measuring 34 S/ 32 S ratios in oils. The evaluation of historical records of marine environmental conditions using annual bands in coral samples was also investigated. (author)

  17. Method validation for determination of heavy metals in wine and slightly alcoholic beverages by ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Voica, Cezara; Dehelean, Adriana; Pamula, A, E-mail: cezara.voica@itim-cj.r [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania)

    2009-08-01

    The Organisation International de la Vigne et du Vin (OIV) fixed an uppermost level for some heavy metals in wine. Consequently, the need to determine very low concentration of elements that may be present in wine in trace and ultra trace levels occurred. Inductively coupled plasma mass spectrometry ICP-MS is considered an excellent tool for detailed characterization of the elementary composition of many samples, including samples of drinks. In this study a method of quantitative analysis for the determination of toxic metals (Cr, As, Cd, Ni, Hg, Pb) in wines and slightly alcoholic beverages by ICP-MS was validated. Several parameters have been taken into account and evaluated for the validation of method, namely: linearity, the minimum detection limit, the limit of quantification, accuracy and uncertainty.

  18. Method validation for determination of heavy metals in wine and slightly alcoholic beverages by ICP-MS

    International Nuclear Information System (INIS)

    Voica, Cezara; Dehelean, Adriana; Pamula, A

    2009-01-01

    The Organisation International de la Vigne et du Vin (OIV) fixed an uppermost level for some heavy metals in wine. Consequently, the need to determine very low concentration of elements that may be present in wine in trace and ultra trace levels occurred. Inductively coupled plasma mass spectrometry ICP-MS is considered an excellent tool for detailed characterization of the elementary composition of many samples, including samples of drinks. In this study a method of quantitative analysis for the determination of toxic metals (Cr, As, Cd, Ni, Hg, Pb) in wines and slightly alcoholic beverages by ICP-MS was validated. Several parameters have been taken into account and evaluated for the validation of method, namely: linearity, the minimum detection limit, the limit of quantification, accuracy and uncertainty.

  19. A method for the measurement of 99Tc by quadrupole ICP-MS in dry fallout and sea grass samples

    International Nuclear Information System (INIS)

    Mas, Jose Luis; Bolivar, Juan Pedro; Garcia-Leon, Manuel

    2003-01-01

    A method for the detection of 99 Tc by ICP-MS in environmental samples is proposed and explained in detail. This method combines the capabilities of anion exchange chromatographic TEVA·Spec TM resin with prior isotope concentration using solvent extraction to Tributylphosphate. The problem that the excess of Mo in the solution analyzed by ICP-MS causes in the instrumental response at m/z ratio 99 is described in detail, and the proposed solution takes the form of the referred radiochemical method. The realistic limits of detection of this technique (bearing in mind the particular methodology here applied) are in the range of 20-70 mBq/kg when treating mass amounts in the range of 20-125 g dry weight. A few environmental samples proceeding from a region unaffected by any closer nuclear industry (the Southwest of Spain) are analyzed for checking 99 Tc concentration. (author)

  20. High accuracy determination of trace elements in NIST standard reference materials by isotope dilution ICP-MS

    International Nuclear Information System (INIS)

    Paulsen, P.J.; Beary, E.S.

    1996-01-01

    At NIST (National Institute of Standards and Technology), ICP-MS ID (inductively coupled mass spectrometry isotope dilution) has been used to certify a wide range of elements in a variety of materials with high accuracy. Both the chemical preparation and instrumental procedures are simpler than with other ID mass spectrometric techniques. The ICP-MS has picogram/ml detection limits for most elements using fixed operating parameters. Chemical separations are required only to remove an interference (from molecular ions as well as isobaric atoms), or to pre-concentrate the analyte. For example, chemical separations were required for the analysis of SRM 2711, Montana II Soil, but not for boron in peach leaves, SRM 1547.(3 refs., 3 tabs., 2 figs

  1. Simultaneous determination of metal traces by ICP-MS in environmental waters using SPE preconcentration on different polymeric sorbents

    Czech Academy of Sciences Publication Activity Database

    Holubova, Z.; Moos, Martin; Sommer, L.

    2012-01-01

    Roč. 65, č. 10 (2012), s. 899-906 ISSN 0366-6352 R&D Projects: GA MŠk(CZ) ED1.1.00/02.0073 Institutional support: RVO:67179843 Keywords : solid phase extraction * Amberlite XAD-16 * Amberlite SDB-L * ICP-MS * industrial waters * metal contaminants Subject RIV: EH - Ecology, Behaviour Impact factor: 0.879, year: 2012

  2. Multianalytical determination of trace elements in atmospheric biomonitors by k0-INAA, ICP-MS and AAS

    Science.gov (United States)

    Freitas, M. C.; Pacheco, A. M. G.; Dionísio, I.; Sarmento, S.; Baptista, M. S.; Vasconcelos, M. T. S. D.; Cabral, J. P.

    2006-08-01

    Elemental contents of atmospheric biomonitors—epiphytic lichens and tree bark, exposed in continuous and discontinuous modes—have been assessed through k0-standardised instrumental neutron activation analysis ( k0-INAA) (two different institutions), inductively coupled plasma mass spectrometry (ICP-MS) and atomic absorption spectrometry (AAS). Certified reference materials—ISE-921 (river clay), NIST-1547 (peach leaves), ICHTJ-INCT-TL-1 (tea leaves; TL-1 hereinafter) and IAEA-336 (lichen material), and nonparametric statistics—rank-order correlations (Spearman RS) and enhanced-sign tests (Wilcoxon T)—were used for analytical control and data comparison, respectively. In general, quality of procedures was deemed good, except for k0-INAA in determining Br, Cu and Na, all likely affected by high counting statistics, and/or contamination issues (the latter). Results for Cu, Ni, Pb and Sr (by both ICP-MS and AAS) revealed that, despite an outstanding correlation (asymptotic p=0.000), they could be viewed as statistically equal for Cu only: AAS tended to yield higher values for Pb and Ni, and lower ones for Sr. The comparison between ICP-MS and k0-INAA data from TUDelft, for Al, Ca, Cu, Mg, Mn, Na, Ti and V, showed an excellent correlation (as above) and random (relative) magnitude for Cu, Mg, Mn and Ti only: ICP-MS tended to yield higher values for Al, Na and V, and lower ones for Ca, whereas between k0-INAA data from TUDelft and ITN, for Br, Ca and Na, resulted in systematically higher [Br] and [Ca] variates from TUDelft, even if all corresponding data sets were found to correlate at stringent significance levels. In a few cases, though—Ca, Sr in lichens; Pb in bark—matrix effects did appear to interfere in the outcome of matched-pairs, signed-rank tests, since random hierarchy of variates could be asserted just when lichen and bark data sets were processed separately.

  3. Simultaneous quantification of iodine and high valent metals via ICP-MS under acidic conditions in complex matrices.

    Science.gov (United States)

    Brix, Kristina; Hein, Christina; Sander, Jonas Michael; Kautenburger, Ralf

    2017-05-15

    The determination of iodine as a main fission product (especially the isotopes I-129 and I-131) of stored HLW in a disposal beside its distribution as a natural ingredient of many different products like milk, food and seawater is a matter of particular interest. The simultaneous ICP-MS determination of iodine as iodide together with other elements (especially higher valent metal ions) relevant for HLW is analytically very problematic. A reliable ICP-MS quantification of iodide must be performed at neutral or alkaline conditions in contrast to the analysis of metal ions which are determined in acidic pH ranges. Herein, we present a method to solve this problem by changing the iodine speciation resulting in an ICP-MS determination of iodide as iodate. The oxidation from iodide to iodate with sodium hypochlorite at room temperature is a fast and convenient method with flexible reaction time, from one hour up to three days, thus eliminating the disadvantages of quantifying iodine species via ICP-MS. In the analysed concentration range of iodine (0.1-100µgL -1 ) we obtain likely quantitative recovery rates for iodine between 91% and 102% as well as relatively low RSD values (0.3-4.0%). As an additional result, it is possible to measure different other element species in parallel together with the generated iodate, even high valent metals (europium and uranium beside caesium) at recovery rates in the same order of magnitude (93-104%). In addition, the oxidation process operates above pH 7 thus offering a wide pH range for sample preparation. Even analytes in complex matrices, like 5M saline (NaCl) solution or artificial cement pore water (ACW) can be quantified with this robust sample preparation method. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Comparison of elemental quantity by PIXE and ICP-MS and/or ICP-AES for NIST standards

    International Nuclear Information System (INIS)

    Saitoh, K.; Sera, K.; Gotoh, T.; Nakamura, M.

    2002-01-01

    Urban particulate matter (SRM 1648), Buffalo River sediment (SRM 2704) and pine needle (SRM 1575) standard reference materials prepared by the National Institute of Standards and Technology (NIST, USA) were analyzed by three multi-element analysis methods, i.e., particle induced X-ray emission (PIXE), inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES); values determined by those analysis methods were compared with certified and/or non-certified values of NIST samples. Values determined by PIXE were 70-120% relative to certified and/or non-certified values of NIST samples except for Co in the urban particulate matter, for V and Co in Buffalo River sediment and for Ni and Br in the pine needles samples. In particular, Al, K, Ca, Cr, Mn, Fe, Cu, Zn and Pb were 85-110% in all samples. On the other hand, Na and Fe values determined by ICP-MS were very much different from the certified values in all samples, but the other elements were 70-120%. As for ICP-AES, all elements except for Na were 80-100% in all samples. Comparing the values determined by PIXE and those determined by ICP-MS and/or ICP-AES, there was a slight difference between the samples, but the range was 75-120% except for Na, V, Fe and Co determined by ICP-MS and Na determined by ICP-AES, which was generally consistent with PIXE

  5. Bioimaging of metallothioneins in ocular tissue sections by laser ablation-ICP-MS using bioconjugated gold nanoclusters as specific tags.

    Science.gov (United States)

    Cruz-Alonso, María; Fernandez, Beatriz; Álvarez, Lydia; González-Iglesias, Héctor; Traub, Heike; Jakubowski, Norbert; Pereiro, Rosario

    2017-12-18

    An immunohistochemical method is described to visualize the distribution of metallothioneins 1/2 (MT 1/2) and metallothionein 3 (MT 3) in human ocular tissue. It is making use of (a) antibodies conjugated to gold nanoclusters (AuNCs) acting as labels, and (b) laser ablation (LA) coupled to inductively coupled plasma - mass spectrometry (ICP-MS). Water-soluble fluorescent AuNCs (with an average size of 2.7 nm) were synthesized and then conjugated to antibody by carbodiimide coupling. The surface of the modified AuNCs was then blocked with hydroxylamine to avoid nonspecific interactions with biological tissue. Immunoassays for MT 1/2 and MT 3 in ocular tissue sections (5 μm thick) from two post mortem human donors were performed. Imaging studies were then performed by fluorescence using confocal microscopy, and LA-ICP-MS was performed in the retina to measure the signal for gold. Signal amplification by the >500 gold atoms in each nanocluster allowed the antigens (MT 1/2 and MT 3) to be imaged by LA-ICP-MS using a laser spot size as small as 4 μm. The image patterns found in retina are in good agreement with those obtained by conventional fluorescence immunohistochemistry which was used as an established reference method. Graphical abstract Gold nanoclusters (AuNCs) conjugated to a primary specific antibody serve as a label for amplified bioimaging of metallothioneins (MTs) by laser ablation coupled to inductively coupled plasma - mass spectrometry (ICP-MS) in human ocular tissue sections.

  6. Advanced functional materials in solid phase extraction for ICP-MS determination of trace elements and their species - A review.

    Science.gov (United States)

    He, Man; Huang, Lijin; Zhao, Bingshan; Chen, Beibei; Hu, Bin

    2017-06-22

    For the determination of trace elements and their species in various real samples by inductively coupled plasma mass spectrometry (ICP-MS), solid phase extraction (SPE) is a commonly used sample pretreatment technique to remove complex matrix, pre-concentrate target analytes and make the samples suitable for subsequent sample introduction and measurements. The sensitivity, selectivity/anti-interference ability, sample throughput and application potential of the methodology of SPE-ICP-MS are greatly dependent on SPE adsorbents. This article presents a general overview of the use of advanced functional materials (AFMs) in SPE for ICP-MS determination of trace elements and their species in the past decade. Herein the AFMs refer to the materials featuring with high adsorption capacity, good selectivity, fast adsorption/desorption dynamics and satisfying special requirements in real sample analysis, including nanometer-sized materials, porous materials, ion imprinting polymers, restricted access materials and magnetic materials. Carbon/silica/metal/metal oxide nanometer-sized adsorbents with high surface area and plenty of adsorption sites exhibit high adsorption capacity, and porous adsorbents would provide more adsorption sites and faster adsorption dynamics. The selectivity of the materials for target elements/species can be improved by using physical/chemical modification, ion imprinting and restricted accessed technique. Magnetic adsorbents in conventional batch operation offer unique magnetic response and high surface area-volume ratio which provide a very easy phase separation, greater extraction capacity and efficiency over conventional adsorbents, and chip-based magnetic SPE provides a versatile platform for special requirement (e.g. cell analysis). The performance of these adsorbents for the determination of trace elements and their species in different matrices by ICP-MS is discussed in detail, along with perspectives and possible challenges in the future

  7. Comparison study of RNAA and ICP-MS for the determination of ultra-traces of Th and U in geological and cosmochemical samples

    International Nuclear Information System (INIS)

    Chai, J.; Oura, Y.; Ebihara, M.

    2003-01-01

    In order to determine thorium and uranium traces in geochemical and cosmochemical samples, we developed an ICP-MS procedure, in which an anion-exchange step was introduced after sample digestion to separate major matrix elements, leading to decrease the dilution factor and increase the sensitivity for Th and U. The ICP-MS procedure was compared to the RNAA procedure which we recently developed for the same purpose. Both ICP-MS and RNAA procedures developed were found to yield similar detection limits (sub ppb) for Th and U. (author)

  8. Evaluation of the combined measurement uncertainty in isotope dilution by MC-ICP-MS

    International Nuclear Information System (INIS)

    Fortunato, G.; Wunderli, S.

    2003-01-01

    The combination of metrological weighing, the measurement of isotope amount ratios by a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS) and the use of high-purity reference materials are the cornerstones to achieve improved results for the amount content of lead in wine by the reversed isotope dilution technique. Isotope dilution mass spectrometry (IDMS) and reversed IDMS have the potential to be a so-called primary method, with which close comparability and well-stated combined measurement uncertainties can be obtained. This work describes the detailed uncertainty budget determination using the ISO-GUM approach. The traces of lead in wine were separated from the matrix by ion exchange chromatography after HNO 3 /H 2 O 2 microwave digestion. The thallium isotope amount ratio (n( 205 Tl)/n( 203 Tl)) was used to correct for mass discrimination using an exponential model approach. The corrected lead isotope amount ratio n( 206 Pb)/n( 208 Pb) for the isotopic standard SRM 981 measured in our laboratory was compared with ratio values considered to be the least uncertain. The result has been compared in a so-called pilot study ''lead in wine'' organised by the CCQM (Comite Consultatif pour la Quantite de Matiere, BIPM, Paris; the highest measurement authority for analytical chemical measurements). The result for the lead amount content k(Pb) and the corresponding expanded uncertainty U given by our laboratory was:k(Pb)=1.329 x 10-10mol g-1 (amount content of lead in wine)U[k(Pb)]=1.0 x 10-12mol g-1 (expanded uncertainty U=k x uc, k=2) The uncertainty of the main influence parameter of the combined measurement uncertainty was determined to be the isotope amount ratio R 206,B of the blend between the enriched spike and the sample. (orig.)

  9. Speciation And Uptake of Arsenic Accumulated By Corn Seedlings Using XAS And DRC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Parsons, J.G.; Martinez-Martinez, A.; Peralta-Videa, J.R.; Gardea-Torresdey, J.L.

    2009-05-21

    ICP-MS was used to investigate the uptake of As(III) and As(V) from hydroponics growth media by corn seedlings. It was found that arsenic uptake by the plant roots for the arsenic(V) and arsenic(III) treatments were 95 and 112 ppm, respectively. However, in the shoots of the arsenic (V) treatments had 18 ppm whereas arsenic(III) treatments had 12 ppm. XANES studies showed that As for both treatments arsenic was present as a mixture of an As(III) sulfur complex and an As(V) oxygen complex. The XANES data was corroborated by the EXAFS studies showing the presence of both oxygen and sulfur ligands coordinated to the arsenic. Iron concentrations were found to increase by 4 fold in the As(V) contaminated growth media and 7 fold in the As(III) treatment compared to the control iron concentration of 500 ppm. Whereas, the total iron concentration in the shoots was found to decrease by approximately the same amount for both treatments from 360 ppm in the control to approximately 125 ppm in both arsenic treatments. Phosphorus concentrations were found to decrease in both the roots and shoots compared to the control plants. The total sulfur in the roots was found to increase in the arsenic(III) and arsenic(V) treatments to 560 ppm and 800 ppm, respectively, compared to the control plants 358 ppm. In addition, the total sulfur in shoots of the plants was found to remain relatively constant at approximately 1080 ppm. The potassium concentrations in the plants were found to increase in the roots and decrease in the shoots.

  10. Multielement analysis of Zanthoxylum bungeanum Maxim. essential oil using ICP-MS/MS.

    Science.gov (United States)

    Fu, Liang; Xie, Hualin; Shi, Shuyun

    2018-04-12

    The concentrations of trace elements (Cr, Ni, As, Cd, Hg, and Pb) in Zanthoxylum bungeanum Maxim. essential oil (ZBMEO) were determined by inductively coupled plasma tandem mass spectrometry. The ZBMEO sample was directly analyzed after simple dilution with n-hexane. Aiming for a relatively high vapor pressure of n-hexane and its resultant loading on plasma, we used a narrow injector torch and optimized plasma radio frequency power and carrier gas flow to ensure stable operation of the plasma. An optional gas flow of 20% O 2 in Ar was added to the carrier gas to prevent the incomplete combustion of highly concentrated organic carbon in plasma and the deposition of carbon on the sampling and skimmer cone orifices. In tandem mass spectrometry mode, O 2 was added to the collision/reaction cell to eliminate the interferences. The limits of detection for Cr, Ni, As, Cd, Hg, and Pb were 2.26, 1.64, 2.02, 1.35, 1.76, and 0.97 ng L -1 , respectively. After determination of 23 ZBMEO samples from different regions in China, we found that the average concentration ranges of trace elements in the 23 ZBMEO samples were 0.72-6.02 ng g -1 , 0.09-2.87 ng g -1 , 0.21-5.84 ng g -1 , 0.16-2.15 ng g -1 , 0.13-0.92 ng g -1 , and 0.17-0.73 ng g -1 for Cr, Ni, As, Cd, Hg, and Pb, respectively. The trace elements in ZBMEO differed significantly when different extraction technologies were used. The study revealed that the contents of the toxic elements As, Cd, Hg, and Pb were extremely low, and hence they are unlikely to pose a health risk following ZBMEO ingestion. Graphical abstract The working mechanism of sample analysis by ICP-MS/MS.

  11. Identification of different generations of albite through microchemical fingerprint by LA-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Amorim, Lucas E.D.; Rios, Francisco J.; Freitas, Monica E.; Palmieri, Helena E.L.; Geraldes, Mauro C.; Matos, Evando C. de, E-mail: ledamorim@cdtn.br, E-mail: javier@cdtn.br, E-mail: monicaef@gmail.com, E-mail: help@cdtn.br, E-mail: geraldes@uerj.br, E-mail: carele@inb.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Universidade Estadual do Rio de Janeiro (UERJ), Rio de Janeiro, RJ (Brazil); Indústrias Nucleares do Brasil (INB), Caetité, BA (Brazil)

    2017-07-01

    The Lagoa Real Uranium Province located in the south-central part of the Bahia-BR, in the central portion of the San Francisco Craton, is composed of an association of Paleoproterozoic metagranitoids, alkali-gneisses, and albitites (barren and mineralized). Intense action of metamorphic and metasomatic processes characterize this region. These processes culminated in the transformation of granites into gneisses, albitites and U mineralization in some albitites bodies. There are three types of metagranites, Lagoa do Barro (1,77Ga), Juazerinho (1,75Ga) and São Timóteo (1,74Ga). In view of this information, we aimed to verify if the albite formed by metamorphism in the metagranites has the same fingerprint of the albite present in the barren albitites. We used a LA-ICP-MS system for this. The results allowed the determination of albites fingerprint, allowing the differentiation of at least two generations. The Sr / U ratio allows characterizing these generations. The albitites have albite with minimal microchemical variation. The metagranites Lagoa do Barro and São Timóteo has similar generation of albite. The Juazerinho presents two generations of albite, one with similar to São Timóteo, Lagoa do Barro and albitites and another generation with distinctly higher concentrations of Sr and U. These results show that the same event that generated the albitite's albite interfered with the formation of the metagranite's albite, but another event culminated with the formation of the second generation of the albite in the Juazerinho. (author)

  12. [Analysis of Arsenic Compounds in Blood and Urine by HPLC-ICP-MS].

    Science.gov (United States)

    Lin, L; Zhang, S J; Xu, W C; Luo, R X; Ma, D; Shen, M

    2018-02-01

    To establish an analysis method for the detection of 6 arsenic compounds [AsC, AsB, As(Ⅲ), DMA, MMA and As(V)] in blood and urine by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), and apply it to real cases. Triton was used to damage cells, and then EDTA·2Na·2H2O was used to complex arsenic compounds in cells, and sonication and protein deposition by acetonitrile were performed for sample pretreatment. With the mobile phase consisted of ammonium carbonate and ultrapure water, gradient elution was performed for obtaining the arsenic compounds in samples, which were analysed by ICP-MS with Hamilton PRP-X100 column. The limits of detection in blood were 1.66-10 ng/mL, while the lower limits of quantitation in blood ranged from 5 to 30 ng/mL. The limits of detection in urine were 0.5-10 ng/mL, while the lower limits of quantitation in urine were 5-30 ng/mL. The relative standard deviation of inter-day and intra-day precisions was less than 10%. This method had been successfully applied to 3 cases. This study has established an analysis method for detecting 6 common arsenic compounds in blood and urine, which can be used to detect the arsenic compounds in the blood and urine from arsenic poisoning cases as well as the patients under arsenic treatment. Copyright© by the Editorial Department of Journal of Forensic Medicine.

  13. Identification of different generations of albite through microchemical fingerprint by LA-ICP-MS

    International Nuclear Information System (INIS)

    Amorim, Lucas E.D.; Rios, Francisco J.; Freitas, Monica E.; Palmieri, Helena E.L.; Geraldes, Mauro C.; Matos, Evando C. de

    2017-01-01

    The Lagoa Real Uranium Province located in the south-central part of the Bahia-BR, in the central portion of the San Francisco Craton, is composed of an association of Paleoproterozoic metagranitoids, alkali-gneisses, and albitites (barren and mineralized). Intense action of metamorphic and metasomatic processes characterize this region. These processes culminated in the transformation of granites into gneisses, albitites and U mineralization in some albitites bodies. There are three types of metagranites, Lagoa do Barro (1,77Ga), Juazerinho (1,75Ga) and São Timóteo (1,74Ga). In view of this information, we aimed to verify if the albite formed by metamorphism in the metagranites has the same fingerprint of the albite present in the barren albitites. We used a LA-ICP-MS system for this. The results allowed the determination of albites fingerprint, allowing the differentiation of at least two generations. The Sr / U ratio allows characterizing these generations. The albitites have albite with minimal microchemical variation. The metagranites Lagoa do Barro and São Timóteo has similar generation of albite. The Juazerinho presents two generations of albite, one with similar to São Timóteo, Lagoa do Barro and albitites and another generation with distinctly higher concentrations of Sr and U. These results show that the same event that generated the albitite's albite interfered with the formation of the metagranite's albite, but another event culminated with the formation of the second generation of the albite in the Juazerinho. (author)

  14. Determination of {sup 241}Pu in nuclear waste slurries: A comparative study using LSC and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Jaeggi, M., E-mail: maya.jaeggi@psi.ch [Department Logistics for Radiation Safety and Security, Radioanalytics, CH-5232 Villligen PSI (Switzerland); Roellin, S., E-mail: Stefan.Roellin@babs.admin.ch [Federal Office for Civil Protection, SPIEZ Laboratory, CH-3700 Spiez (Switzerland); Corcho Alvarado, J.A., E-mail: Corcho-Alvarado@chuv.ch [Institute of Radiation Physics, University Hospital and University of Lausanne, Rue du Grand-Pre 1, 1007 Lausanne (Switzerland); Eikenberg, J., E-mail: jost.eikenberg@psi.ch [Department Logistics for Radiation Safety and Security, Radioanalytics, CH-5232 Villligen PSI (Switzerland)

    2012-02-15

    {sup 241}Pu was determined in slurry samples from a nuclear reactor decommissioning project at the Paul Scherrer Institute (Switzerland). To validate the results, the {sup 241}Pu activities of five samples were determined by LSC (TriCarb and Quantulus) and ICP-MS, with each instrument at a different laboratory. In lack of certified reference materials for {sup 241}Pu, the methods were further validated using the {sup 241}Pu information values of two reference sediments (IAEA-300 and IAEA-384). Excellent agreement with the results was found between LSC and ICP-MS in the nuclear waste slurries and the reference sediments. - Highlights: Black-Right-Pointing-Pointer Good agreement between the {sup 241}Pu activity of 5 slurry samples, using 3 measurement techniques. Black-Right-Pointing-Pointer {sup 241}Pu information values of two IAEA samples agreed well for the 3 measurement techniques. Black-Right-Pointing-Pointer Low detection limits were achieved; 1.8 Bq/kg (Quantulus), 2 Bq/kg (ICP-MS) and 3.5 Bq/kg (TriCarb).

  15. Combination of multielement technique (INAA and ICP-MS) for a French air pollution bio-monitoring survey using mosses

    International Nuclear Information System (INIS)

    Ayrault, S.; Deschamps, C.; Amblard, G.; Galsomies, L.; Letrouit-Galinou, M.A.; Bonhomme, P.

    1998-01-01

    This work presents the use of two trace analysis techniques through the data obtained for a significant part of the 557 mosses sampled in France. Sampling were made within the framework of European survey carried out in 1995-1996 and proposed by the Nordic Council. The analyses were produced with a combination of two multielement analysis techniques: INAA (Instrumental Neutron Activation Analysis) and ICP-MS (Inductively Coupled Plasma Mass Spectrometry). Theses two techniques were suitable for trace analyses in mosses. They were clearly complementary and provided for 36 elements including the heavy metals of key interest in air pollution studies. The choice of the technique for a given element depended on the feasibility (e g. Pb is not attainable by INAA), the detection limit, the analytical variability, the preparation procedures and the concentration ranges (5-100 μg/g for Pb, 0.5-5 μg/g for As). INAA measured the total content in the sample, while ICP-MS demanded a mineralization procedure resulting in losses/contamination hazards. Thus, INAA results were preferred, although this technique was time consuming. However the ICP-MS results for Cd, Cu, Ni and Pb were retained, for different reasons: detection limits (Cd, Cu), no convenient INAA conditions (Ni), and feasibility (Pb). (authors)

  16. Development of a procedure for the multi-element determination of trace elements in wine by ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Castineira, M.M.; Brandt, R.; von Bohlen, A.; Jakubowski, N. [Institut fuer Spektrochemie und Angewandte Spektroskopie e.V., Dortmund (Germany)

    2001-07-01

    An inductively coupled plasma mass spectrometric (ICP-MS) procedure has been developed for the determination of trace elements in wine. The procedure consists in simple 1+1 dilution of the wine and semi-quantitative analysis (without external calibration) using In as internal standard. Thirty-one elements at concentrations ranging from 0.1 mg mL{sup -1} to 0.5 ng mL{sup -1} can be determined by ICP-MS analysis with and without digestion. It was investigated whether a matrix effect observed for EtOH in the wine matrix can be overcome by application of a micro-concentric nebulizer with a membrane desolvator (MCN 6000). The results obtained for the MCN 6000 are compared with those obtained by use of a conventional Meinhard nebulizer. It is shown that the observed matrix effect can only be compensated by use of an internal standard for the Meinhard nebulizer, but not for the MCN 6000. Results for ICP-MS are compared with those obtained by total reflection X-ray fluorescence spectrometry (TXRF). (orig.)

  17. Speciation of iodine-containing proteins in Nori seaweed by gel electrophoresis laser ablation ICP-MS.

    Science.gov (United States)

    Romarís-Hortas, V; Bianga, J; Moreda-Piñeiro, A; Bermejo-Barrera, P; Szpunar, J

    2014-09-01

    An analytical approach providing an insight into speciation of iodine in water insoluble fraction of edible seaweed (Nori) was developed. The seaweed, harvested in the Galician coast (Northwestern Spain), contained 67.7±1.3 μg g(-1) iodine of which 25% was water soluble and could be identifies as iodide. Extraction conditions of water insoluble residue using urea, NaOH, SDS and Triton X-100 were investigated. The protein pellets obtained in optimized conditions (after precipitation of urea extracts with acetone), were digested with trypsin and protease XIV. Size exclusion chromatography-ICP-MS of both enzymatic digests demonstrated the occurrence of iodoaminoacids putatively present in proteins. Intact proteins could be separated by gel electrophoresis after an additional extraction of the protein extract with phenol. Sodium dodecyl sulfate polyacrylamide gel electrophoresis (SDS PAGE) with laser ablation ICP-MS detection of (127)I indicated the presence of iodine in protein bands corresponding to molecular masses of 110 kDa, 40 kDa, 27 kDa, 20 kDa and 10 kDa. 2D IEF-SDS PAGE with laser ablation ICP-MS (127)I imaging allowed the detection of 5 iodine containing protein spots in the alkaline pI range. Copyright © 2014 Elsevier B.V. All rights reserved.

  18. Possible interferences of mercury sulfur compounds with ethylated and methylated mercury species using HPLC-ICP-MS

    International Nuclear Information System (INIS)

    Wilken, R.D.; Nitschke, F.; Falter, R.

    2003-01-01

    The HPLC-ICP-MS coupling technique is able to separate and detect methyl, ethyl and inorganic mercury isotopes specifically. An identification of ethyl mercury(+) is not possible when the widely used sodium tetraethylborate derivatisation method in combination with GC-AFS/AAS or ICP-MS techniques is performed because it contains ethyl groups. An unidentified compound with the same retention time as ethyl mercury was found in the HPLC chromatograms of industrial sewage samples and humic-rich soils of microcosm experiments after applying water vapour distillation. We also observed such unidentified peaks in samples of heavily contaminated sites in Eastern Germany, separated by HPLC fractionation only. In the experiments described, different mercury sulfur adducts were synthesised and tested for their retention times in the HPLC-ICP-MS system. It was found that the compound CH 3 -S-Hg + showed the same retention time as the ethyl mercury standard. It is therefore possible that ethyl mercury detected in chromatography by comparison of the retention time could also be due to an adduct of a sulfur compound and a mercury species. CH 3 -S-Hg + should be tested in other chromatographic mercury speciation methods for this effect. This work can also be regarded as a contribution to the discussion of artificially occurring methyl mercury in sediments during sample preparation. (orig.)

  19. Methodology for determination of trace elements in mineral phases of iron banded formation by LA-ICP-MS

    International Nuclear Information System (INIS)

    Sousa, Denise V.M. de; Nalini Junior, Herminio A.; Sampaio, Geraldo M.S.; Abreu, Adriana T. de; Lana, Cristiano de C.

    2015-01-01

    The study of the chemical composition of mineral phases of iron formation (FF), especially of trace elements, is an important tool in the understanding of the genesis of these rocks and the contribution of the phases in the composition of whole rock. Low mass fraction of such elements in the mineral phases present in this rock type requires a suitable analytical procedure. The laser ablation technique coupled with ICP-MS (LA-ICP-MS) has been widely used for determination of trace elements in geological samples. Thus, the aim of this study is to develop calibration curves for determination of trace elements (Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in mineral phases of banded iron formations by LA-ICP-MS. Several certified reference materials (CRM) were used for calibrate the equipment. The analytical conditions were checked by CRM NIST SRM 614. The results were satisfactory, since the curves showed good linearity coefficients, good accuracy and precision of results. (author)

  20. Detection of transgenerational barium dual-isotope marks in salmon otoliths by means of LA-ICP-MS.

    Science.gov (United States)

    Huelga-Suarez, Gonzalo; Fernández, Beatriz; Moldovan, Mariella; García Alonso, J Ignacio

    2013-03-01

    The present study evaluates the use of an individual-specific transgenerational barium dual-isotope procedure and its application to salmon specimens from the Sella River (Asturias, Spain). For such a purpose, the use of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) in combination with multiple linear regression for the determination of the isotopic mark in the otoliths of the specimens is presented. In this sense, a solution in which two barium-enriched isotopes ((137)Ba and (135)Ba) were mixed at a molar ratio of ca. 1:3 (N Ba137/N Ba135) was administered to eight returning females caught during the spawning period. After injection, these females, as well as their offspring, were reared in a governmental hatchery located in the council of Cangas de Onís (Asturias, Spain). For comparison purposes, as well as for a time-monitoring control, egg and larva data obtained by solution analysis ICP-MS are also given. Otoliths (9-month-old juveniles) of marked offspring were analysed by LA-ICP-MS demonstrating a 100 % marking efficacy of this methodology. The capabilities of the molar fraction approach for 2D imaging of fish otoliths are also addressed.

  1. Metabolomic and elemental analysis of camel and bovine urine by GC-MS and ICP-MS.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Alhaider, Abdul Qader; Raish, Mohammad; Shakeel, Faiyaz

    2017-01-01

    Recent studies from the author's laboratory indicated that camel urine possesses antiplatelet activity and anti-cancer activity which is not present in bovine urine. The objective of this study is to compare the volatile and elemental components of bovine and camel urine using GC-MS and ICP-MS analysis. We are interested to know the component that performs these biological activities. The freeze dried urine was dissolved in dichloromethane and then derivatization process followed by using BSTFA for GC-MS analysis. Thirty different compounds were analyzed by the derivatization process in full scan mode. For ICP-MS analysis twenty eight important elements were analyzed in both bovine and camel urine. The results of GC-MS and ICP-MS analysis showed marked difference in the urinary metabolites. GC-MS evaluation of camel urine finds a lot of products of metabolism like benzene propanoic acid derivatives, fatty acid derivatives, amino acid derivatives, sugars, prostaglandins and canavanine. Several research reports reveal the metabolomics studies on camel urine but none of them completely reported the pharmacology related metabolomics. The present data of GC-MS suggest and support the previous studies and activities related to camel urine.

  2. Magnetophoretic separation ICP-MS immunoassay using Cs-doped multicore magnetic nanoparticles for the determination of salmonella typhimurium.

    Science.gov (United States)

    Jeong, Arong; Lim, H B

    2018-02-01

    In this work, a magnetophoretic separation ICP-MS immunoassay using newly synthesized multicore magnetic nanoparticles (MMNPs) was developed for the determination of salmonella typhimurium (typhi). The uniqueness of this method was the use of MMNPs doped with Cs for both separation and detection, which enable us to achieve fast analysis, high sensitivity, and good reliability. For demonstration, heat-killed typhi in a phosphate buffer solution was determined by ICP-MS after the MMNP-typhi reaction product was separated from unreacted MMNPs in a micropipette tip filled with 25% polyethylene glycol through magnetophoretic separation. The calibration curve obtained by plotting 133 Cs intensity vs. the number of synthetic standard, showed a coefficient of determination (R 2 ) of 0.94 with a limit of detection (LOD) of 102 cells/mL without cell culturing. Excellent recoveries, between 98-100%, were obtained from four replicates and compared with a sandwich-type ICP-MS immunoassay for further confirmation. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. ICP-MS/MS-Based Ionomics: A Validated Methodology to Investigate the Biological Variability of the Human Ionome.

    Science.gov (United States)

    Konz, Tobias; Migliavacca, Eugenia; Dayon, Loïc; Bowman, Gene; Oikonomidi, Aikaterini; Popp, Julius; Rezzi, Serge

    2017-05-05

    We here describe the development, validation and application of a quantitative methodology for the simultaneous determination of 29 elements in human serum using state-of-the-art inductively coupled plasma triple quadrupole mass spectrometry (ICP-MS/MS). This new methodology offers high-throughput elemental profiling using simple dilution of minimal quantity of serum samples. We report the outcomes of the validation procedure including limits of detection/quantification, linearity of calibration curves, precision, recovery and measurement uncertainty. ICP-MS/MS-based ionomics was used to analyze human serum of 120 older adults. Following a metabolomic data mining approach, the generated ionome profiles were subjected to principal component analysis revealing gender and age-specific differences. The ionome of female individuals was marked by higher levels of calcium, phosphorus, copper and copper to zinc ratio, while iron concentration was lower with respect to male subjects. Age was associated with lower concentrations of zinc. These findings were complemented with additional readouts to interpret micronutrient status including ceruloplasmin, ferritin and inorganic phosphate. Our data supports a gender-specific compartmentalization of the ionome that may reflect different bone remodelling in female individuals. Our ICP-MS/MS methodology enriches the panel of validated "Omics" approaches to study molecular relationships between the exposome and the ionome in relation with nutrition and health.

  4. Comparison of Dilution, Filtration, and Microwave Digestion Sample Pretreatments in Elemental Profiling of Wine by ICP-MS.

    Science.gov (United States)

    Godshaw, Joshua; Hopfer, Helene; Nelson, Jenny; Ebeler, Susan E

    2017-09-25

    Wine elemental composition varies by cultivar, geographic origin, viticultural and enological practices, and is often used for authenticity validation. Elemental analysis of wine by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is challenging due to the potential for non-spectral interferences and plasma instability arising from organic matrix components. Sample preparation mitigates these interferences, however, conflicting recommendations of best practices in ICP-MS analysis of wine have been reported. This study compared direct dilution, microwave-assisted acid digestion, and two filtration sample pretreatments, acidification prior to filtration and filtration followed by acidification, in elemental profiling of one white and three red table wines by ICP-MS. Of 43 monitored isotopes, 37 varied by sample preparation method, with significantly higher results of 17 isotopes in the microwave-digested samples. Both filtration treatments resulted in lower results for 11 isotopes compared to the other methods. Finally, isotope dilution determination of copper based on natural abundances and the 63 Cu: 65 Cu instrument response ratio agreed with external calibration and confirmed a significant sample preparation effect. Overall, microwave digestion did not compare favorably, and direct dilution was found to provide the best compromise between ease of use and result accuracy and precision, although all preparation strategies were able to differentiate the wines.

  5. Size exclusion chromatography with online ICP-MS enables molecular weight fractionation of dissolved phosphorus species in water samples.

    Science.gov (United States)

    Venkatesan, Arjun K; Gan, Wenhui; Ashani, Harsh; Herckes, Pierre; Westerhoff, Paul

    2018-04-15

    Phosphorus (P) is an important and often limiting element in terrestrial and aquatic ecosystem. A lack of understanding of its distribution and structures in the environment limits the design of effective P mitigation and recovery approaches. Here we developed a robust method employing size exclusion chromatography (SEC) coupled to an ICP-MS to determine the molecular weight (MW) distribution of P in environmental samples. The most abundant fraction of P varied widely in different environmental samples: (i) orthophosphate was the dominant fraction (93-100%) in one lake, two aerosols and DOC isolate samples, (ii) species of 400-600 Da range were abundant (74-100%) in two surface waters, and (iii) species of 150-350 Da range were abundant in wastewater effluents. SEC-DOC of the aqueous samples using a similar SEC column showed overlapping peaks for the 400-600 Da species in two surface waters, and for >20 kDa species in the effluents, suggesting that these fractions are likely associated with organic matter. The MW resolution and performance of SEC-ICP-MS agreed well with the time integrated results obtained using conventional ultrafiltration method. Results show that SEC in combination with ICP-MS and DOC has the potential to be a powerful and easy-to-use method in identifying unknown fractions of P in the environment. Copyright © 2018 Elsevier Ltd. All rights reserved.

  6. Determination of technetium-99 in environmental standard reference materials by ICP-MS

    International Nuclear Information System (INIS)

    Tagami, K.; Uchida, S.

    2000-01-01

    Technetium-99 is an artificial radionuclide which is produced in the fission of 235 U or 239 Pu with a relatively high fission yield of ca. 6%. Because of its long half-life of 2.1 x 10 5 y, 99 Tc has been accumulating in the environment, and thus, is considered to present a potential risk for humans. It is important for dose assessments to identify the behavior of the nuclide in the environment. Analysis data of global fallout 99 Tc in environmental samples would give useful information for predicting the nuclide's behavior; however, due to its low concentration and analytical difficulties, not much data are available. Besides, no environmental standard reference material (SRM) for 99 Tc is available. If we could get suitable SRMs for 99 Tc analysis, it would be easier to determine the concentration of 99 Tc in environmental samples. The purpose of this study was to investigate the possibility of several SRMs to be used as references for low-level 99 Tc. For this, ICP-MS was used for 99 Tc determination. In recent years, ICP-MS has been used for 99 Tc measurements instead of radioactivity counting methods. The samples used were as follows: A) IAEA-373 (a grass sample collected on grassland near Chernobyl Nuclear Power Reactor, Ukraine), B) IAEA-375 (a soil sample collected on a field near Chernobyl Nuclear Power Reactor, Russia), C) IAEA-135 (a sea sediment sample affected by Sellafield, UK), D) five seaweed samples of which the concentration levels are different from each other (collected around the coast near Sellafield, UK). Throughout the chemical separation, 95m Tc was used as a yield monitor. The sample was incinerated for at least 2 h at 450degC. After 99 Tc extraction from the sample at 90degC for 3 h with 4M HNO 3 , the sample was filtered and the residue on the filter was washed with deionized water. The solution was diluted to ca. 0.1M HNO 3 then passed through TEVA resin column (EIChroM Industries, Inc.) to extract Tc onto the resin. Then Tc was

  7. Relationship between growth of marbled flounder (Pleuronectes yokohamae) and Cs concentration in their muscle determined by ICP-MS

    International Nuclear Information System (INIS)

    Isoyama, Naohiko; Oikawa, Shinji; Misonoo, Jun

    2008-01-01

    For the purpose of marine environmental radioactivity monitoring, stable Cs and 137 Cs concentrations were obtained from 214 marbled flounder (Pleuronectes yokohamae) samples collected from off the coast of Ibaraki prefecture in Japan in 2005 and 2006. Prior to the investigation, an analytical method for the determination of Cs in muscle of marbled flounder samples by inductively coupled plasma mass spectrometry (ICP-MS) was seriously considered from the view point of sample preparation (wet way) to a Cs measurement. Since major problems in determining Cs by the ICP-MS is the interference of matrix materials and molecular ions on Cs peak area (m/z 133), a known amount of In (m/s 115) was added to the sample solutions as an internal standard. To check the accuracy of the determination, duplication analysis and standard reference materials were used. Analytical results of Cs in muscles samples by ICP-MS agreed well with duplicated samples, and standard reference materials. The standard length and body weight were obtained from a total of 214 flounder samples. The stable Cs, stable K and 137 Cs concentrations in muscle were determined by the ICP-MS, flame photometry and radiochemical analysis, respectively. The mean standard length correlates closely with the mean body weight. The stable Cs concentration was in proportion to the body weight, also, the 137 Cs concentration correlated closely with stable Cs concentration in muscle. On the other hand, a stable K concentration was found to be uniform, and unrelated with 137 Cs and stable Cs concentrations. The specific activities, the ratio of 137 Cs/stable Cs in muscle, was found to be 5.5 - 6.7 with an average of 6.2 ± 0.35 (SD) among five different size groups of the standard length of marbled flounder samples. From these results, ICP-MS provided useful tools for the determination of a trace amount of Cs in muscle samples, combined with wet way pretreatment techniques. In addition, marbled flounder proved to be a

  8. Ion chromatography separation of lanthanides at trace concentrations from Gd Matrix and quantification by ICP-MS

    International Nuclear Information System (INIS)

    Raut, V.V.; Jeyakumar, S.; Nagar, B.K.; Deb, S.B.; Saxena, M.K.; Tomar, B.S.

    2014-01-01

    Gadolinium compounds are mainly used as burnable poison. The presence of certain impurities is undesirable in the nuclear grade Gd compounds. Gd 2 O 3 , a most common raw material used for the preparation of nuclear grade Gd compounds. Analysis of rare earth impurities in Gd-matrices is one of the important exercises carried out to ensure the purity of Gd 2 O 3 . Determination of lanthanides at trace concentrations in lanthanide (Gd) matrix is complicated and difficult to realize. This is because the selective separation of REE's in one of the lanthanide elements is a challenging task. The present study was carried out to explore the feasibility of separating trace level lanthanides from Gd matrix by ion interaction chromatography (IIC) and to develop an analytical methodology for the determination of lanthanides by inductively coupled plasma mass spectrometry (ICP-MS). In the present investigation, the reversed phase column was dynamically modified into sulphonic acid functionalized surface by using 0.025 M n-Octane sulphonic acid (OSA). With α-HIBA eluent system, the elution order follows as Lu to La. The separations are employed with gradient elution mode. Since the sample has large excess of Gd, elution profiles with concentration gradient of HIBA were attempted. Separated fractions of Light lanthanides (LLn) and Heavy lanthanides (HLn) were collected and analyzed by ICP-MS. During MS analysis, it was observed that due to high concentration of salt (Na salt of OSA) present in the collected fractions caused difficulty in ICP-MS . Hence the experiments were carried out using another ion interacting reagent viz. 0.03 M camphor-10-sulphonic acid (CSA). Initial concentration of HIBA was kept at 0.025 M up to 15 min for the elution of HLns i.e. from Lu to Tb and it was then increased to 0.05 M to 0.3 M in 30 min. After elution of Tb, outlet of the column was switched to drain for 7 min to separate bulk Gd fraction. From 22 to 35 min effluent fraction containing Eu

  9. Comparison of the suitability of alkaline or enzymatic sample pre-treatment for characterization of silver nanoparticles in human tissue by single particle ICP-MS

    DEFF Research Database (Denmark)

    Vidmar, Janja; Buerki-Thurnherr, Tina; Löschner, Katrin

    2018-01-01

    and their size are required for studying NP accumulation in placental tissue. In the present study, we applied and compared two sample preparation techniques, alkaline and enzymatic treatment, followed by single particle ICP-MS (spICP-MS) analysis, for characterizing AgNPs spiked to human placental tissue. Both...... sample preparation approaches are currently used for AgNPs in biological tissues but have not been directly compared yet. We showed that the method using enzymatic tissue treatment followed by spICP-MS is efficient for determination of mass and number concentration and size distribution of AgNPs in human...... placental tissues. Properties of the AgNPs were preserved during enzymatic digestion and comparable with the primary particles. The matrix effect on the determination of Ag sensitivity and transport efficiency in spICP-MS analysis was systematically evaluated as well. The method was applied to human...

  10. Sensitivities of selenite, selenate, selenomethionine and trimethylselenonium ion in aqueous solution and in blood plasma - ETAAS compared with ICP-MS

    DEFF Research Database (Denmark)

    Gammelgaard, B.; Larsen, Erik Huusfeldt

    1998-01-01

    coupled plasma mass spectrometry (ICP-MS). Using ETAAS, the sensitivities for Se(IV), SeMet and TMSe in aqueous solution were similar, whereas the sensitivity of Se(VI) was 63% of that value. In blood plasma, the ETAAS sensitivities of Se(IV) and Se(VI) were equal, whereas the sensitivities of Se......Met and TMSe were 87 and 56%, respectively, of that value. In contrast, the ICP-MS sensitivities obtained for Se(VI), TMSe and SeMet were between 96 and 98% of that obtained for Se(IV) in aqueous solution and in blood plasma. It is concluded, that ICP-MS is superior to ETAAS as the problem of differences...... in sensitivity of the selenium species when using ETAAS are not prevalent when using the ICP-MS technique....

  11. Practical limitations of single particle ICP-MS in the determination of nanoparticle size distributions and dissolution: case of rare earth oxides.

    Science.gov (United States)

    Fréchette-Viens, Laurie; Hadioui, Madjid; Wilkinson, Kevin J

    2017-01-15

    The applicability of single particle ICP-MS (SP-ICP-MS) for the analysis of nanoparticle size distributions and the determination of particle numbers was evaluated using the rare earth oxide, La 2 O 3 , as a model particle. The composition of the storage containers, as well as the ICP-MS sample introduction system were found to significantly impact SP-ICP-MS analysis. While La 2 O 3 nanoparticles (La 2 O 3 NP) did not appear to interact strongly with sample containers, adsorptive losses of La 3+ (over 24h) were substantial (>72%) for fluorinated ethylene propylene bottles as opposed to polypropylene (size distributions. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Optimisation and application of ICP-MS and alpha-spectrometry for determination of isotopic ratios of depleted uranium and plutonium in samples collected in Kosovo

    OpenAIRE

    Boulyga, S. F.; Testa, C.; Desideri, D.; Becker, J. S.

    2001-01-01

    The determination of environmental contamination with natural and artificial actinide isotopes and evaluation of their source requires precise isotopic determination of actinides, above all uranium and plutonium. This can be achieved by alpha spectrometry or by inductively coupled plasma mass spectrometry (ICP-MS) after chemical separation of actinides. The performance of a sector-field ICP-MS (ICP-SFMS) coupled to a low-flow micronebulizer with a membrane desolvation unit, "Aridus'', was stu...

  13. Determination of the structure and composition of Au-Ag bimetallic spherical nanoparticles using single particle ICP-MS measurements performed with normal and high temporal resolution.

    Science.gov (United States)

    Kéri, Albert; Kálomista, Ildikó; Ungor, Ditta; Bélteki, Ádám; Csapó, Edit; Dékány, Imre; Prohaska, Thomas; Galbács, Gábor

    2018-03-01

    In this study, the information that can be obtained by combining normal and high resolution single particle ICP-MS (spICP-MS) measurements for spherical bimetallic nanoparticles (BNPs) was assessed. One commercial certified core-shell Au-Ag nanoparticle and three newly synthesized and fully characterized homogenous alloy Au-Ag nanoparticle batches of different composition were used in the experiments as BNP samples. By scrutinizing the high resolution spICP-MS signal time profiles, it was revealed that the width of the signal peak linearly correlates with the diameter of nanoparticles. It was also observed that the width of the peak for same-size nanoparticles is always significantly larger for Au than for Ag. It was also found that it can be reliably determined whether a BNP is of homogeneus alloy or core-shell structure and that, in the case of the latter, the core comprises of which element. We also assessed the performance of several ICP-MS based analytical methods in the analysis of the quantitative composition of bimetallic nanoparticles. Out of the three methods (normal resolution spICP-MS, direct NP nebulization with solution-mode ICP-MS, and solution-mode ICP-MS after the acid dissolution of the nanoparticles), the best accuracy and precision was achieved by spICP-MS. This method allows the determination of the composition with less than 10% relative inaccuracy and better than 3% precision. The analysis is fast and only requires the usual standard colloids for size calibration. Combining the results from both quantitative and structural analyses, the core diameter and shell thickness of core-shell particles can also be calculated. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Radionuclide content of simulated and fully radioactive SRLLL waste glasses: comparison of results from ICP-MS, gamma spectrometry and alpha spectrometry

    International Nuclear Information System (INIS)

    Wolf, S.F.; Bates, J.K.

    1995-01-01

    We have measured the transuranic content of two transuranic=doped, simulated waste glasses, using inductively coupled plasma-mass spectrometry (ICP-MS), γ-spectrometry, and α-spectrometry. Average concentrations measured by each technique were within ± 10% of the as-doped concentrations. We also report the transuranic content of three fully radioactive SRL waste glasses that were determined using γ- and α-spectrometry measurements to deconvolute isobaric interferences present in the ICP-MS analyses

  15. ICP MS ニヨル カンキョウ シリョウチュウ ノ コンセキ ゲンソ ノ ソクテイ 1 ICP MS ソウチ ノ サイテキ ジョウケン オヨビ ソノ ブンセキ セイド

    OpenAIRE

    "猶原,順/大西,諭/佐藤,昭彦[他]"; "ナオハラ,ジュン/オオニシ,サトシ/サトウ,アキヒコ"; "Naohara,Jun/Oonishi,Satoshi/Satou,Akihiko"

    1992-01-01

    "For determination of trace elements in environmental sample by inductively coupled plasma mass spectrometry (ICP-MS), the optimum condition of ICP-MS was determined and the stability of ICP-MS and the precision of elements concentration were investigated. The optimum condition was the sampling depth : 13 mm and RF-power : 1.2 KW. The stability of ICP-MS was indicated little drift of ionic strength after plasma lighting, however, ICP-MS was stabilized after 40 minutes. The coefficient variati...

  16. Analysis of metallic nanoparticles and their ionic counterparts in complex matrix by reversed-phase liquid chromatography coupled to ICP-MS.

    Science.gov (United States)

    Yang, Yuan; Luo, Li; Li, Hai-Pu; Wang, Qiang; Yang, Zhao-Guang; Qu, Zhi-Peng; Ding, Ru

    2018-05-15

    Developing quantification and characterization methodology for metallic nanoparticles (MNPs) and their ionic component in complex matrix are crucial for the evaluation of their environmental behavior and health risks to humans. In this study, reversed phase high performance liquid chromatography combined ICP-MS was established for the characterization of MNPs in complex matrix. The ionic component could be separated from NPs with the optimized parameters of aqueous mobile phase. Good linear relationship between average diameter and retention time of NPs was obtained using HPLC-ICP-MS and the size smaller than 40 nm could be determined with this method, the detected results were in accordance with TEM results. The low detection limit of AuNPs and Au(Ⅲ) (both in sub-μg/L level) showed that this method was promising for the characterization of AuNPs and Au(Ⅲ) in environmental water. The mass concentration of ionic Au(Ⅲ) in environmental water could be detected using the proposed HPLC-ICP-MS and the concentration of AuNPs was obtained by subtracting the Au(Ⅲ) concentration from the total Au (The concentration of total Au was detected by ICP-MS after microwave digestion). Furthermore this proposed HPLC-ICP-MS method and single particle-ICPMS (SP-ICP-MS) was used for the analysis of the Ag speciation in commercial antibacterial products. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Can we trust mass spectrometry for determination of arsenic peptides in plants: comparison of LC-ICP-MS and LC-ES-MS/ICP-MS with XANES/EXAFS in analysis of Thunbergia alata.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Meharg, Andrew A; Charnock, John M; Feldmann, Jörg

    2008-04-01

    The weakest step in the analytical procedure for speciation analysis is extraction from a biological material into an aqueous solution which undergoes HPLC separation and then simultaneous online detection by elemental and molecular mass spectrometry (ICP-MS/ES-MS). This paper describes a study to determine the speciation of arsenic and, in particular, the arsenite phytochelatin complexes in the root from an ornamental garden plant Thunbergia alata exposed to 1 mg As L(-1) as arsenate. The approach of formic acid extraction followed by HPLC-ES-MS/ICP-MS identified different As(III)-PC complexes in the extract of this plant and made their quantification via sulfur (m/z 32) and arsenic (m/z 75) possible. Although sulfur sensitivity could be significantly increased when xenon was used as collision gas in ICP-qMS, or when HR-ICP-MS was used in medium resolution, the As:S ratio gave misleading results in the identification of As(III)-PC complexes due to the relatively low resolution of the chromatography system in relation to the variety of As-peptides in plants. Hence only the parallel use of ES-MS/ICP-MS was able to prove the occurrence of such arsenite phytochelatin complexes. Between 55 and 64% of the arsenic was bound to the sulfur of peptides mainly as As(III)(PC(2))(2), As(III)(PC(3)) and As(III)(PC(4)). XANES (X-ray absorption near-edge spectroscopy) measurement, using the freshly exposed plant root directly, confirmed that most of the arsenic is trivalent and binds to S of peptides (53% As-S) while 38% occurred as arsenite and only 9% unchanged as arsenate. EXAFS data confirmed that As-S and As-O bonds occur in the plants. This study confirms, for the first time, that As-peptides can be extracted by formic acid and chromatographically separated on a reversed-phase column without significant decomposition or de-novo synthesis during the extraction step.

  18. ICP-MS as advantageous analytical technique for the determination of long-lived /sup 99/Tc in the environment

    International Nuclear Information System (INIS)

    Ihsanullah

    1992-05-01

    Technetium (Tc) was the first artificially created by man and has no stable isotope. The most crucial technetium isotope environmentally /sup 99/Tc is a pure beta emitter with a half-life of 2.1 X 105 years. The main source of /sup 99/Tc to the environment is the disposal of liquid wastes from nuclear installations or during separation and recovery of spent nuclear fuels. Because of its long half life, high fission yield, mobility and current interest in the collective long term doses, it is necessary to establish a knowledge of the behavior of /sup 99/Tc in the environment for complete assessment of the impact of nuclear industry. Due to various analytical difficulties however, data on the behavior of Tc in the environment are limited. In the literature, many techniques are reported for the analysis of Tc. A very sensitive, precise and powerful technique is required which can be applied to environmental samples in order to gain information by obtaining more precise data to assess the impact of Tc releases on man. Attention has been focussed for this purpose on a new powerful technique i.e. inductively coupled plasma mass spectrometry (ICP-MS). This report has been directed towards the development of ICP-MS. The technique gives a very high sensitivity enabling long lived radionuclides including /sup 99/Tc to be measured directly down to pg ml-1 levels in solution. Because of its versatility ICP-MS is finding applications for trace multielement analysis and low detection limits in almost all fields. (author)

  19. Bioimaging mass spectrometry of trace elements – recent advance and applications of LA-ICP-MS: A review

    Energy Technology Data Exchange (ETDEWEB)

    Becker, J.Sabine, E-mail: s.becker@fz-juelich.de [Central Institute for Engineering, Electronics and Analytics (ZEA-3), Forschungszentrum Jülich, Jülich D-52425 (Germany); Matusch, Andreas, E-mail: a.matusch@fz-juelich.de [Institute for Neuroscience and Medicine (INM-2), Forschungszentrum Jülich, Jülich D-52425 (Germany); Wu, Bei, E-mail: b.wu@fz-juelich.de [Central Institute for Engineering, Electronics and Analytics (ZEA-3), Forschungszentrum Jülich, Jülich D-52425 (Germany)

    2014-07-04

    Highlights: • Bioimaging LA-ICP-MS is established for trace metals within biomedical specimens. • Trace metal imaging allows to study brain function and neurodegenerative diseases. • Laser microdissection ICP-MS was applied to mouse brain hippocampus and wheat root. - Abstract: Bioimaging using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) offers the capability to quantify trace elements and isotopes within tissue sections with a spatial resolution ranging about 10–100 μm. Distribution analysis adds to clarifying basic questions of biomedical research and enables bioaccumulation and bioavailability studies for ecological and toxicological risk assessment in humans, animals and plants. Major application fields of mass spectrometry imaging (MSI) and metallomics have been in brain and cancer research, animal model validation, drug development and plant science. Here we give an overview of latest achievements in methods and applications. Recent improvements in ablation systems, operation and cell design enabled progressively better spatial resolutions down to 1 μm. Meanwhile, a body of research has accumulated covering basic principles of the element architecture in animals and plants that could consistently be reproduced by several laboratories such as the distribution of Fe, Cu, Zn in rodent brain. Several studies investigated the distribution and delivery of metallo-drugs in animals. Hyper-accumulating plants and pollution indicator organisms have been the key topics in environmental science. Increasingly, larger series of samples are analyzed, may it be in the frame of comparisons between intervention and control groups, of time kinetics or of three-dimensional atlas approaches.

  20. Microwave-induced combustion of crude oil for further rare earth elements determination by USN–ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, J.S.F. [Departamento de Química Inorgânica, Universidade Federal do Rio Grande do Sul, 97105-900 Porto Alegre, RS (Brazil); Pereira, L.S.F.; Mello, P.A. [Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Guimarães, R.C.L.; Guarnieri, R.A.; Fonseca, T.C.O. [CENPES/PETROBRAS, 21941-945 Rio de Janeiro, RJ (Brazil); Flores, E.M.M., E-mail: ericommf@gmail.com [Departamento de Química, Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil)

    2014-09-24

    Highlights: • Microwave-induced combustion was applied for light and heavy crude oils digestion. • It was feasible to determine all the REEs in heavy crude oil by ICP-MS. • Only diluted acid solutions were used in agreement to green chemistry recommendations. - Abstract: A procedure for light and heavy crude oils digestion by microwave-induced combustion (MIC) is proposed for the first time for further rare earth elements (REE) determination by inductively coupled plasma mass spectrometry (ICP-MS) equipped with an ultrasonic nebulizer (USN). Samples of crude oil (API density of 10.8–23.5, up to 250 mg) were inserted in polycarbonate capsules and combusted using 20 bar of oxygen and 50 μL of 6 mol L{sup −1} ammonium nitrate as igniter. Nitric acid solutions (1–14.4 mol L{sup −1}) were evaluated for analyte absorption and a reflux step was applied after combustion (5 min of microwave irradiation at 1400 W) in order to achieve better analyte recoveries. Accuracy was evaluated using a spiked sample and also by comparison of results obtained by microwave-assisted digestion combined to ultraviolet radiation (MW–UV) and by neutron activation analysis (NAA). Using 3 mol L{sup −1} HNO{sub 3}, quantitative recoveries (better than 97%) were obtained for all analytes. Blank values were always negligible. Agreement was higher than 96% for La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Y by comparison of results with those obtained by MW–UV and by NAA (only for La, Ce, Nd, Sm, and Yb). Residual carbon content in digests using MIC was always below 1%. As an advantage over conventional procedures for crude oil digestion, using MIC, it was possible to use diluted acid as absorbing solution, obtaining better limits of detection and avoiding interferences in REE determination by USN–ICP-MS.

  1. Determination of chemical form of iodine with IC-ICP-MS system and its application to the environmental samples

    International Nuclear Information System (INIS)

    Yoshida, S.; Katou, S.; Sekimoto, H.; Muramatsu, Y.

    2005-01-01

    Iodine-129 is one of the important radionuclides possibly released into the environment from nuclear weapons testing and from the nuclear facilities such as nuclear fuel reprocessing plants. Because of its long half-life (1.57 x 10 7 y), knowing its long-term behavior in the environment is a major concern. As I-129 is expected to act together with stable iodine (I-127) in the environment after long time, the biogeochemical cycling of stable iodine in the environment can be used for the reliable safety assessment of I-129. Chemical form is the one of the important factors controlling the 'iodine behavior in the environment. Iodide (I - ) and iodate (IO 3 - ) are known to be the major chemical form in the aqueous solution. However, the information on the chemical form of iodine in the environmental sample is limited because of lack of reliable analytical technique for trace level of iodine in the environment. In this study, the analytical system by using ion chromatograph (IC) followed by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the separate determination of I - and IO 3 - in the aqueous solution. The IC with anion exchange column (EXCELPAK ICS-A23) was used for the separation of I - and IO 3 - with 30 mM (NH 4 ) 2 CO 3 as eluent. Separated iodine was determined with ICP-MS on line. with the detection limit 0.1 - 1 μg/L. The total iodine concentration was also measured by the direct determination with ICP-MS. The iodine in the several environmental samples such as irrigation water in paddy field was successfully determined with information of chemical form. In incubation experiment with flooded soil, the change of the chemical form of iodine in the soil solution with change of Eh was observed. Detailed data will be discussed in the presentation.

  2. Green and efficient sample preparation method for the determination of catalyst residues in margarine by ICP-MS.

    Science.gov (United States)

    Hartwig, Carla Andrade; Pereira, Rodrigo Mendes; Novo, Diogo La Rosa; Oliveira, Dirce Taina Teixeira; Mesko, Marcia Foster

    2017-11-01

    Responding to the need for green and efficient methods to determine catalyst residues with suitable precision and accuracy in samples with high fat content, the present work evaluates a microwave-assisted ultraviolet digestion (MW-UV) system for margarines and subsequent determination of Ni, Pd and Pt using inductively coupled plasma mass spectrometry (ICP-MS). It was possible to digest up to 500mg of margarine using only 10mL of 4molL -1 HNO 3 with a digestion efficiency higher than 98%. This allowed the determination of catalyst residues using the ICP-MS and free of interferences. For this purpose, the following experimental parameters were evaluated: concentration of digestion solution, sample mass and microwave irradiation program. The residual carbon content was used as a parameter to evaluate the efficiency of digestion and to select the most suitable experimental conditions. The accuracy evaluation was performed by recovery tests using a standard solution and certified reference material, and recoveries ranging from 94% to 99% were obtained for all analytes. The limits of detection for Ni, Pd and Pt using the proposed method were 35.6, 0.264 and 0.302ngg -1 , respectively. When compared to microwave-assisted digestion (MW-AD) in closed vessels using concentrated HNO 3 (used as a reference method for sample digestion), the proposed MW-UV could be considered an excellent alternative for the digestion of margarine, as this method requires only a diluted nitric acid solution for efficient digestion. In addition, MW-UV provides appropriate solutions for further ICP-MS determination with suitable precision (relative standard deviation < 7%) and accuracy for all evaluated analytes. The proposed method was applied to margarines from different brands produced in Brazil, and the concentration of catalyst residues was in agreement with the current legislation or recommendations. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. A study on the variation of strontium isotopic ratio in Darjeeling tea using MC-ICP-MS

    International Nuclear Information System (INIS)

    Lagad, Rupali A.; Alamelu, D.; Jagadish Kumar, S.; Aggarwal, Suresh K.; Rai, Vinai; Singh, S.K.

    2011-01-01

    In the present study, an analytical procedure based on the determination of the Sr isotope ratio 87 Sr/ 86 Sr in the Darjeeling tea samples by MC-ICP-MS was developed and applied to 15 green tea samples obtained from different tea gardens in Darjeeling. Variation in 87 Sr/ 86 Sr ratio was observed among eleven different tea gardens fro different geographical locations. The obtained data on 87 Sr/ 86 Sr ration in authentic tea leaves samples can be useful while comparing it with processed tea samples from respective regions

  4. Label-free DNA hybridization detection and single base-mismatch discrimination using CE-ICP-MS assay.

    Science.gov (United States)

    Li, Yan; Sun, Shao-kai; Yang, Jia-lin; Jiang, Yan

    2011-12-07

    Detecting a specific DNA sequence and discriminating single base-mismatch is critical to clinical diagnosis, paternity testing, forensic sciences, food and drug industry, pathology, genetics, environmental monitoring, and anti-bioterrorism. To this end, capillary electrophoresis (CE) coupled with the inductively coupled plasma mass spectrometry (ICP-MS) method is developed using the displacing interaction between the target ssDNA and the competitor Hg(2+) for the first time. The thymine-rich capture ssDNA 1 is interacted with the competitor Hg(2+), forming an assembled complex in a hairpin-structure between the thymine bases arrangement at both sides of the capture ssDNA 1. In the presence of a target ssDNA with stronger affinity than that of the competitor Hg(2+), the energetically favorable hybridization between capture ssDNA 1 and the target ssDNA destroys the hairpin-structure and releases the competitor as free Hg(2+), which was then read out and accurately quantified by CE-ICP-MS assay. Under the optimal CE separation conditions, free Hg(2+) ions and its capture ssDNA 1 adduct were baseline separated and detected on-line by ICP-MS; the increased peak intensity of free Hg(2+) against the concentration of perfectly complementary target ssDNA was linear over the concentration range of 30-600 nmol L(-1) with a limit of detection of 8 nmol L(-1) (3s, n = 11) in the pre-incubated mixture containing 1 μmol L(-1) Hg(2+) and 0.2 μmol L(-1) capture ssDNA 1. This new assay method is simple in design since any target ssDNA binding can in principle result in free Hg(2+) release by 6-fold Hg(2+) signal amplification, avoiding oligonucleotide labeling or assistance by excess signal transducer and signal reporter to read out the target. Due to element-specific detection of ICP-MS in our assay procedure, the interference from the autofluorescence of substrata was eliminated.

  5. Sensitivity of DF-ICP-MS, PERALS and alpha-spectrometry for the determination of actinides. A comparison

    International Nuclear Information System (INIS)

    Ayranov, M.; Kraehenbuehl, U.

    2009-01-01

    We applied three techniques (DF-ICP-MS, PERALS and alpha-spectrometry) for the determination of minor actinides at environmental levels. For each method the limit of detection and the resolution were estimated in order to study the content and isotopic composition of the actinides. Two international reference materials, IAEA-135 (Irish Sea Sediment) and IAEA-300 (Baltic Sea sediment) were analyzed for activity concentrations of 238 Pu, 239 Pu, 240 Pu, 241 Pu and 241 Am. The sensitivities of the three determination techniques were compared. (author)

  6. Combination of LC-ICP-MS, LC-MS and NMR for investigation of the oxidative degradation of selenomethionine

    DEFF Research Database (Denmark)

    Gammelgaard, B.; Cornett, Claus; Olsen, J.

    2003-01-01

    Selenomethionine (SeMet) was oxidized by heating an acidic solution with hydrogen peroxide. Samples were taken before and during the oxidation process. The oxidation products were separated by cation exchange chromatography followed by ICP-MS detection to identify the selenium containing compounds...... as well as electrospray ionization MS detection to determine the masses of the degradation products. Furthermore, the samples were analyzed by Se-77-NMR. The first appearing degradation product was selenomethionine selenoxide, which was converted via the deaminated selenoxide to methane seleninic acid...

  7. Analysis of archaeological ceramics and glass samples by microPIXE and LA-ICP-MS methods

    International Nuclear Information System (INIS)

    Uzonyi, I.; Elekes, Z.; Kiss, A.Z.

    1999-01-01

    The availability of a proton microprobe at ATOMKI and LA-ICP-MS and SEM techniques at the French institutes made it possible to start a joint research of archaeological ceramics and glass samples in the framework of COST-GI program about one year ago. Concerning ceramics the task has been the determination of provenance of some roman amphorae samples. In another project glass samples found in the royal palaces of Buda and Visegrad were analyzed. The results may be utilized both in exact dating and determination of provenance of glass artefacts of unknown origin. (K.A.)

  8. Determination of trace level of palladium and platinum content in anticancer drug Imatinib base by ICP-MS

    International Nuclear Information System (INIS)

    Yadav, Ravi; Salunke-Gawali, Sunita

    2013-01-01

    Metal impurities in Pharmaceutical drug substance is of great concern not only because of the intrinsic toxicity of certain contaminants but also due to the opposite effect that the contaminants which may have on drug stability and shelf life. Therefore it is necessary to monitor the organic as well as inorganic impurities throughout the process of manufacturing process at every stage from raw material, intermediate and finished products. An Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) method has been developed for Palladium and Platinum content in the anticancer drug, Imatinib mesylate. Rhodium (Rh) was used as internal standard for determination of Palladium and Platinum content on in Imatinib mesylate. (author)

  9. LA-ICP-MS for Trace Analysis of Long-Lived Radionuclides in Solid Non-conducting Radioactive Waste Samples

    International Nuclear Information System (INIS)

    Becker, J.S.; Gastel, M.; Tenzler, D.; Dietze, H.J.

    1999-01-01

    The characterization of radioactive waste materials from nuclear reactors for recycling and final storage requires fast, sensitive and precise analytical methods, which are able to determine long-lived radionuclidic ultra traces in a short time. For the determination of long-lived α and β ray-emitting nuclides besides the classical radiochemical methods which are mostly include time-consuming radiochemical separation procedures, to an increasing extent inductively coupled plasma mass spectrometry (ICP-MS) has been used successfully as a powerful trace, ultra trace and isotopic analytical method for the determination of long-lived radionuclides in aqueous solutions [1-3

  10. ICP-MS measurement of silver diffusion coefficient in graphite IG-110 between 1048K and 1284K

    Science.gov (United States)

    Carter, L. M.; Seelig, J. D.; Brockman, J. D.; Robertson, J. D.; Loyalka, S. K.

    2018-01-01

    Silver-110m has been shown to permeate intact silicon carbide and pyrolytic carbon coating layers of the TRISO fuel particles during normal High Temperature Gas-Cooled Reactor (HTGR) operational conditions. The diffusion coefficients for silver in graphite IG-110 measured using a release method designed to simulate HTGR conditions of high temperature and flowing helium in the temperature range 1048-1253 K are reported. The measurements were made using spheres milled from IG-110 graphite that were infused with silver using a pressure vessel technique. The Ag diffusion was measured using a time release technique with an ICP-MS instrument for detection. The results of this work are:

  11. Strontium isotope ratios - a possible tool to study the authenticity of Indian tea using MC-ICP-MS

    International Nuclear Information System (INIS)

    Lagad, Rupali A.; Alamelu, D.; Aggarwal, Suresh K.; Singh, Sunil K.

    2011-01-01

    In the present study, an analytical procedure based on determination of the Sr isotope ratio 87 Sr/ 86 Sr in the Indian tea samples by MC-ICP-MS was developed and applied to 28 tea samples from four different Indian regions. The 87 Sr/ 86 Sr isotope ratio of the tea samples in different Indian regions is strongly dependent on the soil and growth environment condition. The analysis results of 28 Indian tea samples revealed that 87 Sr/ 86 Sr atom ratio follows the order Darjeeling > Kangra > Assam > Munnar

  12. Distribution of titanium dioxide in mice after nasal inhalation using SRXRF and ICP-MS

    International Nuclear Information System (INIS)

    Wang, J.X.; Yu, H.W.; Sun, J.; Li, Y.F.; Xing, L.; Chen, C.Y.; Li, B.; Gao, Y.X.; Chai, Z.F.; Zhao, Y.L.

    2005-01-01

    distribution area of micro TiO 2 was wider than nano TiO 2 in olfactory bulb and brain, and micro TiO 2 was easier to entry into olfactory bulb through olfactory tract than nano TiO 2 . Possibly this is because nano TiO 2 is prone to aggregate and suspend in H 2 O solution. Quantitative titanium contents in visceral organs were determined by Inductively Coupled Plasma Mass Spectrometry (ICP-MS, Thermo Elemental X7, Thermo Electron Co.). The selected tissues (200-300 mg) were digested by nitric acid (MOS grade) at about 140 degree C. H 2 O 2 (MOS grade) was used to driven off the nitric vapor until the solution was clear. Finally, the solution volume was fixed to 3 ml by 2 % nitric acid. The single indium solution (20 ppb) was chosen as the internal standard element. The detection limit of Ti was several ng/ml. The present results indicate that TiO 2 could be translocated to the brain through the olfactory pathway and induce irregular arrangement of neurons and glial cells in the hippocampal region and cerebral cortex. Metabolic way of TiO 2 in brain and its potential neurotoxicity should be investigated further.

  13. Sem-EDXRF and ICP-MS investigation of the morphological and chemical composition of depleted uranium particles from Kuwait areas affected by the 1991 Gulf War

    International Nuclear Information System (INIS)

    Danesi, P.R.; Burns, K.; Campbell, M.; Ciurapinski, A.; Donohue, D.; Admon, U.; Burkart, W.

    2004-01-01

    Selected soil samples collected in Kuwait locations where residues of DU ammunition existed as a legacy of the 1991 Gulf War, have been investigated by scanning electron microscopy equipped with an energy dispersive X-ray fluorescence detector (SEM- EDXRF) with the objective to identify the presence of DU particles and characterize their shape and size. The isotopic and total bulk concentrations of uranium in the samples were measured by inductively coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry. The samples studied by SEM-EDXRF were prepared by gently tapping an aluminum stab covered with a doubled-sided adhesive carbon disk, thereby ensuring that the physical integrity of the samples was maintained. The results have indicted that soil collected just below (∼ 5 cm) corroded DU penetrators contained several DU oxide particles (isotopic ratio 235 U/ 238 U = 0.0021) ranging in size from 1 to 10 microns (approximate geometrical diameter) having an irregular shape. The particles are most likely corrosion products from the DU penetrators. Some particles are imbedded in a larger matrix containing aluminum oxide (corrosion product of the penetrator jacket) and silica (sand). Swipes collected inside holes in tanks hit by DU ammunition, using ultra-pure cotton cloths, have indicated the presence of many small DU particles in the range 1 to 10 microns. In this case the particles were found to contain also small quantities of Fe, probably the results on alloying process occurring when the DU penetrators impact with the tank armor. (author)

  14. Multielement determination of major-to-ultratrace elements in salmon egg by ICP-AES and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Matsuura, Hirotaka; Haraguchi, Hiroki [Nagoya Univ., Graduate School of Engineering, Dept. of Applied Chemistry, Nagoya, Aichi (Japan)

    2002-04-01

    The multielement determination of major-to-ultratrace elements in salmon egg was carried out by ICP-AES and ICP-MS. First, salmon eggs (30 eggs used) were digested with conc. nitric acid and 60% perchloric acid by heating almost to dryness repeatedly. Finally, the residues of salmon eggs were dissolved in 1 M nitric acid and the sample solutions were analyzed by ICP-AES and ICP-MS. About 40 elements could be determined over the concentration range in 9 orders of magnitude. The concentrations of bio-essential elements, such as Zn, Fe, and Cu, in salmon egg were 10-100 times higher than those in human blood serum. In addition, the major-to-ultratrace elements in cell cytoplasm and cell membrane were separately determined in a similar manner to those in whole egg cell. The concentrations of most bio-essential elements were higher in cell cytoplasm than in cell membrane, while those of Fe and Cu were higher in cell membrane than in cell cytoplasm of salmon egg. (author)

  15. An alternative interface for CE-ICP-MS cadmium speciation in metallothioneins based on volatile species generation

    International Nuclear Information System (INIS)

    Alvarez-Llamas, G.; Fernandez de la Campa, M.R.; Sanz-Medel, A.

    2005-01-01

    An alternative CE-ICP-MS interface based on volatile species generation (VSG) is here developed, evaluated and compared to the conventional sample introduction systems via nebulisation. For this purpose, the speciation of Cd-metallothioneins (MTs) in rabbit liver is taken as a model. Cd, bound to the different MT isoforms previously separated by CE, is transformed into volatile species at the exit of the capillary and on-line detected by ICP-MS. Optimum conditions for Cd VSG have been investigated in a flow injection device, using NaBH 4 as hydrogenation reagent in a HCl medium containing cobalt and thiourea as catalysts. Sample volume injected, CE separation voltage and reagents flows have been optimised. Analytical performance characteristics of the CE-VSG-ICP-(Q)MS coupling developed were evaluated, in terms of repeatability and linearity of response, using standard rabbit liver metallothionein isoforms (MT1 and MT2). Detection limits for Cd-MTs turned out to be almost one order of magnitude better than those derived from using a conventional Babington nebuliser-based interface. Compared to a MicroMist-based interface detection limits resulted to be similar, but the observed peak height was eight times higher using the VSG interface, indicating the enhanced analyte transport efficiency derived from VSG sample introduction systems

  16. Determination of traces of 237Np in environmental samples by ICP-MS after separation using TOA extraction chromatography

    International Nuclear Information System (INIS)

    Ji, Y.Q.; Li, J.Y.; Luo, S.G.; Wu, T.; Liu, J.L.

    2001-01-01

    A simple, rapid, cost-efficient, and robust method for separation of 237 Np with an extraction chromatographic column (TOA: tri-n-octylamine on Teflon powder) is outlined in detail and further improved for direct ICP-MS analysis. The column efficiently retained 237 Np in 2 mol L -1 HNO 3 medium and all of the 237 Np was easily eluted with 0.02 mol L -1 oxalic acid in 0.16 mol L -1 HNO 3 at 95 C. The separated solutions were free from most matrix elements and were aspirated into the ICP-MS directly. The decontamination factor for 238 U is more than 10 4 . The instrumental detection limit for 237 Np was 0.46 pg mL -1 , which corresponds to 1.2 x 10 -5 Bq mL -1 . The method is more rapid than traditional radiometric techniques. It is also considered to be more suitable for environmental monitoring than existing methods based on TOA. (orig.)

  17. Determination of traces of 237Np in environmental samples by ICP-MS after separation using TOA extraction chromatography.

    Science.gov (United States)

    Ji, Y Q; Li, J Y; Luo, S G; Wu, T; Liu, J L

    2001-09-01

    A simple, rapid, cost-efficient, and robust method for separation of 237Np with an extraction chromatographic column (TOA: tri-n-octylamine on Teflon powder) is outlined in detail and further improved for direct ICP-MS analysis. The column efficiently retained 237Np in 2 mol L(-1) HNO3 medium and all of the 237Np was easily eluted with 0.02 mol L(-1) oxalic acid in 0.16 mol L(-1) HNO3 at 95 degrees C. The separated solutions were free from most matrix elements and were aspirated into the ICP-MS directly. The decontamination factor for 238U is more than 10(4). The instrumental detection limit for 237Np was 0.46 pg mL(-1), which corresponds to 1.2 x 10(-5) Bq mL(-1). The method is more rapid than traditional radiometric techniques. It is also considered to be more suitable for environmental monitoring than existing methods based on TOA.

  18. The application of LA-ICP-MS in the examination of the thin plating layers found in late Roman coins

    Energy Technology Data Exchange (ETDEWEB)

    Vlachou-Mogire, C. [Numismatic Museum, 12 El. Venizelou Avenue, 106 71 Athens (Greece)], E-mail: vlachou_mogire@yahoo.co.uk; Stern, B.; McDonnell, J.G. [Department of Archaeological Sciences, University of Bradford, Bradford BD7 1RD (United Kingdom)

    2007-12-15

    During the late Roman period the production of complex copper alloy (Cu-Sn-Pb-Ag) coins with a silvered surface, became common practice. Previous analyses of these coins did not solve key technological issues and in particular, the silvering process. Two methods have been suggested for the production of the thin plating layers in late Roman coins the dipping in molten silver chloride and the use of silvering pastes. However, there are questions about their use. More recent research showed that hot-dipping methods, such as the dipping in molten silver chloride, were not really suitable for mass production. Also, the earliest references to the use of silvering pastes dated to 17th century AD. A review of ancient sources and historic literature indicated silver amalgam plating as the possible method for the production of the plating in late Roman coins. Results derived from non-destructive LA-ICP-MS analysis have demonstrated, for the first time, the presence of Hg in the surface layers of these coins. The optimization of the method and the factors influenced the analyses results, are discussed. The examination of the coins by means of EPMA confirmed the ICP-MS results. The introduction of a new technique for the examination of plating layers, helped in the identification of amalgam silvering as the method used in the production of the coins.

  19. Determination of trace elements in kidneys, livers and brains of rats with sealer implants by ICP-MS

    International Nuclear Information System (INIS)

    Simsek, Neslihan; Akinci, Levent; Alan, Hilal; Gecör, Orhan; Özan, Ülkü

    2017-01-01

    Following root canal treatment, sealers may contact periapical tissue. The purpose of this study was to evaluate the systemic toxic effects of epoxy resin-based sealers (AH Plus and Obtuseal). Inductively coupled plasma-mass spectrometry (ICP-MS) was used to measure levels of trace elements (beryllium, magnesium, aluminium, calcium, chromium, arsenic and lead) in the brain, kidney and liver of rats. Twenty sterilized polyethylene tubes were then filled with AH Plus and Obtuseal and implanted into the dorsal subcutaneous tissue of 10 rats; three unoperated animals were used as a control group. After 45 days, the rats were sacrificed by cervical dislocation following anaesthesia, and brains, kidneys and livers were removed from all experimental animals. ICP-MS analysis was used to determine levels of trace elements. Data were analysed using Kruskal– Wallis and Connover post hoc tests. No significant differences were found in aluminium and calcium levels, but brains, kidneys and livers showed significantly higher amounts of magnesium and chromium than the corresponding controls. In the kidney and liver samples, arsenic levels were found to be higher than in the control group. Lead was detected at higher levels only in liver samples from the AH Plus group. Beryllium was not detected in any organ. It was concluded that AH Plus and Obtuseal release minimal quantities of trace elements when in contact with subcutaneous tissue, and further studies are needed to understand the systemic effects of these materials

  20. Detection of lead nanoparticles in game meat by single particle ICP-MS following use of lead-containing bullets.

    Science.gov (United States)

    Kollander, Barbro; Widemo, Fredrik; Ågren, Erik; Larsen, Erik H; Loeschner, Katrin

    2017-03-01

    This study investigated whether game meat may contain nanoparticles of lead from ammunition. Lead nanoparticles in the range 40 to 750 nm were detected by ICP-MS in single particle mode in game shot with lead-containing bullets. The median diameter of the detected nanoparticles was around 60 nm. The particle mass concentration ranged from 290 to 340 ng/g meat and the particle number concentrations from 27 to 50 million particles/g meat. The size limit of detection strongly depended on the level of dissolved lead and was in the range of 40 to 80 nm. In game meat sampled more than 10 cm away from the wound channel, no lead particles with a diameter larger than 40 nm were detected. In addition to dissolved lead in meat that originated from particulates, the presence of lead nano particles in game meat represents a hitherto unattended source of lead with a largely unknown toxicological impact to humans. Graphical Abstract Detection of lead nanoparticles in game meat by single particle ICP-MS following use of leadcontaining bullets.

  1. Sample preparation method for ICP-MS measurement of 99Tc in a large amount of environmental samples

    International Nuclear Information System (INIS)

    Kondo, M.; Seki, R.

    2002-01-01

    Sample preparation for measurement of 99 Tc in a large amount of soil and water samples by ICP-MS has been developed using 95m Tc as a yield tracer. This method is based on the conventional method for a small amount of soil samples using incineration, acid digestion, extraction chromatography (TEVA resin) and ICP-MS measurement. Preliminary concentration of Tc has been introduced by co-precipitation with ferric oxide. The matrix materials in a large amount of samples were more sufficiently removed with keeping the high recovery of Tc than previous method. The recovery of Tc was 70-80% for 100 g soil samples and 60-70% for 500 g of soil and 500 L of water samples. The detection limit of this method was evaluated as 0.054 mBq/kg in 500 g soil and 0.032 μBq/L in 500 L water. The determined value of 99 Tc in the IAEA-375 (soil sample collected near the Chernobyl Nuclear Reactor) was 0.25 ± 0.02 Bq/kg. (author)

  2. Determination of ultratrace amounts of uranium and thorium in aluminium and aluminium alloys by electrothermal vaporization/ICP-MS

    International Nuclear Information System (INIS)

    Nakamura, Yasushi; Kobayashi, Yoshio; Kakurai, Yousuke

    1993-01-01

    A method has been developed for determining the 0.01 ng g -1 level of uranium and thorium in aluminium and aluminium alloys by electrothermal vaporization (ETV)/ICP-MS. This method was found to be significantly interfered with any matrices or other elements contained. An ion-exchange technique was therefore applied to separate uranium and thorium from aluminium and other elements. It was known that uranium are adsorbed on an anion-exchange resin and thorium are adsorbed on cation-exchange resin. However, aluminium and copper were eluted with 6 M hydrochloric acid. Dissolve the sample with hydrochloric acid containing copper which was added for analysis of pure aluminium, and oxidize with hydrogen peroxide. Concentration of hydrochloric acid in the solution was adjusted to 6 M, and then passed the solution through the mixed ion-exchange resin column. After the uranium and thorium were eluted with 1 M hydrofluoric acid-0.1 M hydrochloric acid, the solution was evaporated to dryness. It was then dissolved with 1 M hydrochloric acid. Uranium and thorium were analyzed by ETV/ICP-MS using tungsten and molybdenum boats, respectively, since the tungsten boat contained high-level thorium and the molybdenum boat contained uranium. The determination limit of uranium and thorium were 0.003 and 0.005 ng g -1 , respectively. (author)

  3. Metrological approach to quantitative analysis of clinical samples by LA-ICP-MS: A critical review of recent studies.

    Science.gov (United States)

    Sajnóg, Adam; Hanć, Anetta; Barałkiewicz, Danuta

    2018-05-15

    Analysis of clinical specimens by imaging techniques allows to determine the content and distribution of trace elements on the surface of the examined sample. In order to obtain reliable results, the developed procedure should be based not only on the properly prepared sample and performed calibration. It is also necessary to carry out all phases of the procedure in accordance with the principles of chemical metrology whose main pillars are the use of validated analytical methods, establishing the traceability of the measurement results and the estimation of the uncertainty. This review paper discusses aspects related to sampling, preparation and analysis of clinical samples by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) with emphasis on metrological aspects, i.e. selected validation parameters of the analytical method, the traceability of the measurement result and the uncertainty of the result. This work promotes the introduction of metrology principles for chemical measurement with emphasis to the LA-ICP-MS which is the comparative method that requires studious approach to the development of the analytical procedure in order to acquire reliable quantitative results. Copyright © 2018 Elsevier B.V. All rights reserved.

  4. 230Th, 232Th and 238U determinations in phosphoric acid fertilizer and process products by ICP-MS

    International Nuclear Information System (INIS)

    Nascimento, Marcos R.L. do; Guerreiro, Luisa M.R.; Bonifacio, Rodrigo L.; Taddei, Maria H.T.

    2015-01-01

    Through processing of Santa Quiteria-CE mine phosphate rock, Brazil has established a project for production of phosphoric acid fertilizer and uranium as a by-product. Under leaching conditions of phosphate rock with sulfuric acid, which is the common route for preparing phosphoric acid fertilizer, a large part of uranium, thorium and their decay products naturally present in the rock are solubilized. In order to assess the contamination potential in phosphoric acid and others process products, this paper describes a previous precipitation and direct methods for routine analysis of thorium and uranium isotopes by ICP-MS. In all samples, 230 Th, 232 Th and 238 U were directly determined after dilution, except 230 Th in phosphoric acid loaded with uranium sample, which to overcome equipment contamination effect, was determined after its separation by oxalate precipitation using lanthanum as a carrier. The results obtained by the proposed method by ICP-MS, were in good agreement when compared to alpha spectrometry for 230 Th, and ICP-OES and spectrophotometry with arsenazo III for elementary uranium and thorium determinations. (author)

  5. Improved Precision and Accuracy of Quantification of Rare Earth Element Abundances via Medium-Resolution LA-ICP-MS.

    Science.gov (United States)

    Funderburg, Rebecca; Arevalo, Ricardo; Locmelis, Marek; Adachi, Tomoko

    2017-11-01

    Laser ablation ICP-MS enables streamlined, high-sensitivity measurements of rare earth element (REE) abundances in geological materials. However, many REE isotope mass stations are plagued by isobaric interferences, particularly from diatomic oxides and argides. In this study, we compare REE abundances quantitated from mass spectra collected with low-resolution (m/Δm = 300 at 5% peak height) and medium-resolution (m/Δm = 2500) mass discrimination. A wide array of geological samples was analyzed, including USGS and NIST glasses ranging from mafic to felsic in composition, with NIST 610 employed as the bracketing calibrating reference material. The medium-resolution REE analyses are shown to be significantly more accurate and precise (at the 95% confidence level) than low-resolution analyses, particularly in samples characterized by low (ICP-MS methods, particularly those relying on mass analyzers that do not offer tuneable mass-resolution and/or collision cell technologies that can reduce oxide and/or argide formation. Graphical Abstract ᅟ.

  6. An approach for quantification of platinum distribution in tissues by LA-ICP-MS imaging using isotope dilution analysis.

    Science.gov (United States)

    Moraleja, I; Mena, M L; Lázaro, A; Neumann, B; Tejedor, A; Jakubowski, N; Gómez-Gómez, M M; Esteban-Fernández, D

    2018-02-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been revealed as a convenient technique for trace elemental imaging in tissue sections, providing elemental 2D distribution at a quantitative level. For quantification purposes, in the last years several approaches have been proposed in the literature such as the use of CRMs or matrix matched standards. The use of Isotope Dilution (ID) for quantification by LA-ICP-MS has been also described, being mainly useful for bulk analysis but not feasible for spatial measurements so far. In this work, a quantification method based on ID analysis was developed by printing isotope-enriched inks onto kidney slices from rats treated with antitumoral Pt-based drugs using a commercial ink-jet device, in order to perform an elemental quantification in different areas from bio-images. For the ID experiments 194 Pt enriched platinum was used. The methodology was validated by deposition of natural Pt standard droplets with a known amount of Pt onto the surface of a control tissue, where could be quantified even 50pg of Pt, with recoveries higher than 90%. The amount of Pt present in the whole kidney slices was quantified for cisplatin, carboplatin and oxaliplatin-treated rats. The results obtained were in accordance with those previously reported. The amount of Pt distributed between the medullar and cortical areas was also quantified, observing different behavior for the three drugs. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Magnetic sulfur-doped porous carbon for preconcentration of trace mercury in environmental water prior to ICP-MS detection.

    Science.gov (United States)

    Peng, Chuyu; He, Man; Chen, Beibei; Huang, Lijin; Hu, Bin

    2017-11-20

    A novel magnetic sulfur-doped porous carbon (MSPC) was fabricated via a simple one-step carbonization of a mixture of sucrose, basic magnesium sulfate whiskers and Fe 3 O 4 @SiO 2 nanoparticles. Due to the high S content, the prepared MSPC possessed high adsorption capacity for Hg 2+ (343 mg g -1 ) with good selectivity. Based on this, a method coupling magnetic solid phase extraction (MSPE) with inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Hg 2+ in environmental water samples. Various parameters such as pH, desorption solvent and its concentration, desorption volume and time, sample volume, and adsorption time that affect the determination have been optimized. Under the optimal conditions, a high enrichment factor of 100-fold was obtained, the limit of detection (LOD) was found to be 0.52 pg mL -1 with a relative standard deviation (c = 10 pg mL -1 , n = 7) of 7.1%, and a good linearity was obtained within the concentration range of 2-5000 pg mL -1 for Hg 2+ . Besides, the proposed method has very fast adsorption/desorption kinetics, target Hg 2+ could be rapidly adsorbed on the prepared MSPC in 2 min and desorbed from the MSPC in 2 min with the assistance of a permanent magnet. Therefore, the proposed method of MSPE-ICP-MS exhibits good application potential in the determination of trace Hg 2+ in environmental water samples.

  8. Combination of ICP-MS, capillary electrophoresis, and their hyphenation for probing Ru(III) metallodrug-DNA interactions.

    Science.gov (United States)

    Foteeva, Lidia S; Matczuk, Magdalena; Pawlak, Katarzyna; Aleksenko, Svetlana S; Nosenko, Sergey V; Karandashev, Vasily K; Jarosz, Maciej; Timerbaev, Andrei R

    2017-03-01

    Determination of the DNA-binding reactivity and affinity is an important part of a successful program for the selection of metallodrug candidates. For such assaying, a range of complementary analytical techniques was proposed and tested here using one of few anticancer metal-based drugs that are currently in clinical trials, indazolium trans-[tetrachloridobis(1H-indazole)ruthenate(III), and a DNA oligonucleotide. A high reactivity of the Ru drug was confirmed in affinity capillary electrophoresis (CE) mode, where adduct formation takes place in situ (i.e., in the capillary filled with an oligonucleotide-containing electrolyte). To further characterize the binding kinetics, a drug-oligonucleotide mixture was incubated for a different period of time, followed by ultrafiltration separation into two different in molecular weight fractions (>3 and ICP-MS), revealing that at least two DNA adducts exist at equilibrium conditions. Using standalone ICP-MS, dominant equilibrium amount of the bound ruthenium was found to occur in a fraction of 5-10 kDa, which includes the oligonucleotide (ca. 6 kDa). Importantly, in all three assays, the drug was used for the first time in in-vitro studies, not in the intact form but as its active species released from the transferrin adduct at simulated cancer cytosolic conditions. This circumstance makes the established analytical platform promising to provide a detailed view on metallodrug targeting, including other possible biomolecules and ex vivo samples.

  9. Cellular processing of gold nanoparticles: CE-ICP-MS evidence for the speciation changes in human cytosol.

    Science.gov (United States)

    Legat, Joanna; Matczuk, Magdalena; Timerbaev, Andrei R; Jarosz, Maciej

    2018-01-01

    The cellular uptake of gold nanoparticles (AuNPs) may (or may not) affect their speciation, but information on the chemical forms in which the particles exist in the cell remains obscure. An analytical method based on the use of capillary electrophoresis hyphenated with inductively coupled plasma mass spectrometry (ICP-MS) has been proposed to shed light on the intracellular processing of AuNPs. It was observed that when being introduced into normal cytosol, the conjugates of 10-50 nm AuNPs with albumin evolved in human serum stayed intact. On the contrary, under simulated cancer cytosol conditions, the nanoconjugates underwent decomposition, the rate of which and the resulting metal speciation patterns were strongly influenced by particle size. The new peaks that appeared in ICP-MS electropherograms could be ascribed to nanosized species, as upon ultracentrifugation, they quantitatively precipitated whereas the supernatant showed only trace Au signals. Our present study is the first step to unravel a mystery of the cellular chemistry for metal-based nanomedicines.

  10. Laser ablation: Laser parameters: Frequency, pulse length, power, and beam charter play significant roles with regard to sampling complex samples for ICP/MS analysis

    International Nuclear Information System (INIS)

    Smith, M.R.; Alexander, M.L.; Hartman, J.S.; Koppenaal, D.W.

    1996-01-01

    Inductively coupled plasma mass spectrometry is used to investigate the influence of laser parameters with regard to sampling complex matrices ranging from relatively homogenous glasses to multi-phase sludge/slurry materials including radioactive Hanford tank waste. The resulting plume composition caused by the pulsed laser is evaluated as a function of wavelength, pulse energy, pulse length, focus, and beam power profiles. The author's studies indicate that these parameters play varying and often synergistic roles regarding quantitative results. (In a companion paper, particle transport and size distribution studies are presented.) The work described here will illustrate other laser parameters such as focusing and consequently power density and beam power profiles which are shown to influence precision and accuracy. Representative sampling by the LA approach is largely dependent on the sample's optical properties as well as laser parameters. Experimental results indicate that optimal laser parameters; short wavelength (UV), relatively low power (300 mJ), low-to-sub ns pulse lengths, and laser beams with reasonable power distributions (i.e., Gaussian or top-hat beam profiles) provide superior precision and accuracy. Remote LA-ICP/MS analyses of radioactive sludges are used to illustrate these optimal conditions laser ablation sampling

  11. High temperature liquid chromatography hyphenated with ESI-MS and ICP-MS detection for the structural characterization and quantification of halogen containing drug metabolites

    International Nuclear Information System (INIS)

    Vlieger, Jon S.B. de; Giezen, Mark J.N.; Falck, David; Tump, Cornelis; Heuveln, Fred van; Giera, Martin; Kool, Jeroen; Lingeman, Henk; Wieling, Jaap; Honing, Maarten; Irth, Hubertus; Niessen, Wilfried M.A.

    2011-01-01

    Highlights: → Hyphenation of high temperature liquid chromatography to ICP-MS and ESI-MS. → Structural characterization of kinase inhibitor metabolites with high resolution MS n experiments. → Quantification of drug metabolites with ICP-MS based on Iodine detection. → Significant changes in ESI-MS response after small structural changes. - Abstract: In this paper we describe the hyphenation of high temperature liquid chromatography with ICP-MS and ESI-MS for the characterization of halogen containing drug metabolites. The use of temperature gradients up to 200 deg. C enabled the separation of metabolites with low organic modifier content. This specific property allowed the use of detection methods that suffer from (significant) changes in analyte response factors as a function of the organic modifier content such as ICP-MS. Metabolites of two kinase inhibitors (SB-203580-Iodo and MAPK inhibitor VIII) produced by bacterial cytochrome P450 BM3 mutants and human liver microsomes were identified based on high resolution MS n data. Quantification was done using their normalized and elemental specific response in the ICP-MS. The importance of these kinds of quantification strategies is stressed by the observation that the difference of the position of one oxygen atom in a structure can greatly affect its response in ESI-MS and UV detection.

  12. Study on procedure for determination of Cr, As, Se, Cd, Hg, Pb in some kinds of herb products such as: kind of fungus, philamin... by ICP-MS

    International Nuclear Information System (INIS)

    Pham Ngoc Khai; Do Van Thuan; Nguyen Thi Kim Dung; Nguyen Hong Minh

    2007-01-01

    The determination of Cr, As, Se, Cd, Hg, Pb in herb products such as: kind of fungus, philamin, etc by ICP-MS has been studied. The effects of the parameters of ICP-MS instrument, concentration of nitric acid and high concentration of some elements on the determination of Cr, As, Se, Cd, Hg, Pb by ICP-MS has been concerned. The study and choice the suitable internal standard for the accurate determination of Hg has been sold. The suitable parameters of the microwave, composition and content of the acid mixture for the complete decomposition of the sample have been studied. The recommended procedure has been applied to the determination of Cr, As, Se, Cd, Hg, Pb in the standard samples and real samples. The error of the results is acceptable. (author)

  13. Determination of 236U and transuranium elements in depleted uranium ammunition by α-spectrometry and ICP-MS

    International Nuclear Information System (INIS)

    Desideri, D.; Meli, M.A.; Roselli, C.; Testa, C.; Boulyga, S.F.; Becker, J.S.

    2002-01-01

    It is well known that ammunition containing depleted uranium (DU) was used by NATO during the Balkan conflict. To evaluate the origin of DU (the enrichment of natural uranium or the reprocessing of spent nuclear fuel) it is necessary to directly detect the presence of activation products ( 236 U, 239 Pu, 240 Pu, 241 Am, and 237 Np) in the ammunition. In this work the analysis of actinides by α-spectrometry was compared with that by inductively coupled plasma mass spectrometry (ICP-MS) after selective separation of ultratraces of transuranium elements from the uranium matrix. 242 Pu and 243 Am were added to calculate the chemical yield. Plutonium was separated from uranium by extraction chromatography, using tri-n-octylamine (TNOA), with a decontamination factor higher than 10 6 ; after elution plutonium was determined by ICP-MS ( 239 Pu and 240 Pu) and α-spectrometry ( 239+240 Pu) after electroplating. The concentration of Pu in two DU penetrator samples was 7 x 10 -12 g g -1 and 2 x 10 -11 g g -1 . The 240 Pu/ 239 Pu isotope ratio in one penetrator sample (0.12±0.04) was significantly lower than the 240 Pu/ 239 Pu ratios found in two soil samples from Kosovo (0.35±0.10 and 0.27±0.07). 241 Am was separated by extraction chromatography, using di(2-ethylhexyl)phosphoric acid (HDEHP), with a decontamination factor as high as 10 7 . The concentration of 241 Am in the penetrator samples was 2.7 x 10 -14 g g -1 and -15 g g -1 . In addition 237 Np was detected at ultratrace levels. In general, ICP-MS and α-spectrometry results were in good agreement.The presence of anthropogenic radionuclides ( 236 U, 239 Pu, 240 Pu, 241 Am, and 237 Np) in the penetrators indicates that at least part of the uranium originated from the reprocessing of nuclear fuel. Because the concentrations of radionuclides are very low, their radiotoxicological effect is negligible. (orig.)

  14. Determination of {sup 236}U and transuranium elements in depleted uranium ammunition by {alpha}-spectrometry and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Desideri, D.; Meli, M.A.; Roselli, C.; Testa, C. [General Chemistry Institute, Urbino University, Urbino (Italy); Boulyga, S.F.; Becker, J.S. [Central Department of Analytical Chemistry, Research Centre Juelich, Juelich (Germany)

    2002-11-01

    It is well known that ammunition containing depleted uranium (DU) was used by NATO during the Balkan conflict. To evaluate the origin of DU (the enrichment of natural uranium or the reprocessing of spent nuclear fuel) it is necessary to directly detect the presence of activation products ({sup 236}U, {sup 239}Pu, {sup 240}Pu, {sup 241}Am, and {sup 237}Np) in the ammunition. In this work the analysis of actinides by {alpha}-spectrometry was compared with that by inductively coupled plasma mass spectrometry (ICP-MS) after selective separation of ultratraces of transuranium elements from the uranium matrix. {sup 242}Pu and {sup 243}Am were added to calculate the chemical yield. Plutonium was separated from uranium by extraction chromatography, using tri-n-octylamine (TNOA), with a decontamination factor higher than 10{sup 6}; after elution plutonium was determined by ICP-MS ({sup 239}Pu and {sup 240}Pu) and {alpha}-spectrometry ({sup 239+240}Pu) after electroplating. The concentration of Pu in two DU penetrator samples was 7 x 10{sup -12} g g{sup -1} and 2 x 10{sup -11} g g{sup -1}. The {sup 240}Pu/{sup 239}Pu isotope ratio in one penetrator sample (0.12{+-}0.04) was significantly lower than the {sup 240}Pu/{sup 239}Pu ratios found in two soil samples from Kosovo (0.35{+-}0.10 and 0.27{+-}0.07). {sup 241}Am was separated by extraction chromatography, using di(2-ethylhexyl)phosphoric acid (HDEHP), with a decontamination factor as high as 10{sup 7}. The concentration of {sup 241}Am in the penetrator samples was 2.7 x 10{sup -14} g g{sup -1} and <9.4 x 10{sup -15} g g{sup -1}. In addition {sup 237}Np was detected at ultratrace levels. In general, ICP-MS and {alpha}-spectrometry results were in good agreement.The presence of anthropogenic radionuclides ({sup 236}U, {sup 239}Pu,{sup 240}Pu, {sup 241}Am, and {sup 237}Np) in the penetrators indicates that at least part of the uranium originated from the reprocessing of nuclear fuel. Because the concentrations of

  15. Determination of (236)U and transuranium elements in depleted uranium ammunition by alpha-spectrometry and ICP-MS.

    Science.gov (United States)

    Desideri, D; Meli, M A; Roselli, C; Testa, C; Boulyga, S F; Becker, J S

    2002-11-01

    It is well known that ammunition containing depleted uranium (DU) was used by NATO during the Balkan conflict. To evaluate the origin of DU (the enrichment of natural uranium or the reprocessing of spent nuclear fuel) it is necessary to directly detect the presence of activation products ((236)U, (239)Pu, (240)Pu, (241)Am, and (237)Np) in the ammunition. In this work the analysis of actinides by alpha-spectrometry was compared with that by inductively coupled plasma mass spectrometry (ICP-MS) after selective separation of ultratraces of transuranium elements from the uranium matrix. (242)Pu and (243)Am were added to calculate the chemical yield. Plutonium was separated from uranium by extraction chromatography, using tri- n-octylamine (TNOA), with a decontamination factor higher than 10(6); after elution plutonium was determined by ICP-MS ((239)Pu and (240)Pu) and alpha-spectrometry ((239+240)Pu) after electroplating. The concentration of Pu in two DU penetrator samples was 7 x 10(-12) g g(-1) and 2 x 10(-11) g g(-1). The (240)Pu/(239)Pu isotope ratio in one penetrator sample (0.12+/-0.04) was significantly lower than the (240)Pu/(239)Pu ratios found in two soil samples from Kosovo (0.35+/-0.10 and 0.27+/-0.07). (241)Am was separated by extraction chromatography, using di(2-ethylhexyl)phosphoric acid (HDEHP), with a decontamination factor as high as 10(7). The concentration of (241)Am in the penetrator samples was 2.7 x 10(-14) g g(-1) and <9.4 x 10(-15) g g(-1). In addition (237)Np was detected at ultratrace levels. In general, ICP-MS and alpha-spectrometry results were in good agreement. The presence of anthropogenic radionuclides ((236)U, (239)Pu,(240)Pu, (241)Am, and (237)Np) in the penetrators indicates that at least part of the uranium originated from the reprocessing of nuclear fuel. Because the concentrations of radionuclides are very low, their radiotoxicological effect is negligible.

  16. Simultaneous analysis of free and humic acid complexed europium and gadolinium species by CE-ICP-MS

    International Nuclear Information System (INIS)

    Kautenburger, R.; Nowotka, K.; Beck, H.P.

    2005-01-01

    Full text of publication follows: For the long-term safety assessment of waste repositories, detailed information about geo-chemical behaviour of radioactive and toxic metal ions under environmental conditions (geological matrix and aquifer systems) is necessary. It includes knowledge about the mechanism of relevant geochemical reactions, as well as thermodynamic and kinetic data. Several previous studies have shown that humic acid can play an important role in the immobilisation or mobilization of metal ions due to complexation and colloid formation. In this project we investigate the complexation behaviour of humic acid (purified Aldrich humic acid) and its influence on the migration of the lanthanides europium and gadolinium (homologues of the actinides americium and curium) in the the ternary system consisting of these heavy metals, humic acid and kaolinite (KGa-1b) as geological model system under conditions close to nature. Capillary electrophoresis (CE, Beckman Coulter P/ACE MDQ), with its excellent separation performance, was coupled to Inductively Coupled Plasma Mass Spectrometry (ICP-MS, VG Elemental Plasma Quad 3) to obtain a high sensitivity for the determination of the rare earth elements europium (Eu 3+ ) and gadolinium (Gd 3+ ) and their complexes with humic acid. Additionally, the used humic acid was halogenated with iodine as ICP-MS marker. A fused-silica capillary was flexibly fitted into a MicroMist 50 μl nebulizer with a Cinnabar cyclonic spray chamber. The chamber was chilled to a temperature of 4 deg. C for best sensitivity. 200 ppb of caesium were added to the CE separation buffer to observe the capillary flow. A make-up fluid including 4 ppb Ho as an internal standard was combined with the flow from the capillary within the interface to obtain a fluid throughput high enough to maintain a continuous nebulization. Very low detection limits were achieved, 100 ppt for 153 Eu and 125 ppt for 158 Gd. With this optimized CE-ICP-MS coupling

  17. Matrix-Matched Iron-Oxide Laser Ablation ICP-MS U–Pb Geochronology Using Mixed Solution Standards

    Directory of Open Access Journals (Sweden)

    Liam Courtney-Davies

    2016-08-01

    Full Text Available U–Pb dating of the common iron-oxide hematite (α-Fe2O3, using laser-ablation inductively-coupled-plasma mass-spectrometry (LA-ICP-MS, provides unparalleled insight into the timing and processes of mineral deposit formation. Until now, the full potential of this method has been negatively impacted by the lack of suitable matrix-matched standards. To achieve matrix-matching, we report an approach in which a U–Pb solution and ablated material from 99.99% synthetic hematite are simultaneously mixed in a nebulizer chamber and introduced to the ICP-MS. The standard solution contains fixed U- and Pb-isotope ratios, calibrated independently, and aspiration of the isotopically homogeneous solution negates the need for a matrix-matched, isotopically homogenous natural iron-oxide standard. An additional advantage of using the solution is that the individual U–Pb concentrations and isotope ratios can be adjusted to approximate that in the unknown, making the method efficient for dating hematite containing low (~10 ppm to high (>1 wt % U concentrations. The above-mentioned advantage to this solution method results in reliable datasets, with arguably-better accuracy in measuring U–Pb ratios than using GJ-1 Zircon as the primary standard, which cannot be employed for such low U concentrations. Statistical overlaps between 207Pb/206Pb weighted average ages (using GJ-1 Zircon and U–Pb upper intercept ages (using the U–Pb mixed solution method of two samples from iron-oxide copper-gold (IOCG deposits in South Australia demonstrate that, although fractionation associated with a non-matrix matched standard does occur when using GJ-1 Zircon as the primary standard, it does not impact the 207Pb/206Pb or upper intercept age. Thus, GJ-1 Zircon can be considered reliable for dating hematite using LA-ICP-MS. Downhole fractionation of 206Pb/238U is observed to occur in spot analyses of hematite. The use of rasters in future studies will hopefully minimize

  18. {sup 90}Sr in human excretion samples. Comparison of MC-ICP-MS and conventional low-level beta-counting; {sup 90}Sr in menschlichen Ausscheidungsproben. Vergleich zwischen MC-ICP-MS und konventioneller Low Level Beta-Messung

    Energy Technology Data Exchange (ETDEWEB)

    Burow, M.; Schumacher, C.; Zoriy, M. [Forschungszentrum Juelich GmbH (Germany). Geschaeftsbereich fuer Sicherheit und Strahlenschutz

    2016-07-01

    At the present for determination of {sup 90}Sr in different human excretion samples manly radiochemical methods are applied, for example LL-beta- counter or liquid scintillation method. These methods require an isolation of strontium from other interfering radioactive species such as e.g. lead, polonium, plutonium, neptunium and potassium (for example, separation on Sr Resin, Fa. Eichrom, France) and afterwards long counting time restrict the usage in some application fields. On the other hand, the liquid scintillation techniques that may be used for detection present a challenge in the analysis of {sup 90}Sr in the presence of {sup 90}Y. However spectra of both radionuclides overlap in a certain zone and this may be resolved by mathematical calculations of {sup 90}Y ingrowth or by simply waiting for radiochemical equilibrium to be reached (2-3 weeks). In the case of emergency, monitoring of operating personal or civil population for possible incorporation of {sup 90}Sr via excretion samples a readily available, faster and reliable analytical procedure may prove to be of great importance. For these purposes, an analytical method for the determination of {sup 90}Sr in urine with high-sensitive MC-ICP-MS was developed in the radiochemical laboratory of the Department for Safety and Radiation Protection. The method was optimized to avoid a multitude of isobaric interferences that occur on m/z 90 using a cold-plasma operation condition of ICP-MS. The reported LOD as low as 0,3-1 Bq/l in the water samples was found to be acceptable for majority of our analytical tasks.

  19. Development of methodologies used in the areas of safeguards and nuclear forensics based on LA-HR-ICP-MS technique; Desenvolvimento de metodologias utilizadas nas areas de salvaguardas e forense nuclear baseadas na tecnica LA-HR-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Marin, Rafael Coelho

    2013-07-01

    Environmental sampling performed by means of swipe samples is a methodology frequently employed by International Atomic Energy Agency (IAEA) to verify if the signatory States of the Safeguards Agreements are conducing unauthorized activities. Swipe samples analysis is complementary to the Safeguards ordinary procedures used to verify the information given by the States. In this work it was described a methodology intending to strengthen the nuclear safeguards and nuclear forensics procedures. The proposal is to study and evaluate the laser ablation high resolution inductively coupled plasma mass spectrometry (LA-HR-ICP-MS) technique as an alternative to analyze the real-life swipe samples. The precision achieved through the standard (CRM - 125A) measurements, represented by the relative standard deviation (RSD), was respectively 1.3 %, 0.2 % e 7.6 % for the {sup 234}U/{sup 238}U, {sup 235}U/{sup 238}U e {sup 236}U/{sup 238}U isotopes ratios. The percent uncertainties (u %), which covers the RSD, ranged from 3.5 % to 29.8 % to the {sup 235}U/{sup 238}U measurements and from 16.6 % to 42.9 % to the {sup 234}U/{sup 238}U isotope ratio. These results were compatible with former studies performed by the LA-HR-ICP-MS that analyzed real-life swipe samples collected at a nuclear facility. Swipe samples collected from several points of the nuclear facility presented enrichment level ranging from (2.3 ± 0.7) % (sample 3) to (17.3 ± 2.8) % (sample 18). They also allowed detecting different enrichment levels within the facility. (author)

  20. Arsenic speciation in biological environmental samples of aquatic ecosystems by using HPLC-ICP-MS; Speciation von Arsen in biologischen Umweltproben aus aquatischen Oekosystemen mittels HPLC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Falk, K.

    1999-09-01

    The physicochemical forms of arsenic (arsenic species) which are present in the environment vary significantly with respect to toxicity, bioavailability, stability and transport behaviour. Therefore, it is necessary for an assessment of the toxic potential to humans and the environment to investigate not only the total arsenic concentrations but also to differentiate the single species. By that the knowledge about ecological correlations and pathways will be increased. The present thesis reports the results of a Ph.D. study on the development and optimisation of analytical methods for arsenic speciation and their application to biological samples from different aquatic ecosystems in Germany. The method development included separation of 12 naturally occurring arsenic species by high-performance liquid chromatography (HPLC) followed by an arsenic selective detection by inductively coupled plasma-mass spectrometry (ICP-MS). The arsenic species As (III), As (V), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AB), arsenocholine (AC), trimethylarsine oxid (TMAO) and tetramethylarsonium (Tetra) were separated with ion-exchange chromatography, whereas reversed-phase chromatography was used for the separation of four arsenosugars. Because of the partly low arsenic concentration in biological samples a very good detection power was required. Therefore, an HPLC-ICP-MS system was tested with different nebulizers. Using the high efficiency nebulizer HHPN (Hydraulic High Pressure Nebulizer), detection limits in the low pg-range could be achieved. The developed analytical methods were applied to arsenic speciation in four marine matrices, which are representative of different trophic levels in the food chain. All samples originated from an ecosystem in the North Sea.

  1. Application of isotope-dilution laser ablation ICP-MS for direct determination of Pu concentrations in soils at pg g(-1) levels.

    Science.gov (United States)

    Boulyga, Sergei F; Tibi, Markus; Heumann, Klaus G

    2004-01-01

    The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3x10(-13) g g(-1) for Pu isotopes in soil samples containing uranium at a concentration of a few microg g(-1). The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH+ and PbO2+ ions and by the peak tail of 238U+ ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of alpha-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of (239+240)Pu (9.8 +/- 3.0 mBq g(-1)) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4 +/- 0.2 mBq g(-1). However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if "hot" particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples.

  2. Application of isotope-dilution laser ablation ICP-MS for direct determination of Pu concentrations in soils at pg g-1 levels

    International Nuclear Information System (INIS)

    Boulyga, Sergei F.; Tibi, Markus; Heumann, Klaus G.

    2004-01-01

    The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3 x 10 -13 g g -1 for Pu isotopes in soil samples containing uranium at a concentration of a few μg g -1 . The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH + and PbO 2 + ions and by the peak tail of 238 U + ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of α-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of 239+240 Pu (9.8±3.0 mBq g -1 ) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4±0.2 mBq g -1 . However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if ''hot'' particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples. (orig.)

  3. In situ quantification of Br and Cl in minerals and fluid inclusions by LA-ICP-MS: a powerful tool to identify fluid sources

    Science.gov (United States)

    Hammerli, Johannes; Rusk, Brian; Spandler, Carl; Emsbo, Poul; Oliver, Nicholas H.S.

    2013-01-01

    Bromine and chlorine are important halogens for fluid source identification in the Earth's crust, but until recently we lacked routine analytical techniques to determine the concentration of these elements in situ on a micrometer scale in minerals and fluid inclusions. In this study, we evaluate the potential of in situ Cl and Br measurements by LA-ICP-MS through analysis of a range of scapolite grains with known Cl and Br concentrations. We assess the effects of varying spot sizes, variable plasma energy and resolve the contribution of polyatomic interferences on Br measurements. Using well-characterised natural scapolite standards, we show that LA-ICP-MS analysis allows measurement of Br and Cl concentrations in scapolite, and fluid inclusions as small as 16 μm in diameter and potentially in sodalite and a variety of other minerals, such as apatite, biotite, and amphibole. As a demonstration of the accuracy and potential of Cl and Br analyses by LA-ICP-MS, we analysed natural fluid inclusions hosted in sphalerite and compared them to crush and leach ion chromatography Cl/Br analyses. Limit of detection for Br is ~8 μg g−1, whereas relatively high Cl concentrations (> 500 μg g−1) are required for quantification by LA-ICP-MS. In general, our LA-ICP-MS fluid inclusion results agree well with ion chromatography (IC) data. Additionally, combined cathodoluminescence and LA-ICP-MS analyses on natural scapolites within a well-studied regional metamorphic suite in South Australia demonstrate that Cl and Br can be quantified with a ~25 μm resolution in natural minerals. This technique can be applied to resolve a range of hydrothermal geology problems, including determining the origins of ore forming brines and ore deposition processes, mapping metamorphic and hydrothermal fluid provinces and pathways, and constraining the effects of fluid–rock reactions and fluid mixing.

  4. Determination and identification of hydrophilic and hydrophobic arsenic species in methanol extract of fresh cod liver by RP-HPLC with simultaneous ICP-MS and ESI-Q-TOF-MS detection.

    Science.gov (United States)

    Arroyo-Abad, Uriel; Lischka, Susanne; Piechotta, Christian; Mattusch, Jürgen; Reemtsma, Thorsten

    2013-12-01

    The present study was focused on the determination and identification of arsenic species in methanolic extracts of cod liver. Arsenic species were fractionated and the fractions analysed by RP-HPLC-ICP-MS coupled with ESI-Q-TOF-MS. The total concentration of arsenic in the fresh cod liver was analysed by ICP-MS to be 1.53±0.02 mg As kg(-1)w.w. and the extraction recovery was ca. 100% and the column recovery >93%. Besides polar inorganic and methylated arsenic species (>70%) more hydrophobic arsenic-containing fatty acids and hydrocarbons occurred. Based on the mass spectrometric data proposals for molecular structures were elaborated for 20 of the organic As species included 10 arsenic-containing fatty acids (AsFA) and an arsenic-containing hydrocarbon (AsHC) mentioned for the first time in fresh cod liver. Arsenobetaine was found as main water-soluble arsenic compound in cod liver followed by higher molecular mass arsenic-containing fatty acids and hydrocarbons. Copyright © 2013 Elsevier Ltd. All rights reserved.

  5. Determination of 241Am in sediments by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS).

    Science.gov (United States)

    Agarande, M; Benzoubir, S; Bouisset, P; Calmet, D

    2001-08-01

    Trace levels (pg kg(-1)) of 241Am in sediments were determined by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS) using a microconcentric nebulizer. 241Am was isolated from major elements like Ca and Fe by different selective precipitations. In further steps. Am was first separated from other transuranic elements and purified by anion exchange and extraction chromatography prior to the mass spectrometric measurements. The ID HR ICP-MS results are compared with isotope dilution alpha spectrometry.

  6. Imaging of Selenium by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) in 2-D Electrophoresis Gels and Biological Tissues.

    Science.gov (United States)

    Cruz, Elisa Castañeda Santa; Susanne Becker, J; Sabine Becker, J; Sussulini, Alessandra

    2018-01-01

    Selenium and selenoproteins are important components of living organisms that play a role in different biological processes. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is a powerful analytical technique that has been employed to obtain distribution maps of selenium in biological tissues in a direct manner, as well as in selenoproteins, previously separated by their molecular masses and isoelectric points using two-dimensional polyacrylamide gel electrophoresis (2-D PAGE). In this chapter, we present the protocols to perform LA-ICP-MS imaging experiments, allowing the distribution visualization and determination of selenium and/or selenoproteins in biological systems.

  7. A novel strategy to evaluate the degradation of quantum dots: identification and quantification of CdTe quantum dots and corresponding ionic species by CZE-ICP-MS.

    Science.gov (United States)

    Meng, Peijun; Xiong, Yamin; Wu, Yingting; Hu, Yue; Wang, Hui; Pang, Yuanfeng; Jiang, Shuqing; Han, Sihai; Huang, Peili

    2018-05-09

    In view of the significance and urgency of the speciation analysis of quantum dots (QDs) and their degradation products for clarifying their degradation rules and toxicity mechanisms, a method for the identification and quantification of CdTe QDs and corresponding ionic species in complex matrices was developed using capillary zone electrophoresis (CZE) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). The quality assessment of commercial CdTe QDs and serum pharmacokinetics of synthesized CdTe QDs in rats were successfully undertaken using the developed CZE-ICP-MS method.

  8. TEM and SP-ICP-MS analysis of the release of silver nanoparticles from decoration of pastry.

    Science.gov (United States)

    Verleysen, E; Van Doren, E; Waegeneers, N; De Temmerman, P-J; Abi Daoud Francisco, M; Mast, J

    2015-04-08

    Metallic silver is an EU approved food additive referred to as E174. It is generally assumed that silver is only present in bulk form in the food chain. This work demonstrates that a simple treatment with water of "silver pearls", meant for decoration of pastry, results in the release of a subfraction of silver nanoparticles. The number-based size and shape distributions of the single, aggregated, and/or agglomerated particles released from the silver pearls were determined by combining conventional bright-field TEM imaging with semiautomatic particle detection and analysis. In addition, the crystal structure of the particles was studied by electron diffraction and chemical information was obtained by combining HAADF-STEM imaging with EDX spectroscopy and mapping. The TEM results were confirmed by SP-ICP-MS. The representative Ag test nanomaterial NM-300 K was used as a positive control to determine the uncertainty on the measurement of the size and shape of the particles.

  9. Health impacts of mercury cycling in contaminated environments of Central India studied by NAA and ICP-MS

    International Nuclear Information System (INIS)

    Patel, Khageshwar Singh

    2002-01-01

    The environmental and atmospheric samples i.e. surface water, ground water, surface soil, sediment, rain and fog from various sites of contaminated environments of central India were collected in year, 2000-2001. The concentration levels of total-Hg in these samples were analyzed by using techniques i.e. cold vapor- atomic absorption spectrophotometer (CV-AAS), X-ray fluorescence spectrophotometer XFS). Further, the data base of total Hg in the environmental samples would be validated in other laboratories i.e. Prof Dr. Klaus Heumann (Johannes Gutenberg-University, Mainz, Germany), David Amouroux (University of Pau, France) and Dr Joerg Feldmann (University of Aberdeen, Scotland, UK) for exploration of the Hg-contaminated environments by using techniques i.e. ICP-MS/GC, gas chromatography-induced couple atomic emission spectrophotometer (GC-ICP-AES), neutron activation analysis (NAA). (author)

  10. Determination of uranium in boric acid samples at Paks Nuclear Power Plant by ICP-MS method

    International Nuclear Information System (INIS)

    Komlosi, E.Zs.; Menyhart, A.; Varju, I.

    2005-01-01

    Measurement of uranium became necessary in 2003, after the incident of unit 2 in April, when the fission products, uranium and transuranium isotopes got into the cooling water. The measurement of uranium with ICP-MS method was initiated in January 2004. Apparatus type Agilent 7500a was used. Uranium concentration and uranium isotope ratio were measured in samples with different - but known - boric acid concentration. Internal standard was used for the elimination of the matrix effect. The samples have high boric acid concentration (in few samples over 20 g/litres). Two methods were used for the reduction of the boric acid concentration: dilution and evaporation with ethyl alcohol. Both methods were found successful and exact. The limit of detection is 0.1 ng/litres for the Uranium-238. (N.T.)

  11. Determination of selenium in red blood cells by inductively coupled plasma mass spectrometry (ICP-MS) after microwave digestion

    International Nuclear Information System (INIS)

    Tinggi, U.; Francis, R.; Shanin, M.; Scheelings, P.; Gianduzzo, T.; Nicol, D.

    2004-01-01

    Selenium is an essential trace element and its levels in blood have been widely used for assessing Se status in humans. A suitable method for the determination of Se in red blood cells (RBC) using ICP-MS after microwave digestion was developed. The blood samples were obtained from patients with benign prostatic hyperplasia (BPH), who attended urology clinics at the Princess Alexandra hospital, Brisbane, Australia. No apparent polyatomic and matrix interferences were encountered when 82 Se isotope was used for the analysis of Se levels in RBC. Whole Blood Seronorm Trace Elements (SERO, Norway) and dogfish muscle (DORM-1, NRCC) were used as reference materials for method validation. The method was rapid and accurate, and ideal for routine analysis of Se in RBC, and in particular for assessing of Se status in humans. (author)

  12. Health impacts of mercury cycling in contaminated environments of central India studied by NAA and ICP-MS

    International Nuclear Information System (INIS)

    Patel, K.S.

    2001-01-01

    The heavy metal pollution in the Indian continent is increasing due to rapid industrialisation. Among heavy metals, the element: mercury is considered as global pollutant. In central India it is considered as global pollutant. Central India has been chosen for the investigation of the mercury pollution and their health impacts in the proposed project. The concentration and flux levels of the organic, inorganic and total mercury and their variations, sources and co-relation are investigated in various atmospheric and environmental compartments air, dry deposit, wet deposits, water, soil, sediment, etc. of central India lying between 18-23 deg. N latitude and 80-84 deg. longitude. The techniques CVAAS, NAA, XFS, ICP-MS, etc. would be used for monitoring the various chemical species of mercury employing established methodologies. (author)

  13. Detection of lead nanoparticles in game meat by single particle ICP-MS following use of lead-containing bullets

    DEFF Research Database (Denmark)

    Kollander, Barbro; Widemo, Fredrik; Ågren, Erik

    2017-01-01

    This study investigated whether game meat may contain nanoparticles of lead from ammunition. Lead nanoparticles in the range 40 to 750 nm were detected by ICP-MS in single particle mode in game shot with lead-containing bullets. The median diameter of the detected nanoparticles was around 60 nm....... The particle mass concentration ranged from 290 to 340 ng/g meat and the particle number concentrations from 27 to 50 million particles/g meat. The size limit of detection strongly depended on the level of dissolved lead and was in the range of 40 to 80 nm. In game meat sampled more than 10 cm away from...... the wound channel, no lead particles with a diameter larger than 40 nm were detected. In addition to dissolved lead in meat that originated from particulates, the presence of lead nano particles in game meat represents a hitherto unattended source of lead with a largely unknown toxicological impact...

  14. Spectrochemical pure cerium dioxide preparation and its quality control by inductively coupled plasma and mass spectrometry (ICP/MS)

    International Nuclear Information System (INIS)

    Da Silva Queiroz, C.A.; De Souza, J.E.; Abrao, A.

    1998-01-01

    Full text: A simple and economic procedure for the purification until 500 g CeO 2 batch is presented. The purified material will be used as spectrochemical standard. It is obtained by association of the fractional precipitation technique in the system REC 3 /H 2 O 2 /NH 4 OH to enrich the cerium up to 90% and then refined by ion exchange up to 99.9% CeO2. The 99,9% CeO 2 warranty control of purity was accomplished by inductively coupled plasma and mass spectrometry (ICP/ MS) and compared with activation analysis data, exhibiting impurities traces of same values of the international spec pure standard. The following results (average values) for the contaminant rare earths are (ppm):La(36), Pr(19), Nd(161), Sm(11), Eu(5,3),Gd(113),Tb(89),Dy(2),Ho(0.05),Er(1), Tm(0), Yb(11), Lu (19) and Y(2.1), respectively

  15. Measurement of 240Pu/239Pu isotopic ratios in soils from the Marshall Islands using ICP-MS.

    Science.gov (United States)

    Muramatsu, Y; Hamilton, T; Uchida, S; Tagami, K; Yoshida, S; Robison, W

    2001-10-20

    Nuclear weapons tests conducted by the United States in the Marshall Islands produced significant quantities of regional or tropospheric fallout contamination. Here we report on some preliminary inductively coupled plasma-mass spectrometry (ICP-MS) measurements of plutonium isolated from seven composite soil samples collected from Bikini, Enewetak and Rongelap Atolls in the northern Marshall Islands. These data show that 240Pu/239Pu isotopic signatures in surface soils from the Marshall Island vary significantly and could potentially be used to help quantify the range and extent of fallout deposition (and associated impacts) from specific weapons tests. 137Cs and 60Co were also determined on the same set of soil samples for comparative purposes.

  16. Trace element analysis in quartz by using laser ablation ICP-MS: A tool for deciphering magma evolution

    Czech Academy of Sciences Publication Activity Database

    Svojtka, Martin; Ackerman, Lukáš; Breiter, Karel

    2011-01-01

    Roč. 75, č. 3 (2011), s. 1972-1972 ISSN 0026-461X. [Goldschmidt Conference. 14.08.2011-19.08.2011, Prague] R&D Projects: GA ČR GAP210/10/1105 Institutional research plan: CEZ:AV0Z30130516 Keywords : quart2 * granite * rhyolite * trace elements * LA-ICP-MS Subject RIV: DD - Geochemistry http://docserver.ingentaconnect.com/deliver/connect/minsoc/0026461x/v75n3/s19.pdf?expires=1325856038&id=66552841&titleid=895&accname=Geological+institute+ASCR+library&checksum=7D602E3E9A0822A467A5A0278C6CB325

  17. Development of new applications of inductively coupled plasma mass spectrometry (ICP-MS) hyphenated with different sample introduction systems

    OpenAIRE

    Ugarte Baztán, Ana

    2014-01-01

    225 p. : il. Texto en español con conclusiones en inglés Hoy en día, la espectrometría de masas con plasma de acoplamiento inductivo (ICP-MS) es una de las técnicas más potentes y versátiles para el análisis de elementos traza dada su robustez y bajos límites de detección. En el presente trabajo se pretende ampliar el abanico de aplicaciones de esta técnica desarrollando nuevas combinaciones de la misma a distintos sistemas de introducción de muestra. En primera lugar, se presenta el a...

  18. Measurement of 240Pu/239Pu isotopic ratios in soils from the Marshall Islands using ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Muramatsu, Y.; Uchida, S.; Tagami, K.; Yoshida, S. [Environmental and Toxicological Researches Group, National Institute of Radiological Sciences, Anagawa 4-9-1, Inage-ku, 263-8555 Chiba (Japan); Hamilton, T.; Robison, W. [Health and Ecological Assessment Division, Lawrence Livermore National Laboratory, P.O. Box 808, L-453, 94551-0808 Livermore, CA (United States)

    2001-10-20

    Nuclear weapons tests conducted by the United States in the Marshall Islands produced significant quantities of regional or tropospheric fallout contamination. Here we report on some preliminary inductively coupled plasma-mass spectrometry (ICP-MS) measurements of plutonium isolated from seven composite soil samples collected from Bikini, Enewetak and Rongelap Atolls in the northern Marshall Islands. These data show that 240Pu/239Pu isotopic signatures in surface soils from the Marshall Island vary significantly and could potentially be used to help quantify the range and extent of fallout deposition (and associated impacts) from specific weapons tests. 137Cs and 60Co were also determined on the same set of soil samples for comparative purposes.

  19. Measurement of 240Pu/239Pu isotopic ratios in soils from the Marshall Islands using ICP-MS

    International Nuclear Information System (INIS)

    Muramatsu, Y.; Uchida, S.; Tagami, K.; Yoshida, S.; Hamilton, T.; Robison, W.

    2001-01-01

    Nuclear weapons tests conducted by the United States in the Marshall Islands produced significant quantities of regional or tropospheric fallout contamination. Here we report on some preliminary inductively coupled plasma-mass spectrometry (ICP-MS) measurements of plutonium isolated from seven composite soil samples collected from Bikini, Enewetak and Rongelap Atolls in the northern Marshall Islands. These data show that 240Pu/239Pu isotopic signatures in surface soils from the Marshall Island vary significantly and could potentially be used to help quantify the range and extent of fallout deposition (and associated impacts) from specific weapons tests. 137Cs and 60Co were also determined on the same set of soil samples for comparative purposes

  20. Development and application of a method for Cr(III) determination in dairy products by HPLC-ICP-MS.

    Science.gov (United States)

    Hernandez, Fanny; Jitaru, Petru; Cormant, Florence; Noël, Laurent; Guérin, Thierry

    2018-02-01

    This study describes the development of an analytical approach for the determination of Cr(III) in dairy products by microwave assisted extraction, complexation in situ by ethylenediaminetetraacetate (EDTA) and high performance liquid chromatography hyphenated to inductively coupled plasma-mass spectrometry (HPLC-ICP-MS). The extraction step was optimised by using an experimental design. A limit of quantification of 38µgkg -1 dry weight (d.w.) was obtained whereas the bias (%) measured ranged from 10 to 18%. The repeatability and intermediate precision varied between 1.2-5.0% and 7.5-13.5%, respectively. The method was applied to the analysis of several dairy samples beforehand characterized in terms of Cr(VI) and total chromium (Cr total ). Cr(III) concentrations ranged from <13 to 255µgkg -1 d.w. The results showed a good agreement between Cr(III) and Cr total concentration levels. Copyright © 2017 Elsevier Ltd. All rights reserved.

  1. Biocompatible Polymer Nanoformulation To Improve the Release and Safety of a Drug Mimic Molecule Detectable via ICP-MS.

    Science.gov (United States)

    Ferrari, Raffaele; Talamini, Laura; Violatto, Martina Bruna; Giangregorio, Paola; Sponchioni, Mattia; Morbidelli, Massimo; Salmona, Mario; Bigini, Paolo; Moscatelli, Davide

    2017-01-03

    Fluorescent poly(ε-caprolactone)-based nanoparticles (NPs) have been synthesized and successfully loaded with a titanium organometallic compound as a mimic of a water-insoluble drug. The nature of this nanovector enabled us to combine the quantification of the metal in tissues after systemic administration in healthy immunocompetent mice by inductively coupled plasma mass spectroscopy (ICP-MS) followed by the visualization of NPs in organ sections by confocal microscopy. This innovative method of nanodrug screening has enabled us to elucidate the crucial parameters of their kinetics. The organometallic compound is a good mimic of most anticancer drugs, and this approach is an interesting starting point to design the relevance of a broad range of nanoformulations in terms of safety and targeted delivery of the cargoes.

  2. Determination of Trace and Volatile Element Abundance Systematics of Lunar Pyroclastic Glasses 74220 and 15426 Using LA-ICP-MS

    Science.gov (United States)

    McIntosh, E. Carrie; Porrachia, Magali; McCubbin, Francis M.; Day, James M. D.

    2017-01-01

    Since their recognition as pyroclastic glasses generated by volcanic fire fountaining on the Moon, 74220 and 15426 have garnered significant scientific interest. Early studies recognized that the glasses were particularly enriched in volatile elements on their surfaces. More recently, detailed analyses of the interiors of the glasses, as well as of melt inclusions within olivine grains associated with the 74220 glass beads, have determined high H2O, F, Cl and S contents. Such elevated volatile contents seem at odds with evidence from moderately volatile elements (MVE), such as Zn and K, for a volatile- depleted Moon. In this study, we present initial results from an analytical campaign to study trace element abundances within the pyroclastic glass beads. We report trace element data determined by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for 15426 and 74220.

  3. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Bentlin, Fabrina R.S. [Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501.970 Porto Alegre, RS (Brazil); Santos, Clarissa M.M. dos; Flores, Erico M.M. [Departamento de Quimica Universidade Federal de Santa Maria, 97105-900 Santa Maria, RS (Brazil); Pozebon, Dirce, E-mail: dircepoz@iq.ufrgs.br [Universidade Federal do Rio Grande do Sul, Av. Bento Goncalves 9500, 91501.970 Porto Alegre, RS (Brazil)

    2012-01-13

    Highlights: Black-Right-Pointing-Pointer Ultrasound was investigated and applied for red wine samples preparation. Black-Right-Pointing-Pointer Aliquots of 50 {mu}L of sample were nebulized and transported to plasma. Black-Right-Pointing-Pointer FI and pneumatic nebulization/aerosol desolvation were used. Black-Right-Pointing-Pointer LODs of the ICP-MS method for lanthanides determination were at ng L{sup -1} level. Black-Right-Pointing-Pointer Lanthanides concentration allowed red wines classification. - Abstract: This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 {mu}L of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L{sup -1}, respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration.

  4. Rapid age determination of oysters using LA-ICP-MS line scans of shell Mg/Ca ratios

    Science.gov (United States)

    Gillikin, D. P.; Durham, S. R.; Goodwin, D. H.

    2016-02-01

    Magnesium to calcium (Mg/Ca) ratios exhibit a strong temperature dependence in foraminifera and corals, but not in bivalve mollusks. Various studies have reported Mg/Ca-temperature relationships with R2 values ranging from 0.3 to 0.8 and significantly different relationships for bivalves growing at different salinities. However, this poor temperature correlation does not render Mg/Ca data useless. A weak temperature dependence would allow time (seasons and years) to be determined along the growth axis of shells. This would provide information about age, growth rate and also allow other proxies to be aligned with time. Typically, oxygen isotopes (δ18O) are used to age shells without clear periodic growth lines, which is time consuming and expensive. Line scans using laser ablation systems can cover several centimeters of shell in a few minutes. We test this method on the resilifer of two oyster species (Crassostrea gigas and C. virginica) using a 193 nm Laser-Ablation-ICP-MS. Living oysters were collected from San Francisco Bay, North Carolina, South Carolina, and the Gulf of Mexico; fossil shells (Pleistocene) were also collected in South Carolina. Shells were sampled for δ18O values and Mg/Ca ratios. We use annual cycles in δ18O values to confidently determine age, then apply the Mg/Ca technique. Shells of both species exhibit annual cyclicity in Mg/Ca ratios using spot and line scan laser sampling, which matche the seasonal cyclicity determined using δ18O values. Results show a good correlation between ages determined using the different methods. We conclude that LA-ICP-MS line scans offer a rapid and inexpensive technique for determining age, growth rate, and timing of shell growth in oyster reslifers.

  5. Combined U-Pb and Lu-Hf isotope analyses by laser ablation MC-ICP-MS: methodology and applications

    Energy Technology Data Exchange (ETDEWEB)

    Matteini, Massimo; Dantas, Elton L.; Pimentel, Marcio M.; Bühn, Bernhard, E-mail: massimo@unb.br [Universidade de Brasilia (UnB), DF (Brazil). Instituto de Geociencias

    2010-06-15

    The Lutetium-Hafnium isotopic system represents one of the most innovative and powerful tools for geochronology and isotopic studies. Combined U-Pb and Lu-Hf in situ analyses on zircon by LA-MC-ICP-MS permit to characterize isotopically the host magma from which it crystallized furnishing significant information for sediment provenance and crustal evolution studies. In this paper e describe the Lu-Hf systematic by LA-MC-ICP-MS developed in the laboratory of Geochronology of the University of Brasilia and report the results obtained by repeated analyses of {sup 176}Hf/{sup 177}Hf isotopic ratio of three zircon standards: GJ-1 = 0.282022 ± 11 (n=56), Temora 2 = 0.282693 ± 14 (n=25) and UQZ = 0.282127 ± 33 (n=11). The {sup 176}Hf/{sup 177}Hf ratio (0.282352 ± 22, n=14) of gem quality zircon used as in-house standard have been also characterized. As a geological application, we analyzed two complex zircons selected from a migmatitic rocks from the Borborema Province, NE Brazil. On the basis of U-Pb and Lu-Hf data, two main crystallization events have been identified in both studied zircons. An older event at ca. 2.05 Ga recognized in the inherited cores represents a well-characterized paleoproterozoic magmatic event that affected the whole Borborema Province. A second crystallization event at ∼ 575 Ma, recognized at the rims, represents a Neoproterozoic (Brazilian) high grade metamorphic-magmatic event. (author)

  6. Separation techniques for the clean-up of radioactive mixed waste for ICP-AES/ICP-MS analysis

    International Nuclear Information System (INIS)

    Swafford, A.M.; Keller, J.M.

    1993-01-01

    Two separation techniques were investigated for the clean-up of typical radioactive mixed waste samples requiring elemental analysis by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). These measurements frequently involve regulatory or compliance criteria which include the determination of elements on the EPA Target Analyte List (TAL). These samples usually consist of both an aqueous phase and a solid phase which is mostly an inorganic sludge. Frequently, samples taken from the waste tanks contain high levels of uranium and thorium which can cause spectral interferences in ICP-AES or ICP-MS analysis. The removal of these interferences is necessary to determine the presence of the EPA TAL elements in the sample. Two clean-up methods were studied on simulated aqueous waste samples containing the EPA TAL elements. The first method studied was a classical procedure based upon liquid-liquid extraction using tri-n- octylphosphine oxide (TOPO) dissolved in cyclohexane. The second method investigated was based on more recently developed techniques using extraction chromatography; specifically the use of a commercially available Eichrom TRU·Spec trademark column. Literature on these two methods indicates the efficient removal of uranium and thorium from properly prepared samples and provides considerable qualitative information on the extraction behavior of many other elements. However, there is a lack of quantitative data on the extraction behavior of elements on the EPA Target Analyte List. Experimental studies on these two methods consisted of determining whether any of the analytes were extracted by these methods and the recoveries obtained. Both methods produced similar results; the EPA target analytes were only slightly or not extracted. Advantages and disadvantages of each method were evaluated and found to be comparable

  7. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS

    International Nuclear Information System (INIS)

    Bentlin, Fabrina R.S.; Santos, Clarissa M.M. dos; Flores, Érico M.M.; Pozebon, Dirce

    2012-01-01

    Highlights: ► Ultrasound was investigated and applied for red wine samples preparation. ► Aliquots of 50 μL of sample were nebulized and transported to plasma. ► FI and pneumatic nebulization/aerosol desolvation were used. ► LODs of the ICP-MS method for lanthanides determination were at ng L −1 level. ► Lanthanides concentration allowed red wines classification. - Abstract: This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 μL of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L −1 , respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration.

  8. Development of methodologies used in the areas of safeguards and nuclear forensics based on LA-HR-ICP-MS technique

    International Nuclear Information System (INIS)

    Marin, Rafael Coelho

    2013-01-01

    Environmental sampling performed by means of swipe samples is a methodology frequently employed by International Atomic Energy Agency (IAEA) to verify if the signatory States of the Safeguards Agreements are conducing unauthorized activities. Swipe samples analysis is complementary to the Safeguards ordinary procedures used to verify the information given by the States. In this work it was described a methodology intending to strengthen the nuclear safeguards and nuclear forensics procedures. The proposal is to study and evaluate the laser ablation high resolution inductively coupled plasma mass spectrometry (LA-HR-ICP-MS) technique as an alternative to analyze the real-life swipe samples. The precision achieved through the standard (CRM - 125A) measurements, represented by the relative standard deviation (RSD), was respectively 1.3 %, 0.2 % e 7.6 % for the 234 U/ 238 U, 235 U/ 238 U e 236 U/ 238 U isotopes ratios. The percent uncertainties (u %), which covers the RSD, ranged from 3.5 % to 29.8 % to the 235 U/ 238 U measurements and from 16.6 % to 42.9 % to the 234 U/ 238 U isotope ratio. These results were compatible with former studies performed by the LA-HR-ICP-MS that analyzed real-life swipe samples collected at a nuclear facility. Swipe samples collected from several points of the nuclear facility presented enrichment level ranging from (2.3 ± 0.7) % (sample 3) to (17.3 ± 2.8) % (sample 18). They also allowed detecting different enrichment levels within the facility. (author)

  9. Quantitative characterization of TiO2 nanoparticle release from textiles by conventional and single particle ICP-MS

    Science.gov (United States)

    Mackevica, Aiga; Olsson, Mikael Emil; Hansen, Steffen Foss

    2018-01-01

    TiO2 is ubiquitously present in a wide range of everyday items, both as an intentionally incorporated additive and naturally occurring constituent. It can be found in a wide range of consumer products, including personal care products, food contact materials, and textiles. Normal use of these products may lead to consumer and/or environmental exposure to TiO2, possibly in form of nanoparticles. The aim of this study is to perform a leaching test and apply state-of-the-art methods to investigate nano-TiO2 and total Ti release from five types of commercially available conventional textiles: table placemats, wet wipes, microfiber cloths, and two types of baby bodysuits, with Ti contents ranging from 2.63 to 1448 μg/g. Released particle analysis was performed using conventional and single particle inductively coupled plasma mass spectrometry (ICP-MS and spICP-MS), in conjunction with transmission electron microscopy (TEM), to measure total and particulate TiO2 release by mass and particle number, as well as size distribution. Less than 1% of the initial Ti content was released over 24 h of leaching, with the highest releases reaching 3.13 μg/g. The fraction of nano-TiO2 released varied among fabric types and represented 0-80% of total TiO2 release. Particle mode sizes were 50-75 nm, and TEM imaging revealed particles in sizes of 80-200 nm. This study highlights the importance of using a multi-method approach to obtain quantitative release data that is able to provide an indication regarding particle number, size distribution, and mass concentration, all of which can help in understanding the fate and exposure of nanoparticles.

  10. Determination of trace elements in human liver biopsy samples by ICP-MS and TXRF: hepatic steatosis and nickel accumulation

    Energy Technology Data Exchange (ETDEWEB)

    Varga, Imre; Szoboszlai, Norbert [L. Eoetvoes University, Department of Inorganic and Analytical Chemistry, P.O. Box 32, Budapest (Hungary); Szebeni, Agnes [MI Central Hospital, Ultrasound Laboratory, Budapest (Hungary); Kovacs, Bela [Debrecen University - Centre of Agricultural Sciences, Department of Food Science and Quality Assurance, P.O. Box 36, Debrecen (Hungary)

    2005-10-01

    Human liver biopsy samples, collected from 52 individuals, were analysed by inductively coupled plasma-mass spectrometry (ICP-MS) and total reflection X-ray fluorescence (TXRF) spectrometry in a retrospective study (i.e. patient selection and liver biopsy were not for the purpose of element analysis). The freeze-dried samples (typically 0.5-2 mg dry weight) were digested in a laboratory microwave digestion system and solutions with a final volume of 1 mL were prepared. The concentrations of Cr, Mn, Fe, Ni, Cu, Zn, Rb, and Pb were determined by use of a Thermo Elemental X7 ICP-MS spectrometer. TXRF measurements were performed with an Atomika Extra IIA spectrometer. Yttrium was employed as an internal standard, prepared by dissolution of 5N-purity yttria (Y{sub 2}O{sub 3}) in our laboratory. The accuracy was tested by analysis of NIST 1577a Bovine Liver certified reference material. The concentrations of Fe, Cu, Zn, and Rb determined in human liver biopsy samples were in good agreement with data published by other authors. The distribution of nickel in the samples was surprisingly uneven - nickel concentrations ranged from 0.7 to 12 {mu}g g{sup -1} (dry weight) in 38 samples and in several samples were extremely high, 36-693 {mu}g g{sup -1}. Analysis of replicate procedural blanks and control measurements were performed to prevent misinterpretation of the data. For patients with steatosis (n=14) Ni concentrations were consistently high except for two who had levels close to those measured for the normal group. As far as we are aware no previous literature data are available on the association of steatosis with high concentration of nickel in human liver biopsies taken from living patients. (orig.)

  11. A comparison of sample preparation strategies for biological tissues and subsequent trace element analysis using LA-ICP-MS.

    Science.gov (United States)

    Bonta, Maximilian; Török, Szilvia; Hegedus, Balazs; Döme, Balazs; Limbeck, Andreas

    2017-03-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is one of the most commonly applied methods for lateral trace element distribution analysis in medical studies. Many improvements of the technique regarding quantification and achievable lateral resolution have been achieved in the last years. Nevertheless, sample preparation is also of major importance and the optimal sample preparation strategy still has not been defined. While conventional histology knows a number of sample pre-treatment strategies, little is known about the effect of these approaches on the lateral distributions of elements and/or their quantities in tissues. The technique of formalin fixation and paraffin embedding (FFPE) has emerged as the gold standard in tissue preparation. However, the potential use for elemental distribution studies is questionable due to a large number of sample preparation steps. In this work, LA-ICP-MS was used to examine the applicability of the FFPE sample preparation approach for elemental distribution studies. Qualitative elemental distributions as well as quantitative concentrations in cryo-cut tissues as well as FFPE samples were compared. Results showed that some metals (especially Na and K) are severely affected by the FFPE process, whereas others (e.g., Mn, Ni) are less influenced. Based on these results, a general recommendation can be given: FFPE samples are completely unsuitable for the analysis of alkaline metals. When analyzing transition metals, FFPE samples can give comparable results to snap-frozen tissues. Graphical abstract Sample preparation strategies for biological tissues are compared with regard to the elemental distributions and average trace element concentrations.

  12. Ultrasound assisted enzymatic hydrolysis for isolating titanium dioxide nanoparticles from bivalve mollusk before sp-ICP-MS.

    Science.gov (United States)

    Taboada-López, María Vanesa; Iglesias-López, Sara; Herbello-Hermelo, Paloma; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

    2018-08-14

    Applicability of single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) using dwell times equal to or shorter than 100 μs has been tested for assessing titanium dioxide nanoparticles (TiO 2 NPs) in bivalve mollusks. TiO 2 NPs isolation from fresh mollusk tissues was achieved by ultrasound assisted enzymatic hydrolysis procedure using a pancreatin/lipase mixture. Optimum extraction conditions imply ultrasonication (60% amplitude) for 10 min, and 7.5 mL of a solution containing 3.0 g L -1 of pancreatin and lipase (pH 7.4). The developed method was found to be repeatable (repeatability of 17% for the over-all procedure, TiO 2 NPs concentration of 5.33 × 10 7  ± 8.89 × 10 6 , n = 11), showing a limit of detection of 5.28 × 10 6 NPs g -1 , and a limit of detection in size of 24.4-30.4 nm, based on the 3σ criteria, and on the 3σ/5 σ criteria, respectively. The analytical recovery within the 90-99% range (use of TiO 2 NPs standards of 50 nm at 7 and 14 μg L -1 as Ti). Several bivalve mollusks (clams, cockles, mussels, razor clams, oysters and variegated scallops) were analyzed for total titanium (ICP-MS after microwave assisted acid digestion), and for TiO 2 NPs by the proposed method. TiO 2 NPs concentrations were within the 2.36 × 10 7 -1.25 × 10 8 NPs g -1 range, and the most frequent sizes were from 50 to 70 nm. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Spatial investigation of the elemental distribution in Wilson's disease liver after d-penicillamine treatment by LA-ICP-MS.

    Science.gov (United States)

    Hachmöller, Oliver; Zibert, Andree; Zischka, Hans; Sperling, Michael; Groba, Sara Reinartz; Grünewald, Inga; Wardelmann, Eva; Schmidt, Hartmut H-J; Karst, Uwe

    2017-12-01

    At present, the copper chelator d-penicillamine (DPA) is the first-line therapy of Wilson's disease (WD), which is characterized by an excessive copper overload. Lifelong DPA treatments aim to reduce the amount of detrimental excess copper retention in the liver and other organs. Although DPA shows beneficial effect in many patients, it may cause severe adverse effects. Despite several years of copper chelation therapy, discontinuation of DPA therapy can be linked to a rapidly progressing liver failure, indicating a high residual liver copper load. In order to investigate the spatial distribution of remaining copper and additional elements, such as zinc and iron, in rat and human liver samples after DPA treatment, a high resolution (spotsize of 10μm) laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) imaging method was applied. Untreated LPP -/- rats, an established animal model for WD, appeared with a high overall copper concentration and a copper distribution of hotspots distributed over the liver tissue. In contrast, a low (>2-fold decreased) overall copper concentration was detected in liver of DPA treated animals. Importantly, however, copper distribution was highly inhomogeneous with lowest concentrations in direct proximity to blood vessels, as observed using novel zonal analysis. A human liver needle biopsy of a DPA treated WD patient substantiated the finding of an inhomogeneous copper deposition upon chelation therapy. In contrast, comparatively homogenous distributions of zinc and iron were observed. Our study indicates that a high resolution LA-ICP-MS analysis of liver samples is excellently suited to follow efficacy of chelator therapy in WD patients. Copyright © 2017 Elsevier GmbH. All rights reserved.

  14. Limitation of secondary electron multiplier non-linearity on accurate U-Th isotopic determination by MC-ICP-MS

    Science.gov (United States)

    Shen, C.; Wu, C.; Gallet, S.; Cheng, H.; Edwards, R.; Hsieh, Y.; Lin, K.

    2008-12-01

    Contemporary multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS) with discrete dynode secondary electron multipliers (SEMs) can offer U-Th isotopic determinations with subpermil-permil- level precision in femtogram quantities. However, accurate isotopic measurement requires fully understanding SEM mass and intensity biases. In additional to dead-time effect, Richter et al (2001, Int. J. Mass Spectrom., 206, 105-127) reported a nonlinearity on SEMs produced by ETP and MasCom for count rates > 20 thousand counts per second (cps). We evaluated the possible biases for ion beams of 500- 1,600,000 cps on a latest MasCom SEM, SEV TE-Z/17, with more effective ion optical acceptance area (>50%) and better peak shape than previous models, used in a MC-ICP-MS, Thermo Fisher NEPTUNE. With the retarding potential quadruple lens (RPQ) turned off, ion beam intensity can be biased by only dead- time effect, which can be precisely corrected online or offline. With the RPQ on, two additional biases, an exponential-like increase of ion beam intensity from 100-100,000 s cps and an apparent dead-time effect (-2 to 2 ns) at high count rates, are observed. They are likely caused by the slightly defocused ions with a wide kinetic energy spread of ~5 eV, 10 times worse than that with thermal source, passing through the RPQ lens to the SEM, which is installed behind the focal plane. Fortunately, the two biases, which are stable during the daily measurements with the same settings of inlet system, source lenses, zoom optics, and RPQ, can be corrected effectively offline to earn accurate U-Th isotopic measurement.

  15. An environmentally-friendly, highly efficient, gas pressure-assisted sample introduction system for ICP-MS and its application to detection of cadmium and lead in human plasma.

    Science.gov (United States)

    Cao, Yupin; Deng, Biyang; Yan, Lizhen; Huang, Hongli

    2017-05-15

    An environmentally friendly and highly efficient gas pressure-assisted sample introduction system (GPASIS) was developed for inductively-coupled plasma mass spectrometry. A GPASIS consisting of a gas-pressure control device, a customized nebulizer, and a custom-made spray chamber was fabricated. The advantages of this GPASIS derive from its high nebulization efficiencies, small sample volume requirements, low memory effects, good precision, and zero waste emission. A GPASIS can continuously, and stably, nebulize 10% NaCl solution for more than an hour without clogging. Sensitivity, detection limits, precision, long-term stability, double charge and oxide ion levels, nebulization efficiencies, and matrix effects of the sample introduction system were evaluated. Experimental results indicated that the performance of this GPASIS, was equivalent to, or better than, those obtained by conventional sample introduction systems. This GPASIS was successfully used to determine Cd and Pb by ICP-MS in human plasma. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Sem-EDXRF and ICP-MS investigation of the morphological and chemical composition of depleted uranium particles from Kuwait areas affected by the 1991 Gulf War

    Energy Technology Data Exchange (ETDEWEB)

    Danesi, P.R.; Burns, K.; Campbell, M.; Ciurapinski, A.; Donohue, D.; Admon, U.; Burkart, W. [International Atomic Energy Agency Vienna (Austria)

    2004-07-01

    Selected soil samples collected in Kuwait locations where residues of DU ammunition existed as a legacy of the 1991 Gulf War, have been investigated by scanning electron microscopy equipped with an energy dispersive X-ray fluorescence detector (SEM- EDXRF) with the objective to identify the presence of DU particles and characterize their shape and size. The isotopic and total bulk concentrations of uranium in the samples were measured by inductively coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry. The samples studied by SEM-EDXRF were prepared by gently tapping an aluminum stab covered with a doubled-sided adhesive carbon disk, thereby ensuring that the physical integrity of the samples was maintained. The results have indicted that soil collected just below ({approx} 5 cm) corroded DU penetrators contained several DU oxide particles (isotopic ratio {sup 235}U/{sup 238}U = 0.0021) ranging in size from 1 to 10 microns (approximate geometrical diameter) having an irregular shape. The particles are most likely corrosion products from the DU penetrators. Some particles are imbedded in a larger matrix containing aluminum oxide (corrosion product of the penetrator jacket) and silica (sand). Swipes collected inside holes in tanks hit by DU ammunition, using ultra-pure cotton cloths, have indicated the presence of many small DU particles in the range 1 to 10 microns. In this case the particles were found to contain also small quantities of Fe, probably the results on alloying process occurring when the DU penetrators impact with the tank armor. (author)

  17. Development of ICP-MS and ICP-OES methods for determination of gadolinium in samples related to hospital waste water treatment

    Czech Academy of Sciences Publication Activity Database

    Bendakovská, L.; Krejčovská, A.; Černohorský, T.; Zelenková, Jana

    2016-01-01

    Roč. 70, č. 9 (2016), s. 1155-1165 ISSN 0366-6352 Institutional support: RVO:67985874 Keywords : gadolinium * rare-earth elements * bioaccumulation * gadolinium anomaly * inductively coupled plasma mass spectrometry (ICP-MS) * inductively coupled plasma optical emission spectrometry (ICP-OES) Subject RIV: BK - Fluid Dynamics Impact factor: 1.258, year: 2016

  18. Elemental mapping in fossil tooth root section of Ursus arctos by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)

    Czech Academy of Sciences Publication Activity Database

    Vašinová Galiová, M.; Nývltová Fišáková, Miriam; Kynický, J.; Prokeš, L.; Neff, H.; Mason, A. Z.; Gadas, P.; Košler, J.; Kanický, V.

    2013-01-01

    Roč. 105, 15 February 2013 (2013), s. 235-243 ISSN 0039-9140 Institutional research plan: CEZ:AV0Z80010507 Institutional support: RVO:68081758 Keywords : Diagenesis * Diet * Geochemical analysis * Laser ablation ICP-MS * Migration Subject RIV: AC - Archeology, Anthropology, Ethnology Impact factor: 3.511, year: 2013

  19. Simultaneous determination of metal traces using SPE preconcentration on Amberlite XAD-7 by ICP-MS in environmental water and sample ecotoxicology assessment

    Czech Academy of Sciences Publication Activity Database

    Holubova, Z.; Sommer, L.; Moos, Martin; Kuta, J.

    2012-01-01

    Roč. 21, 10A (2012), s. 3127-3135 ISSN 1018-4619 Institutional support: RVO:67179843 Keywords : Solid Phase Extraction * Amberlite XAD-7 * ICP-MS and Waters * Ecotoxicology Subject RIV: EH - Ecology, Behaviour Impact factor: 0.641, year: 2012

  20. New sequential separation procedure for Sr, Nd and Pb isotope ratio measurement in geological material using MC-ICP-MS and TIMS

    Digital Repository Service at National Institute of Oceanography (India)

    Makishima, A.; Nath, B.N.; Nakamura, E.

    A new 3-step sequential separation chemistry for Sr, Nd and Pb from silicate samples, which is suitable for isotope analysis by MC-ICP-MS as well as TIMS, has been developed. The chemistry is designed to minimize the number of evaporation steps...

  1. High-resolution line-scan analysis of resin-embedded sediments using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS)

    NARCIS (Netherlands)

    Hennekam, Rick; Jilbert, Tom; Mason, Paul R D; de Lange, Gert J.; Reichart, Gert Jan

    2015-01-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) line-scanning is a promising technique for producing high-resolution (μm-scale) geochemical records on resin-embedded sediments. However, this approach has not yet been thoroughly tested on sediment samples of known elemental

  2. Possibilities of LA-ICP-MS technique for the spatial elemental analysis of the recent fish scales: Line scan vs. depth profiling

    International Nuclear Information System (INIS)

    Hola, Marketa; Kalvoda, Jiri; Novakova, Hana; Skoda, Radek; Kanicky, Viktor

    2011-01-01

    LA-ICP-MS and solution based ICP-MS in combination with electron microprobe are presented as a method for the determination of the elemental spatial distribution in fish scales which represent an example of a heterogeneous layered bone structure. Two different LA-ICP-MS techniques were tested on recent common carp (Cyprinus carpio) scales: (a)A line scan through the whole fish scale perpendicular to the growth rings. The ablation crater of 55 μm width and 50 μm depth allowed analysis of the elemental distribution in the external layer. Suitable ablation conditions providing a deeper ablation crater gave average values from the external HAP layer and the collagen basal plate. (b)Depth profiling using spot analysis was tested in fish scales for the first time. Spot analysis allows information to be obtained about the depth profile of the elements at the selected position on the sample. The combination of all mentioned laser ablation techniques provides complete information about the elemental distribution in the fish scale samples. The results were compared with the solution based ICP-MS and EMP analyses. The fact that the results of depth profiling are in a good agreement both with EMP and PIXE results and, with the assumed ways of incorporation of the studied elements in the HAP structure, suggests a very good potential for this method.

  3. Application of laser ablation-ICP-MS to determine high-resolution elemental profiles across the Cretaceous/Paleogene boundary at Agost (Spain)

    NARCIS (Netherlands)

    Sosa-Montes de Oca, Claudia; de Lange, Gert J.|info:eu-repo/dai/nl/073930962; Martínez-Ruiz, Francisca; Rodríguez-Tovar, Francisco J.

    2018-01-01

    A high-resolution analysis of the distribution of major and trace elements across a Cretaceous/Paleogene boundary (KPgB) was done using Laser Ablation-Inductivity Coupled Plasma-Mass Spectrometry (LA-ICP-MS) and was compared with traditional distinct sampling and analysis. At the Agost site (SE

  4. The performance of single and multi-collector ICP-MS instruments for fast and reliable 34S/32S isotope ratio measurements†

    Science.gov (United States)

    Pröfrock, Daniel; Irrgeher, Johanna; Prohaska, Thomas

    2016-01-01

    The performance and validation characteristics of different single collector inductively coupled plasma mass spectrometers based on different technical principles (ICP-SFMS, ICP-QMS in reaction and collision modes, and ICP-MS/MS) were evaluated in comparison to the performance of MC ICP-MS for fast and reliable S isotope ratio measurements. The validation included the determination of LOD, BEC, measurement repeatability, within-lab reproducibility and deviation from certified values as well as a study on instrumental isotopic fractionation (IIF) and the calculation of the combined standard measurement uncertainty. Different approaches of correction for IIF applying external intra-elemental IIF correction (aka standard-sample bracketing) using certified S reference materials and internal inter-elemental IIF (aka internal standardization) correction using Si isotope ratios in MC ICP-MS are explained and compared. The resulting combined standard uncertainties of examined ICP-QMS systems were not better than 0.3–0.5% (uc,rel), which is in general insufficient to differentiate natural S isotope variations. Although the performance of the single collector ICP-SFMS is better (single measurement uc,rel = 0.08%), the measurement reproducibility (>0.2%) is the major limit of this system and leaves room for improvement. MC ICP-MS operated in the edge mass resolution mode, applying bracketing for correction of IIF, provided isotope ratio values with the highest quality (relative combined measurement uncertainty: 0.02%; deviation from the certified value: <0.002%). PMID:27812369

  5. Prestatiekenmerken van de bepaling van As, Cd, Pb en Hg in voeding en biologisch materiaal met ICP-MS en AFS

    NARCIS (Netherlands)

    Velde-Koerts T van der; Bom CM; LAC

    1999-01-01

    Een ICP-MS-methode werd ontwikkeld voor de bepaling van As, Cd en Pb in salpeterzuur-destruaten van voeding en biologisch materiaal. De methode werd geoptimaliseerd op basis van minimale spectrale storingen en matrixeffecten met behulp van correctieformules, interne standaarden en

  6. High-resolution line-scan analysis of resin-embedded sediments using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS)

    NARCIS (Netherlands)

    Hennekam, R.; Jilbert, T.; de Lange, G.J.; Reichart, G.J.

    2015-01-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) line-scanning is a promising technique for producing high-resolution (µm-scale) geochemical records on resin-embedded sediments. However, this approach has not yet been thoroughly tested on sediment samples of known elemental

  7. Quantification of low molecular weight selenium metabolites in human plasma after treatment with selenite in pharmacological doses by LC-ICP-MS

    DEFF Research Database (Denmark)

    Flouda, Konstantina; Dersch, Julie Maria; Gabel-Jensen, Charlotte

    2016-01-01

    The paper presents an analytical method for quantification of low molecular weight (LMW) selenium compounds in human plasma based on liquid chromatography inductively coupled plasma mass spectrometry (LC-ICP-MS) and post column isotope dilution-based quantification. Prior to analysis, samples were...

  8. Separation, purification and identification of the major selenium metabolite from human urine by multi-dimensional HPLC-ICP-MS and APCI-MS

    DEFF Research Database (Denmark)

    Gammelgaard, Bente; Madsen, K.G.; Bjerrum, J.

    2003-01-01

    volunteers were collected and analysed by ion-pair chromatography with ICP-MS detection for this major selenium metabolite. Samples containing the metabolite were pooled and solid phase extracted to remove ionic substances. The extracted pool was purified and preconcentrated twice by preparative reversed...

  9. Possibilities of LA-ICP-MS technique for the spatial elemental analysis of the recent fish scales: Line scan vs. depth profiling

    Energy Technology Data Exchange (ETDEWEB)

    Hola, Marketa [Department of Chemistry, Masaryk University of Brno, Kamenice 5, 625 00 Brno (Czech Republic); Kalvoda, Jiri, E-mail: jkalvoda@centrum.cz [Department of Geological Sciences, Masaryk University of Brno, Kotlarska 2, 611 37 Brno (Czech Republic); Novakova, Hana [Department of Chemistry, Masaryk University of Brno, Kamenice 5, 625 00 Brno (Czech Republic); Skoda, Radek [Department of Geological Sciences, Masaryk University of Brno, Kotlarska 2, 611 37 Brno (Czech Republic); Kanicky, Viktor [Department of Chemistry, Masaryk University of Brno, Kamenice 5, 625 00 Brno (Czech Republic)

    2011-01-01

    LA-ICP-MS and solution based ICP-MS in combination with electron microprobe are presented as a method for the determination of the elemental spatial distribution in fish scales which represent an example of a heterogeneous layered bone structure. Two different LA-ICP-MS techniques were tested on recent common carp (Cyprinus carpio) scales: (a)A line scan through the whole fish scale perpendicular to the growth rings. The ablation crater of 55 {mu}m width and 50 {mu}m depth allowed analysis of the elemental distribution in the external layer. Suitable ablation conditions providing a deeper ablation crater gave average values from the external HAP layer and the collagen basal plate. (b)Depth profiling using spot analysis was tested in fish scales for the first time. Spot analysis allows information to be obtained about the depth profile of the elements at the selected position on the sample. The combination of all mentioned laser ablation techniques provides complete information about the elemental distribution in the fish scale samples. The results were compared with the solution based ICP-MS and EMP analyses. The fact that the results of depth profiling are in a good agreement both with EMP and PIXE results and, with the assumed ways of incorporation of the studied elements in the HAP structure, suggests a very good potential for this method.

  10. Imaging of metal bioaccumulation in Hay-scented fern (Dennstaedtia punctilobula) rhizomes growing on contaminated soils by laser ablation ICP-MS

    International Nuclear Information System (INIS)

    Koelmel, Jeremy; Amarasiriwardena, Dulasiri

    2012-01-01

    Understanding Pb removal from the translocation stream is vital to engineering Pb hyperaccumulation in above ground organs, which would enhance the economic feasibility of Pb phytoextraction technologies. We investigated Cu, Pb, Sb and Zn distributions in Hay-scented fern (Dennstaedtia punctilobula) rhizomes on shooting range soils by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), analyzing digested rhizomes, stems, and fronds using ICP-MS. Nutrients Cu and Zn concentrated in fronds while toxic elements Pb and Sb did not, showing potential Pb and Sb sequestration in the rhizome. Frond and rhizome concentration of Pb was 0.17 ± 0.10% and 0.32 ± 0.21% of dry biomass, respectively. The 208 Pb/ 13 C and 121 Sb/ 13 C determined by LA-ICP-MS increased from inner sclerotic cortex to the epidermis, while Pb concentrated in the starchy cortex only in contaminated sites. These results suggest that concentration dependent bioaccumulation in the rhizome outer cortex removes Pb from the vascular transport stream. - Highlights: ► Bioimaged Cu, Pb, Sb, Zn across fern rhizomes from shooting ranges using LA-ICP-MS. ► Pb levels were highest in the outer starchy cortex. ► Pb seemed to displace nutrients Cu and Zn in contaminated site rhizomes. ► [Pb] and [Sb] were correlated across organs suggesting similar transport factors. - Using LA-ICP-MS we determined elemental distributions in Hay-scented fern rhizomes including concentration dependent Pb sequestration patterns in the outer cortex.

  11. Determination of trace element concentrations and stable lead, uranium and thorium isotope ratios by quadrupole-ICP-MS in NORM and NORM-polluted sample leachates

    Energy Technology Data Exchange (ETDEWEB)

    Mas, J.L., E-mail: ppmasb@us.es [Dpto. Fisica Aplicada I, EPS, Universidad de Sevilla, 41012 Sevilla (Spain); Villa, M. [Servicio de Radioisotopos, Centro de Investigacion, Tecnologia e Innovacion (CITIUS), Universidad de Sevilla, Avda. Reina Mercedes 4b, 41012 Sevilla (Spain); Dpto. Fisica Aplicada II, ETS de Arquitectura, Universidad de Sevilla, Avda. Reina Mercedes 2, 41012 Sevilla (Spain); Hurtado, S. [Servicio de Radioisotopos, Centro de Investigacion, Tecnologia e Innovacion (CITIUS), Universidad de Sevilla, Avda. Reina Mercedes 4b, 41012 Sevilla (Spain); Garcia-Tenorio, R. [Dpto. Fisica Aplicada II, ETS de Arquitectura, Universidad de Sevilla, Avda. Reina Mercedes 2, 41012 Sevilla (Spain)

    2012-02-29

    Highlights: Black-Right-Pointing-Pointer Polluted sediment and NORM samples. Black-Right-Pointing-Pointer An efficient yet fast process allowing multi-parametric determinations in <3 days. Black-Right-Pointing-Pointer Trace element concentrations, Pb, Th and U isotope ratios with a single instrument. - Abstract: This work focuses on the monitoring of the potential pollution in scenarios that involve NORM-related industrial activities (environmental or in-door scenarios). The objective was to develop a method to determine extent and origin of the contamination, suitable for monitoring (i.e. simple, fast and economical) and avoiding the use of too many different instruments. It is presented a radiochemical method that allows the determination of trace element concentrations and {sup 206}Pb/{sup 207}Pb/{sup 208}Pb, {sup 238}U/{sup 234}U and {sup 232}Th/{sup 230}Th isotope ratios using a single sample aliquot and a single instrument (ICP-QMS). Eichrom UTEVA{sup Registered-Sign} extraction chromatography minicolumns were used to separate uranium and thorium in sample leachates. Independent ICP-MS determinations of uranium and thorium isotope ratios were carried out afterwards. Previously a small aliquot of the leachate was used for the determination of trace element concentrations and lead isotope ratios. Several radiochemical arrangements were tested to get maximum performances and simplicity of the method. The performances of the method were studied in terms of chemical yields of uranium and thorium and removal of the potentially interfering elements. The established method was applied to samples from a chemical industry and sediments collected in a NORM-polluted scenario. The results obtained from our method allowed us to infer not only the extent, but also the sources of the contamination in the area.

  12. A point focusing double parabolic trough concentrator

    Energy Technology Data Exchange (ETDEWEB)

    Murphree, Quincy C. [Kentucky Mountain Bible College, Vancleve, KY (United States)

    2001-07-01

    This article shows that a point focusing solar concentrator can be made from two reflective parabolic troughs, a primary and a secondary, by orienting their longitudinal axes in perpendicular directions and separating them by the difference of their focal lengths along the optical axis. This offers a new alternative to the conventional 3-D paraboloidal concentrator permitting more flexibility in designs for applications requiring high concentrations. Both advantages and disadvantages are discussed. The intensity concentration ratio distribution is calculated in the focal plane and has elliptically shaped contours due to the inherent compensation of errant rays by the concave secondary. The ratio of the major to minor axes was 2.61 for the case considered, resulting in a concentration {approx}2.61 times that of a comparable concentrator without the compensation afforded by a concave secondary. Still, geometrical constraints limit the concentration to about 2000 suns for mirror quality errors of 5 mr. Optimisation of the compensation effect holds potential for improved performance for other concentrator designs. Finally, the functional dependence of the peak concentration and shading factor upon design parameters are presented. (Author)

  13. Improvement of accuracy for the quantitation of selenoproteins in post-column isotope dilution technique with HPLC ICP/MS

    International Nuclear Information System (INIS)

    Kim, Soo Jin; Pak, Yong Nam

    2016-01-01

    Post-column isotope dilution (PCID) or species-unspecific isotope dilution (ID) is a very useful quantitative technique in chromatography hyphenated with inductively coupled plasma–mass spectrometer (ICP/MS). In quantitative analysis, the calibration curve method is the most common one. However, it is not an absolute technique for the determination of concentration for the samples. ID method is the absolute one for the quantitative measurement technique, which means the quantity could be determined by the fundamental unit such as weight. To use the technique, it needs some requirements and there are several restrictions especially in the application for high-performance liquid chromatography (HPLC). The impurities in eluting solvent were in question. Thus, different purity of AA was examined and the result is shown in Figure 3. Figure 3(a) is the one for low (98%) and Figure 3(b) is high (99.999%) purity AA. The dotted area is for the eluting solvent. When low purity of 98% AA was introduced, the background was increasing while it remained the same for high-purity AA

  14. Sample introduction systems for the analysis of liquid microsamples by ICP-AES and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Todoli, Jose L. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, 03080 Alicante (Spain)]. E-mail: jose.todoli@ua.es; Mermet, Jean M. [Spectroscopy Forever, 01390 Tramoyes (France)

    2006-03-15

    There are many fields in which the available sample volume is the limiting factor for an elemental analysis. Over the last ten years, sample introduction systems used in plasma spectrometry (i.e., Inductively Coupled Plasma Atomic Emission Spectrometry, ICP-AES, and Mass Spectrometry, ICP-MS) have evolved in order to expand the field of applicability of these techniques to the analysis of micro- and nanosamples. A full understanding of the basic processes occurring throughout the sample introduction system is absolutely necessary to improve analytical performance. The first part of the present review deals with fundamental studies concerning the different phenomena taking place from aerosol production to analyte excitation/ionization when the liquid consumption rate does not exceed 100 {mu}l/min. Existing sample introduction systems are currently far from the ideal and a significant effort has been made to develop new and efficient devices. Different approaches for continuously introducing small sample volumes (i.e., microsamples) have been reviewed and compared in the present work. Finally, applications as well as basic guidelines to select the best sample introduction system according to the sample particularities are given at the end of this review.

  15. Analysis of gold(I/III)-complexes by HPLC-ICP-MS demonstrates gold(III) stability in surface waters.

    Science.gov (United States)

    Ta, Christine; Reith, Frank; Brugger, Joël; Pring, Allan; Lenehan, Claire E

    2014-05-20

    Understanding the form in which gold is transported in surface- and groundwaters underpins our understanding of gold dispersion and (bio)geochemical cycling. Yet, to date, there are no direct techniques capable of identifying the oxidation state and complexation of gold in natural waters. We present a reversed phase ion-pairing HPLC-ICP-MS method for the separation and determination of aqueous gold(III)-chloro-hydroxyl, gold(III)-bromo-hydroxyl, gold(I)-thiosulfate, and gold(I)-cyanide complexes. Detection limits for the gold species range from 0.05 to 0.30 μg L(-1). The [Au(CN)2](-) gold cyanide complex was detected in five of six waters from tailings and adjacent monitoring bores of working gold mines. Contrary to thermodynamic predictions, evidence was obtained for the existence of Au(III)-complexes in circumneutral, hypersaline waters of a natural lake overlying a gold deposit in Western Australia. This first direct evidence for the existence and stability of Au(III)-complexes in natural surface waters suggests that Au(III)-complexes may be important for the transport and biogeochemical cycling of gold in surface environments. Overall, these results show that near-μg L(-1) enrichments of Au in environmental waters result from metastable ligands (e.g., CN(-)) as well as kinetically controlled redox processes leading to the stability of highly soluble Au(III)-complexes.

  16. Speciation analysis of antimony in extracts of size-classified volcanic ash by HPLC-ICP-MS.

    Science.gov (United States)

    Miravet, R; López-Sánchez, J F; Rubio, R; Smichowski, P; Polla, G

    2007-03-01

    Although there is concern about the presence of toxic elements and their species in environmental matrices, for example water, sediment, and soil, speciation analysis of volcanic ash has received little attention. Antimony, in particular, an emerging element of environmental concern, has been less studied than other potentially toxic trace elements. In this context, a study was undertaken to assess the presence of inorganic Sb species in ash emitted from the Copahue volcano (Argentina). Antimony species were extracted from size-classified volcanic ash (<36 microm, 35-45 microm, 45-150 microm, and 150-300 microm) by use of 1 mol L(-1) citrate buffer at pH 5. Antimony(III) and (V) in the extracts were separated and quantified by high-performance liquid chromatography combined on-line with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). Antimony species concentrations (microg g(-1)) in the four fractions varied from 0.14 to 0.67 for Sb(III) and from 0.02 to 0.03 for Sb(V). The results reveal, for the first time, the occurrence of both inorganic Sb species in the extractable portion of volcanic ash. Sb(III) was always the predominant species.

  17. Elemental mapping and quantitative analysis of Cu, Zn, and Fe in rat brain sections by laser ablation ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Jackson, Brian [Dartmouth College, Departments of Earth Sciences and Chemistry, Hanover, NH (United States); Harper, Steve [University of Georgia, Savannah River Ecology Laboratory, Aiken, SC (United States); Smith, Laura; Flinn, Jane [George Mason University, Department of Psychology, Fairfax, VA (United States)

    2006-02-15

    This report details the application of laser ablation quadrupole ICP-MS for the (multi)elemental mapping of 100-{mu}m-thick sections of rat brain. The laser spot size used was 60 {mu}m, and the laser scan speed was 120 {mu}m s{sup -1}. The analysis was relatively rapid, allowing mapping of a whole brain thin section ({approx}1 cm{sup 2}) in about 2 h. Furthermore, the method was amenable to multi-element data collection including the physiologically important elements P and S and afforded sub {mu}g g{sup -1} detection limits for the important trace elements Cu and Zn. Calibrations were performed with pressed pellets of biological certified reference materials, and the elemental distributions and concentrations of Cu, Zn, and Fe were determined in whole rat brain sections. The distributions and concentration ranges for these elements were consistent with previous studies and demonstrate the utility of this technique for rapid mapping of brain thin sections. (orig.)

  18. Toxic metal levels in cocoa powder and chocolate by ICP-MS method after microwave-assisted digestion.

    Science.gov (United States)

    Lo Dico, Gianluigi Maria; Galvano, Fabio; Dugo, Giacomo; D'ascenzi, Carlo; Macaluso, Andrea; Vella, Antonio; Giangrosso, Giuseppe; Cammilleri, Gaetano; Ferrantelli, Vincenzo

    2018-04-15

    The Commission Regulation (EC) Regulation N. 488/2014, established the concentration limits for cadmium in specific products based on cocoa and chocolate products as from January 2019. Based on this information there is a need to determine ultratrace levels of elements that might be presents in cocoa and chocolate products. In this work, the concentrations of Arsenic, Antimony, Cadmium, Chromium, Lead, Selenium and Vanadium were evaluated in cocoa powder and chocolate by the validation of an ICP-MS method. Good selectivity/specificity, recovery, repeatability and within-laboratory reproducibility, LOD, LOQ, range of linearity, standard measurement uncertainty parameters for method validation were achieved, in accordance with Commission Regulation. The cocoa powder revealed the maximum metal concentrations of 0.303 ± 0.035 mg/kg for cadmium, 1.228 ± 0.146 mg/kg for lead and 0.094 ± 0.013 mg/kg for arsenic. A significant difference was found between cocoa powder and chocolate samples (p < .05). Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Monte Carlo simulation of expert judgments on human errors in chemical analysis--a case study of ICP-MS.

    Science.gov (United States)

    Kuselman, Ilya; Pennecchi, Francesca; Epstein, Malka; Fajgelj, Ales; Ellison, Stephen L R

    2014-12-01

    Monte Carlo simulation of expert judgments on human errors in a chemical analysis was used for determination of distributions of the error quantification scores (scores of likelihood and severity, and scores of effectiveness of a laboratory quality system in prevention of the errors). The simulation was based on modeling of an expert behavior: confident, reasonably doubting and irresolute expert judgments were taken into account by means of different probability mass functions (pmfs). As a case study, 36 scenarios of human errors which may occur in elemental analysis of geological samples by ICP-MS were examined. Characteristics of the score distributions for three pmfs of an expert behavior were compared. Variability of the scores, as standard deviation of the simulated score values from the distribution mean, was used for assessment of the score robustness. A range of the score values, calculated directly from elicited data and simulated by a Monte Carlo method for different pmfs, was also discussed from the robustness point of view. It was shown that robustness of the scores, obtained in the case study, can be assessed as satisfactory for the quality risk management and improvement of a laboratory quality system against human errors. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Sample introduction systems for the analysis of liquid microsamples by ICP-AES and ICP-MS

    International Nuclear Information System (INIS)

    Todoli, Jose L.; Mermet, Jean M.

    2006-01-01

    There are many fields in which the available sample volume is the limiting factor for an elemental analysis. Over the last ten years, sample introduction systems used in plasma spectrometry (i.e., Inductively Coupled Plasma Atomic Emission Spectrometry, ICP-AES, and Mass Spectrometry, ICP-MS) have evolved in order to expand the field of applicability of these techniques to the analysis of micro- and nanosamples. A full understanding of the basic processes occurring throughout the sample introduction system is absolutely necessary to improve analytical performance. The first part of the present review deals with fundamental studies concerning the different phenomena taking place from aerosol production to analyte excitation/ionization when the liquid consumption rate does not exceed 100 μl/min. Existing sample introduction systems are currently far from the ideal and a significant effort has been made to develop new and efficient devices. Different approaches for continuously introducing small sample volumes (i.e., microsamples) have been reviewed and compared in the present work. Finally, applications as well as basic guidelines to select the best sample introduction system according to the sample particularities are given at the end of this review

  1. Development and Validation of an ICP-MS Method for Simultaneous Determination of Selected Metals in Electronic Cigarette Aerosol

    Directory of Open Access Journals (Sweden)

    Ohashi Shintaro

    2018-04-01

    Full Text Available Safety and quality standards for electronic cigarettes (e-cigarettes have been introduced regionally. In 2016, the U.S. Food and Drug Administration (FDA issued a rule to regulate e-cigarettes, requiring to report harmful and potentially harmful constituents (HPHCs. In the United Kingdom, the British Standards Institution (BSI specified the metals to be monitored for e-cigarettes. In this study, a method was developed and validated for the simultaneous determination of 13 metals (Be, Al, Cr, Fe, Co, Ni, Cu, As, Se, Ag, Cd, Sn and Pb in e-cigarette aerosol. Furthermore, matrix effects of major constituents in the aerosol were investigated using glycerol or 1,2-propylene glycol solutions. E-cigarette aerosol was generated by a rotary smoking machine according to CORESTA Recommended Method N° 81 and collected by an electrostatic precipitator coupled to an impinger containing nitric acid. The collected aerosol was dissolved in nitric acid and an aliquot of this solution was analyzed by inductively coupled plasma mass spectrometry (ICP-MS equipped with a collision/reaction cell.

  2. Radiochemical separation of actinides from environmental samples for determination with DF-ICP-MS and alpha spectrometry

    International Nuclear Information System (INIS)

    Ayranov, M.; Kraehenbuehl, U.; Sahli, H.; Roellin, S.; Burger, M.

    2005-01-01

    The purpose of this study was to develop an optimised sample preparation method for the determination of Pu, Am, and Cm in environmental samples, soils, and sediments, and to compare the sensitivities of DF-ICP-MS, alpha spectrometry, and liquid scintillation alpha spectrometry. Borate fusion was used for sample material digestion. Two methods based on TOPO liquid-liquid extraction and combination of TEVA and TRU extraction chromatography showed highest yields of 92.7% for Pu, 86.8% for Am, and 87.6% for Cm. The detection limits were between 0.014-0.034 Bq/kg for 239 Pu, 0.014-0.093 Bq/kg for 240 Pu, and 0.011-1.20 Bq/kg for 241 Am. Analytical results for 238 Pu, 239 Pu, 240 Pu, 241 Pu and 241 Am and their isotope ratios in certified reference materials (IAEA-135 and IAEA-300) indicated very good accuracy of the methods proposed. (orig.)

  3. Effects of γ-sterilization on butyltin homogeneity and content in sediments: a GC-ICP-MS study

    International Nuclear Information System (INIS)

    Yang, Lu; Bancon-Montigny, Chrystelle; Mester, Zoltan; Sturgeon, Ralph E.; Willie, Scott N.; Boyko, Victor J.

    2003-01-01

    A GC-ICP-MS method based on extraction and alkylation of butyltins with sodium tetraethylborate was used to quantitatively assess the fate of these analytes in solutions and sediments following exposure to γ-irradiation. The effects of a 2.5 Mrad sterilization dose on three butyltin species in both methanolic calibration solutions and in sediment matrices were investigated. Although significant losses of tributyltin (TBT, 90%), dibutyltin (DBT, 100%) and monobutyltin (MBT, 80%) were detected in standard solutions prepared in methanol following γ-irradiation, no species inter-conversion occurred. Some degradation of TBT (38%) and DBT (32%) but no significant change in MBT content was found using a spiked sediment CRM HISS-1. Conversion DBT to MBT in spiked HISS-1 was deduced. Much smaller degradation of TBT (16% loss) and 10% loss of DBT by conversion to MBT (14% gain) was registered using a sediment blend of PACS-2 and HISS-1 (SOPH). Despite some initial losses of TBT and DBT due to irradiation, better than 2% RSD in both TBT and DBT concentrations measured in twelve different bottles of blended sediment SOPH were obtained, indicating the material may be considered homogeneous for these analytes. Results from a long-term five-year stability study of PACS-2 show that all three butyltins are stable during storage at 4 C followed with 2.5 Mrad minimum dose of γ-irradiation sterilization treatment. (orig.)

  4. [Study on distribution of five heavy metal elements in different parts of Cordyceps sinensis by microwave digestion ICP-MS].

    Science.gov (United States)

    Zhou, Li; Hao, Qing-Xiu; Wang, Sheng; Yang, Quan; Kang, Chuan-Zhi; Yang, Wan-Zhen; Guo, Lan-Ping

    2017-08-01

    The contents of five heavy metals (Cu, Pb, As, Cd, Hg) in 17 batches of Cordyceps sinensis were determined by microwave digestion-ICP-MS, and their distribution in C. sinensis were analyzed. The results showed that the contents of Cu, Pb, Cd and Hg in all batches were in accordance with the international standards of Chinese Medicine-Chinese Herbal Medicine Heavy Metal Limit, with their contents in the stroma higher than that in the caterpillar body, and the excess rate of As, which mainly concentrated in the caterpillar body part of C. sinensis, was 88.24%, as the content of As in the caterpillar body was 7 to 12 fold of that in the stroma. In this study, the distribution of five heavy metals in C. sinensis was clarified, and the existing problems of arsenic limit of heavy metal in C. sinensis were analyzed, and some suggestions were put forward. It is hoped that the reference standard can be provided for the limited standard of arsenic in C. sinensis. Copyright© by the Chinese Pharmaceutical Association.

  5. Direct quantification of thorium, uranium and rare earth element concentration in natural waters by ICP-MS

    International Nuclear Information System (INIS)

    Palmieri, Helena E.L.; Knupp, Eliana A.N.; Auler, Lucia M.L.A.; Gomes, Luiza M.F.; Windmoeller, Claudia C.

    2011-01-01

    A direct quantification of the thorium, uranium and rare earth elements in natural water samples using inductively coupled plasma mass spectrometry (ICP-MS) was evaluated with respect to selection of isotopes, detection limits, accuracy, precision, matrix effects for each isotope and spectral interferences. Accuracy of the method was evaluated by analysis of Spectra pure Standards (SPS-SW1 Batch 116-Norway) for the rare earth elements (REEs), thorium, uranium, scandium and yttrium. The measurements were carried out for each of the following analytical isotopes: 139 La, 140 Ce, 141 Pr, 143 Nd, 147 Sm, 151 Eu, 160 Gd, 159 Tb, 163 Dy, 165 Ho, 167 Er, 16 9Tm, 174 Yb, 175 Lu, 45 Sc, 89 Y, 232 Th and 238 U. Recovery percentage values found in these certified samples varied between 95 and 107%. The method was applied to the analysis of spring water samples collected in fountains spread throughout the historical towns of Ouro Preto, Mariana, Sabara and Diamantina in the state of Minas Gerais, Brazil. In the past these fountains played an essential and strategic role in supplying these towns with potable water. Until today this water is used by both the local population and tourists who believe in its quality. REE were quantified at levels comparable to those found in estuarine waters, which are characterized by low REE concentrations. In two fountains analyzed the concentration of REEs presented high levels and thus possible health risks for humans may not be excluded. (author)

  6. Flexible Automation System for Determination of Elemental Composition of Incrustations in Clogged Biliary Endoprostheses Using ICP-MS.

    Science.gov (United States)

    Fleischer, Heidi; Ramani, Kinjal; Blitti, Koffi; Roddelkopf, Thomas; Warkentin, Mareike; Behrend, Detlef; Thurow, Kerstin

    2018-02-01

    Automation systems are well established in industries and life science laboratories, especially in bioscreening and high-throughput applications. An increasing demand of automation solutions can be seen in the field of analytical measurement in chemical synthesis, quality control, and medical and pharmaceutical fields, as well as research and development. In this study, an automation solution was developed and optimized for the investigation of new biliary endoprostheses (stents), which should reduce clogging after implantation in the human body. The material inside the stents (incrustations) has to be controlled regularly and under identical conditions. The elemental composition is one criterion to be monitored in stent development. The manual procedure was transferred to an automated process including sample preparation, elemental analysis using inductively coupled plasma mass spectrometry (ICP-MS), and data evaluation. Due to safety issues, microwave-assisted acid digestion was executed outside of the automation system. The performance of the automated process was determined and validated. The measurement results and the processing times were compared for both the manual and the automated procedure. Finally, real samples of stent incrustations and pig bile were analyzed using the automation system.

  7. Comparison of Microwave Assisted Acid Digestion Methods for ICP-MS Determination of Total Arsenic in Fish Tissue

    International Nuclear Information System (INIS)

    Ghanthimathi, S.; Aminah Abdullah; Salmijah, S.; Ujang, T.; Nurul, I.A.

    2012-01-01

    Fish is one of the most important sources of arsenic exposure in human diet and the Food Safety and Quality Division, Ministry of Health since 2007 has required routine monitoring of total arsenic in sea foods such as fish. This study describes an improved extraction method of total arsenic in fish using microwave assisted acid digestion procedure before being analysed by inductively coupled plasma mass spectrometry (ICP-MS). The parameters studied were pre-treatment of sample, digestion temperature, time programme and the chemicals (HNO 3 / H 2 O 2 ) used. Arsenic contents in fish samples under these conditions were compared using the standards additions technique. Microwave assisted acid digestion method with a combination of ultrapure concentrated nitric acid (HNO 3 ) to concentrated hydrogen peroxide (H 2 O 2 ) at a ratio of 7 mL: 1 mL, run time of 25 min and digestion temperature of 200 degree Celsius with no pre-treatment was found to have recovery of 100.7 % as compared to other digestion procedure where the recovery were 115.5, 111.6 and 101.8 %. Validation using certified reference material (CRM) of fish tissue (DORM-3) showed a recovery of 101.4 ± 2.5 % for total arsenic from the CRM. (author)

  8. Arsenic, Antimony, Chromium, and Thallium Speciation in Water and Sediment Samples with the LC-ICP-MS Technique

    Directory of Open Access Journals (Sweden)

    Magdalena Jabłońska-Czapla

    2015-01-01

    Full Text Available Chemical speciation is a very important subject in the environmental protection, toxicology, and chemical analytics due to the fact that toxicity, availability, and reactivity of trace elements depend on the chemical forms in which these elements occur. Research on low analyte levels, particularly in complex matrix samples, requires more and more advanced and sophisticated analytical methods and techniques. The latest trends in this field concern the so-called hyphenated techniques. Arsenic, antimony, chromium, and (underestimated thallium attract the closest attention of toxicologists and analysts. The properties of those elements depend on the oxidation state in which they occur. The aim of the following paper is to answer the question why the speciation analytics is so important. The paper also provides numerous examples of the hyphenated technique usage (e.g., the LC-ICP-MS application in the speciation analysis of chromium, antimony, arsenic, or thallium in water and bottom sediment samples. An important issue addressed is the preparation of environmental samples for speciation analysis.

  9. Thallium (III) determination in the Baltic seawater samples by ICP MS after preconcentration on SGX C18 modified with DDTC.

    Science.gov (United States)

    Krasnodębska-Ostręga, Beata; Sadowska, Monika; Piotrowska, Katarzyna; Wojda, Marta

    2013-08-15

    The main difficulty of speciation analysis of thallium lies in extremely low concentrations of Tl(III) in comparison to Tl(I), which is the dominating form of thallium in environmental samples. In this study, a sensitive method is presented for separation of trace amounts of Tl(III) from Tl(I) and preconcentration of Tl(III) using octadecyl silica gel modified with diethyldithiocarbamate (DDTC). Under optimal conditions, only Tl(III) is retained on the sorbent, and then eluted with 96% ethanol. After chemical decomposition of Tl(III)-DDTC complex, thallium is determined by inductively coupled plasma mass spectrometry. High performance liquid chromatography with ICP MS detection was used to control the correctness of the obtained results. Parameters affecting solid phase extraction (SPE) such as pH, type, concentration and volume of eluent, breakthrough volume, and the impact of sample salinity (chlorides) and other interfering ions (Cd(II), Zn(II), Pb(II), Cu(II), Sn(II)) were investigated. The limit of detection (LOD), evaluated for 2 mL of sample solution, was 0.10 ng for Tl(I) and 0.43 ng for Tl(III). The method was applied to the determination of Tl(I) and Tl(III) in the Baltic seawater samples enriched in both thallium species. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. Improvement of accuracy for the quantitation of selenoproteins in post-column isotope dilution technique with HPLC ICP/MS

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Soo Jin; Pak, Yong Nam [Dept. of Chemistry Education, Korea National University of Education, Cheongju (Korea, Republic of)

    2016-11-15

    Post-column isotope dilution (PCID) or species-unspecific isotope dilution (ID) is a very useful quantitative technique in chromatography hyphenated with inductively coupled plasma–mass spectrometer (ICP/MS). In quantitative analysis, the calibration curve method is the most common one. However, it is not an absolute technique for the determination of concentration for the samples. ID method is the absolute one for the quantitative measurement technique, which means the quantity could be determined by the fundamental unit such as weight. To use the technique, it needs some requirements and there are several restrictions especially in the application for high-performance liquid chromatography (HPLC). The impurities in eluting solvent were in question. Thus, different purity of AA was examined and the result is shown in Figure 3. Figure 3(a) is the one for low (98%) and Figure 3(b) is high (99.999%) purity AA. The dotted area is for the eluting solvent. When low purity of 98% AA was introduced, the background was increasing while it remained the same for high-purity AA.

  11. Lanthanides determination in red wine using ultrasound assisted extraction, flow injection, aerosol desolvation and ICP-MS.

    Science.gov (United States)

    Bentlin, Fabrina R S; dos Santos, Clarissa M M; Flores, Erico M M; Pozebon, Dirce

    2012-01-13

    This paper deals with the determination of the fourteen naturally occurring elements of the lanthanide series in red wine. Ultrasound (US) was used for sample preparation prior lanthanides determination using ICP-MS. Flow injection (FI) and pneumatic nebulization/aerosol desolvation were used for nebulization of aliquots of 50 μL of sample and its subsequent transportation to plasma. Sample preparation procedures, matrix interference and time of sonication were evaluated. Better results for lanthanides in red wine were obtained by sonication with US probe for 90 s and sample 10-fold diluted. The limits of detection of La, Ce, Nd, Sm, Gd, Pr, Eu, Tb, Dy, Ho, Er, Tm, Lu and Yb were 6.57, 10.8, 9.97, 9.38, 2.71, 1.29, 1.22, 0.52, 2.35, 0.96, 2.30, 0.45, 0.24 and 1.35 ng L(-1), respectively. Red wines of different varieties from three countries of South America were discriminated according to the country of origin by means of multivariate analysis of lanthanides concentration. Copyright © 2011 Elsevier B.V. All rights reserved.

  12. An overview of the LAM-MC-ICP MS national facility: prospects and priorities. PD-3-1

    International Nuclear Information System (INIS)

    Bhaskar Rao, Y.J.; Vijaya Gopal, B.; Babu, E.V.S.S.K.; Sukumaran, N.P.; Sreenivas, B.; Vijaya Kumar, T.; Krishna, K.V.S.S.; Tomson, J.K.

    2007-01-01

    Unraveling the complex history of earth and other planetary bodies is a fundamental challenge to all earth scientists. Trace element distributions and isotopic variations in terrestrial rocks and minerals, materials from the Moon, and other inaccessible parts of the Universe as represented in meteorites hold the key to understanding many planetary and earth processes. At the same time, high precision isotopic data on samples of the Earth's hydrosphere and biosphere are important to understanding Man's habitat and environment. The fact that these natural processes operate on a range of scales in space and time necessitates isotopic composition measurements of many responsive and geochemically distinct trace elements including several naturally radioactive parent and radiogenic daughter isotope systems with half-lives between 10 3 -10 15 years and isotopes of many non-radiogenic (stable) elements as well. This article forms a brief introduction to the instrumentation, capabilities and some current priority projects of the Laser Ablation Microprobe (LAM)-Multicollector Inductively Coupled Plasma Mass Spectrometer (MC-ICP MS) National Facility

  13. Fast and Simple Analytical Method for Direct Determination of Total Chlorine Content in Polyglycerol by ICP-MS.

    Science.gov (United States)

    Jakóbik-Kolon, Agata; Milewski, Andrzej; Dydo, Piotr; Witczak, Magdalena; Bok-Badura, Joanna

    2018-02-23

    The fast and simple method for total chlorine determination in polyglycerols using low resolution inductively coupled plasma mass spectrometry (ICP-MS) without the need for additional equipment and time-consuming sample decomposition was evaluated. Linear calibration curve for 35 Cl isotope in the concentration range 20-800 µg/L was observed. Limits of detection and quantification equaled to 15 µg/L and 44 µg/L, respectively. This corresponds to possibility of detection 3 µg/g and determination 9 µg/g of chlorine in polyglycerol using studied conditions (0.5% matrix-polyglycerol samples diluted or dissolved with water to an overall concentration of 0.5%). Matrix effects as well as the effect of chlorine origin have been evaluated. The presence of 0.5% (m/m) of matrix species similar to polyglycerol (polyethylene glycol-PEG) did not influence the chlorine determination for PEGs with average molecular weights (MW) up to 2000 Da. Good precision and accuracy of the chlorine content determination was achieved regardless on its origin (inorganic/organic). High analyte recovery level and low relative standard deviation values were observed for real polyglycerol samples spiked with chloride. Additionally, the Combustion Ion Chromatography System was used as a reference method. The results confirmed high accuracy and precision of the tested method.

  14. Determination of rare earth elements in seawater by ICP-MS after preconcentration with a chelating resin-packed minicolumn

    International Nuclear Information System (INIS)

    Zhu Yanbei; Itoh, Akihide; Fujimori, Eiji; Umemura, Tomonari; Haraguchi, Hiroki

    2006-01-01

    Rare earth elements (REEs) in seawater were preconcentrated 20-fold (from 50 to 2.5 ml) by a chelating resin-packed minicolumn device and determined by inductively coupled plasma mass spectrometry (ICP-MS). The recoveries for REEs were in the range from 90% for Eu and Dy to 98% for Yb, and their standard deviations were less than 4%. The lower detection limits for REEs ranged from 0.06 ng l -1 for Lu to 0.5 ng l -1 for Sm. The analytical results for REEs in seawater reference materials (NASS-5, CASS-3, and CASS-4), the Take Island coastal seawater, and the Ise Bay coastal seawater were evaluated as the REE distribution patterns with shale-normalization and deep seawater-normalization. Slight relative enrichments of heavy REEs were observed in the Take Island coastal seawater and the Ise Bay coastal seawater, which might be attributed to the input from the river flows containing more dissolved heavy REEs. In addition, positive anomalies of Sm were found in the normalized REE distribution patterns for NASS-5, CASS-3, and CASS-4, which would be attributed to the contamination in the preparation process of reference materials by NRC

  15. Diffusivities of Redox-Sensitive Elements in Basalt vs. Oxygen Fugacity Determined by LA-ICP-MS

    Science.gov (United States)

    Szumila, Ian; Danielson, Lisa; Trail, Dustin

    2017-01-01

    Several diffusion experiments were conducted in a piston cylinder device across a range of oxygen fugacities (FMQ-3 FMQ-1.2, FMQ+6) at 1 GPa and 1300 C. This was done to explore the effects of oxygen fugacity (fO2) on diffusivity of redox sensitive trace elements. This allows investigation of how these elements diffuse across the fO2 range encountered in different reservoirs on planets and moons in our solar system. The University of Rochester LA-ICP-MS system was used for analysis of samples. Analyses were conducted using an Agilent 7900 quadrupole mass spectrometer connected to a Photon Machines 193 nm G2 laser ablation (LA) system equipped with a HelEx 2-volume sample chamber. Spots used were 35 micrometers circles spaced at 65 micrometers intervals. Laser fluence was 7.81 J/cm^2 with a rep rate of 10 Hz. The iolite software package was used to reduce data collected from laser ablation analysis of experiments with Si-29 used as the internal standard isotope. Iolite's global fit module was used to simultaneously fit elements' diffusivities in each experiment while keeping the Matano interface constant. Elements analysed include V, Nb, W, Mo, La, Ce, Pr, Sm, Eu, Gd, Ta, and W. Figures

  16. Biomonitoring of 29 trace elements in whole blood from inhabitants of Cotonou (Benin) by ICP-MS.

    Science.gov (United States)

    Yedomon, Brice; Menudier, Alain; Etangs, Florence Lecavelier Des; Anani, Ludovic; Fayomi, Benjamin; Druet-Cabanac, Michel; Moesch, Christian

    2017-09-01

    This study aimed to investigate the blood concentration of 29 trace elements, metals or metalloids, in a healthy population of Cotonou not directly exposed to metals in order to propose reference values. Blood samples from 70 blood donors were collected in K2 EDTA tubes for trace elements during September 2015 and a questionnaire was used to assess lifestyle exposure. Blood metal concentrations were determined by inductively coupled plasma mass spectrometry (ICP-MS) equipped with a quadrupole-based reaction cell. Among the selected blood donors 51.4% were aged from 18 to 36 years and 49.6% from 37 to 65 years. Among the 29 elements analyzed As, Pb, Mn, Pd, Sb, Co, Se, Sr showed blood concentrations higher than the reference values found in the literature for non-exposed healthy European populations and their geometric means were respectively 5.81; 47.39; 19.71; 1.91; 7.50; 0.66; 163.01; 30.53μg/L. This study provides the first reference value (5th-95th percentiles) for each element in Cotonou, which enables us to carry out further investigations on environmental and occupational exposure. Copyright © 2016 Elsevier GmbH. All rights reserved.

  17. Simultaneous quantification of tumor uptake for targeted and non-targeted liposomes and their encapsulated contents by ICP-MS

    Science.gov (United States)

    Cheng, Zhiliang; Zaki, Ajlan Al; Hui, James Z; Tsourkas, Andrew

    2012-01-01

    Liposomes are intensively being developed for biomedical applications including drug and gene delivery. However, targeted liposomal delivery in cancer treatment is a very complicated multi-step process. Unfavorable liposome biodistribution upon intravenous administration and membrane destabilization in blood circulation could result in only a very small fraction of cargo reaching the tumors. It would therefore be desirable to develop new quantitative strategies to track liposomal delivery systems to improve the therapeutic index and decrease systemic toxicity. Here, we developed a simple and non-radiative method to quantify the tumor uptake of targeted and non-targeted control liposomes as well as their encapsulated contents simultaneously. Specifically, four different chelated lanthanide metals were encapsulated or surface-conjugated onto tumor-targeted and non-targeted liposomes, respectively. The two liposome formulations were then injected into tumor-bearing mice simultaneously and their tumor delivery was determined quantitatively via inductively coupled plasma-mass spectroscopy (ICP-MS), allowing for direct comparisons. Tumor uptake of the liposomes themselves and their encapsulated contents were consistent with targeted and non-targeted liposome formulations that were injected individually. PMID:22882145

  18. Gold Nanoparticle Labeling Based ICP-MS Detection/Measurement of Bacteria, and Their Quantitative Photothermal Destruction

    Science.gov (United States)

    Lin, Yunfeng

    2015-01-01

    Bacteria such as Salmonella and E. coli present a great challenge in public health care in today’s society. Protection of public safety against bacterial contamination and rapid diagnosis of infection require simple and fast assays for the detection and elimination of bacterial pathogens. After utilizing Salmonella DT104 as an example bacterial strain for our investigation, we report a rapid and sensitive assay for the qualitative and quantitative detection of bacteria by using antibody affinity binding, popcorn shaped gold nanoparticle (GNPOPs) labeling, surfance enchanced Raman spectroscopy (SERS), and inductively coupled plasma mass spectrometry (ICP-MS) detection. For qualitative analysis, our assay can detect Salmonella within 10 min by Raman spectroscopy; for quantitative analysis, our assay has the ability to measure as few as 100 Salmonella DT104 in a 1 mL sample (100 CFU/mL) within 40 min. Based on the quantitative detection, we investigated the quantitative destruction of Salmonella DT104, and the assay’s photothermal efficiency in order to reduce the amount of GNPOPs in the assay to ultimately to eliminate any potential side effects/toxicity to the surrounding cells in vivo. Results suggest that our assay may serve as a promising candidate for qualitative and quantitative detection and elimination of a variety of bacterial pathogens. PMID:26417447

  19. sup 9 sup 9 Tc atom counting by quadrupole ICP-MS. Optimisation of the instrumental response

    CERN Document Server

    Mas, J L; Garcia-Leon, M

    2002-01-01

    In this paper, an extensive work is done on the specific tune of a conventional ICP-MS for sup 9 sup 9 Tc atom counting. For this, two methods have been used and compared: the partial variable control method and the 5D Simplex method. Instrumental limits of detection of 0.2 and 0.8 ppt, respectively, were obtained. They are noticeably lower than that found with the automatic tune method of the spectrometer, 47 ppt, which shows the need of a specific tune when very low levels of sup 9 sup 9 Tc have to be determined. A study is presented on the mass interferences for sup 9 sup 9 Tc. Our experiments show that the formation of polyatomic atoms or refractory oxides as well as sup 9 sup 8 Mo hydrides seem to be irrelevant for sup 9 sup 9 Tc atom counting. The opposite occurs with the presence of isobaric interferences, i.e. sup 9 sup 9 Ru, and the effect of abundance sensitivity, or low-mass resolution, which can modify the response at m/z=99 to a non-negligible extent.

  20. DETERMINATION of the TRACE ELEMENT LEVELS in HAIR of SMOKERS and NON-SMOKERS by ICP-MS

    Directory of Open Access Journals (Sweden)

    Elif Varhan Oral

    2016-09-01

    Full Text Available For at least 50 years, determination of the trace element levels in human hair has been used to assess environmental and vocational exposure to toxic elements . As compared to other biological matrices (e.g. blood, urine, human hair is stable and therefore useful as a matrice. In this study, analyses of toxic and essential trace elements, such as Cd, Pb, Cu and Fe, were done in hair samples which we collected from male smokers (10 people and non-smokers (10 people who live in Diyarbakır, Turkey and concentrations in hair samples were compared. Hair samples were washed by a standard procedure proposed by the International Atomic Energy Agency. Then the samples were dried for 16 h at 110°C in an oven. Solubilization procedure was carried out by nitric acid hydrogen peroxide mixture (3:1 in closed vessels in a microwave oven. Trace element analyses were carried out by using inductively coupled plasma-mass spectrometry (ICP-MS  technique. In our study, while concentrations of Cd, Pb, and Fe elements were found to be considerably higher in smokers than non-smokers, similar results were observed in Cu concentrations. The precision and accuracy of the method was evaluated by applying spike method to samples. Analytical recovery results were found between 91.2% and 104.6%.

  1. Using Cluster Analysis and ICP-MS to Identify Groups of Ecstasy Tablets in Sao Paulo State, Brazil.

    Science.gov (United States)

    Maione, Camila; de Oliveira Souza, Vanessa Cristina; Togni, Loraine Rezende; da Costa, José Luiz; Campiglia, Andres Dobal; Barbosa, Fernando; Barbosa, Rommel Melgaço

    2017-11-01

    The variations found in the elemental composition in ecstasy samples result in spectral profiles with useful information for data analysis, and cluster analysis of these profiles can help uncover different categories of the drug. We provide a cluster analysis of ecstasy tablets based on their elemental composition. Twenty-five elements were determined by ICP-MS in tablets apprehended by Sao Paulo's State Police, Brazil. We employ the K-means clustering algorithm along with C4.5 decision tree to help us interpret the clustering results. We found a better number of two clusters within the data, which can refer to the approximated number of sources of the drug which supply the cities of seizures. The C4.5 model was capable of differentiating the ecstasy samples from the two clusters with high prediction accuracy using the leave-one-out cross-validation. The model used only Nd, Ni, and Pb concentration values in the classification of the samples. © 2017 American Academy of Forensic Sciences.

  2. ICP-MS measurements of iodine and bromine in environmental samples collected along the Kuji River, Japan

    International Nuclear Information System (INIS)

    Kushita, Kouhei N.; Amano, Hikaru

    2003-01-01

    From a viewpoint of monitoring the distribution and transfer of long-lived radioiodine ( 129 I) and possible hazardous brominated substances, I and Br contents in various environmental samples collected in the Kuji River area, Japan, were studied by ICP-MS. The feature of the change in concentrations of I and Br, as well as those of other general properties such as pH etc., in Kuji River watershed were coincident with each other. It is considered from the obtained data that the environmental conditions, especially those of the soil of the area, mainly control the distribution of I and Br in the river water. The circulation characteristics of I and Br showed different features in different transfer media, which could be ascribed to the different chemical properties of these elements in each media. It was also shown that the distributions of I and Br are varied even within a small zone of about 20 km width around a high mountain of this area, which is also considered to reflect the environmental characteristics of the district. (author)

  3. Quantification of dermal exposure to nanoparticles from solid nanocomposites by using single particle ICP-MS

    DEFF Research Database (Denmark)

    Mackevica, Aiga; Olsson, Mikael Emil; Hansen, Steffen Foss

    2016-01-01

    , optical or photocatalytical properties. There is a lot of research focusing on effects exerted by nanoparticles, but the knowledge concerning release and subsequential exposure to nanoparticles is very limited, and information regarding potential dermal exposure from nanomaterial containing solid articles...... and characterization. In this study, we have investigated the potential dermal exposure to three different types of nano-enabled consumer products: Ag-containing keyboard covers, TiO2 coated ceramic tiles, and wood painted with CuO containing paint. The potential for dermal transfer from the aforementioned surfaces...

  4. Application of isotope-dilution laser ablation ICP-MS for direct determination of Pu concentrations in soils at pg g{sup -1} levels

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, Sergei F.; Tibi, Markus; Heumann, Klaus G. [Institute of Inorganic Chemistry and Analytical Chemistry, Johannes Gutenberg-University Mainz, Duesbergweg 10-14, 55099, Mainz (Germany)

    2004-01-01

    The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3 x 10{sup -13} g g{sup -1} for Pu isotopes in soil samples containing uranium at a concentration of a few {mu}g g{sup -1}. The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH{sup +} and PbO{sub 2}{sup +} ions and by the peak tail of {sup 238}U{sup +} ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of {alpha}-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of {sup 239+240}Pu (9.8{+-}3.0 mBq g{sup -1}) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4{+-}0.2 mBq g{sup -1}. However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if ''hot'' particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples. (orig.)

  5. Using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to characterize copper, zinc and mercury along grizzly bear hair providing estimate of diet

    Energy Technology Data Exchange (ETDEWEB)

    Noël, Marie, E-mail: marie.noel@stantec.com [Stantec Consulting Ltd. 2042 Mills Road, Unit 11, Sidney BC V8L 4X2 (Canada); Christensen, Jennie R., E-mail: jennie.christensen@stantec.com [Stantec Consulting Ltd. 2042 Mills Road, Unit 11, Sidney BC V8L 4X2 (Canada); Spence, Jody, E-mail: jodys@uvic.ca [School of Earth and Ocean Sciences, Bob Wright Centre A405, University of Victoria, PO BOX 3065 STN CSC, Victoria, BC V8W 3V6 (Canada); Robbins, Charles T., E-mail: ctrobbins@wsu.edu [School of the Environment and School of Biological Sciences, Washington State University, Pullman, WA 99164-4236 (United States)

    2015-10-01

    We enhanced an existing technique, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), to function as a non-lethal tool in the temporal characterization of trace element exposure in wild mammals. Mercury (Hg), copper (Cu), cadmium (Cd), lead (Pb), iron (Fe) and zinc (Zn) were analyzed along the hair of captive and wild grizzly bears (Ursus arctos horribilis). Laser parameters were optimized (consecutive 2000 μm line scans along the middle line of the hair at a speed of 50 μm/s; spot size = 30 μm) for consistent ablation of the hair. A pressed pellet of reference material DOLT-2 and sulfur were used as external and internal standards, respectively. Our newly adapted method passed the quality control tests with strong correlations between trace element concentrations obtained using LA-ICP-MS and those obtained with regular solution-ICP-MS (r{sup 2} = 0.92, 0.98, 0.63, 0.57, 0.99 and 0.90 for Hg, Fe, Cu, Zn, Cd and Pb, respectively). Cross-correlation analyses revealed good reproducibility between trace element patterns obtained from hair collected from the same bear. One exception was Cd for which external contamination was observed resulting in poor reproducibility. In order to validate the method, we used LA-ICP-MS on the hair of five captive grizzly bears fed known and varying amounts of cutthroat trout over a period of 33 days. Trace element patterns along the hair revealed strong Hg, Cu and Zn signals coinciding with fish consumption. Accordingly, significant correlations between Hg, Cu, and Zn in the hair and Hg, Cu, and Zn intake were evident and we were able to develop accumulation models for each of these elements. While the use of LA-ICP-MS for the monitoring of trace elements in wildlife is in its infancy, this study highlights the robustness and applicability of this newly adapted method. - Highlights: • LA-ICP-MS provides temporal trace metal exposure information for wild grizzly bears. • Cu and Zn temporal exposures provide

  6. Using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to characterize copper, zinc and mercury along grizzly bear hair providing estimate of diet

    International Nuclear Information System (INIS)

    Noël, Marie; Christensen, Jennie R.; Spence, Jody; Robbins, Charles T.

    2015-01-01

    We enhanced an existing technique, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), to function as a non-lethal tool in the temporal characterization of trace element exposure in wild mammals. Mercury (Hg), copper (Cu), cadmium (Cd), lead (Pb), iron (Fe) and zinc (Zn) were analyzed along the hair of captive and wild grizzly bears (Ursus arctos horribilis). Laser parameters were optimized (consecutive 2000 μm line scans along the middle line of the hair at a speed of 50 μm/s; spot size = 30 μm) for consistent ablation of the hair. A pressed pellet of reference material DOLT-2 and sulfur were used as external and internal standards, respectively. Our newly adapted method passed the quality control tests with strong correlations between trace element concentrations obtained using LA-ICP-MS and those obtained with regular solution-ICP-MS (r 2 = 0.92, 0.98, 0.63, 0.57, 0.99 and 0.90 for Hg, Fe, Cu, Zn, Cd and Pb, respectively). Cross-correlation analyses revealed good reproducibility between trace element patterns obtained from hair collected from the same bear. One exception was Cd for which external contamination was observed resulting in poor reproducibility. In order to validate the method, we used LA-ICP-MS on the hair of five captive grizzly bears fed known and varying amounts of cutthroat trout over a period of 33 days. Trace element patterns along the hair revealed strong Hg, Cu and Zn signals coinciding with fish consumption. Accordingly, significant correlations between Hg, Cu, and Zn in the hair and Hg, Cu, and Zn intake were evident and we were able to develop accumulation models for each of these elements. While the use of LA-ICP-MS for the monitoring of trace elements in wildlife is in its infancy, this study highlights the robustness and applicability of this newly adapted method. - Highlights: • LA-ICP-MS provides temporal trace metal exposure information for wild grizzly bears. • Cu and Zn temporal exposures provide

  7. Identification of Marchfeld asparagus using Sr isotope ratio measurements by MC-ICP-MS.

    Science.gov (United States)

    Swoboda, S; Brunner, M; Boulyga, S F; Galler, P; Horacek, M; Prohaska, T

    2008-01-01

    This work focuses on testing and application of Sr isotope signatures for the fast and reliable authentication and traceability of Asparagus officinalis originating from Marchfeld, Austria, using multicollector inductively coupled plasma mass spectrometry after optimised Rb/Sr separation. The major sample pool comprises freeze-dried and microwave-digested asparagus samples from Hungary and Slovakia which are compared with Austrian asparagus originating from the Marchfeld region, which is a protected geographical indication. Additional samples from Peru, The Netherlands and Germany were limited in number and allowed therefore only restricted statistical evaluation. Asparagus samples from Marchfeld were harvested within two subsequent years in order to investigate the annual variation. The results show that the Sr isotope ratio is consistent within these 2 years of investigation. Moreover, the Sr isotope ratio of total Sr in soil was found to be significantly higher than in an NH4NO3 extract, reflecting the mobile (bioavailable) phase. The isotope composition in the latter extract corresponds well to the range found in the asparagus samples in Marchfeld, even though the concentration of Sr in asparagus shows no direct correlation to the concentration of Sr in the mobile phase of the soil. The major question was whether the 'Marchfelder Spargel' can be distinguished from samples from the neighbouring countries of Hungary and Slovakia. According to our findings, they can be clearly (100%) singled out from the Hungarian samples and can be distinguished from the Slovakian asparagus samples with a probability of more than 80%.

  8. Identification of Marchfeld asparagus using Sr isotope ratio measurements by MC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Swoboda, S; Brunner, M; Boulyga, S F; Galler, P; Prohaska, T [University of Natural Resources and Applied Life Sciences, Department of Chemistry-VIRIS Project, Vienna (Austria); Horacek, M [Austrian Research Centers GmbH, Seibersdorf (Austria)

    2008-01-15

    This work focuses on testing and application of Sr isotope signatures for the fast and reliable authentication and traceability of Asparagus officinalis originating from Marchfeld, Austria, using multicollector inductively coupled plasma mass spectrometry after optimised Rb/Sr separation. The major sample pool comprises freeze-dried and microwave-digested asparagus samples from Hungary and Slovakia which are compared with Austrian asparagus originating from the Marchfeld region, which is a protected geographical indication. Additional samples from Peru, the Netherlands and Germany were limited in number and allowed therefore only restricted statistical evaluation. Asparagus samples from Marchfeld were harvested within two subsequent years in order to investigate the annual variation. The results show that the Sr isotope ratio is consistent within these 2 years of investigation. Moreover, the Sr isotope ratio of total Sr in soil was found to be significantly higher than in an NH{sub 4}NO{sub 3} extract, reflecting the mobile (bioavailable) phase. The isotope composition in the latter extract corresponds well to the range found in the asparagus samples in Marchfeld, even though the concentration of Sr in asparagus shows no direct correlation to the concentration of Sr in the mobile phase of the soil. The major question was whether the 'Marchfelder Spargel' can be distinguished from samples from the neighbouring countries of Hungary and Slovakia. According to our findings, they can be clearly (100%) singled out from the Hungarian samples and can be distinguished from the Slovakian asparagus samples with a probability of more than 80%. (orig.)

  9. Identification of Marchfeld asparagus using Sr isotope ratio measurements by MC-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Swoboda, S.; Brunner, M.; Boulyga, S.F.; Galler, P.; Prohaska, T. [University of Natural Resources and Applied Life Sciences, Department of Chemistry-VIRIS Project, Vienna (Austria); Horacek, M. [Austrian Research Centers GmbH, Seibersdorf (Austria)

    2008-01-15

    This work focuses on testing and application of Sr isotope signatures for the fast and reliable authentication and traceability of Asparagus officinalis originating from Marchfeld, Austria, using multicollector inductively coupled plasma mass spectrometry after optimised Rb/Sr separation. The major sample pool comprises freeze-dried and microwave-digested asparagus samples from Hungary and Slovakia which are compared with Austrian asparagus originating from the Marchfeld region, which is a protected geographical indication. Additional samples from Peru, the Netherlands and Germany were limited in number and allowed therefore only restricted statistical evaluation. Asparagus samples from Marchfeld were harvested within two subsequent years in order to investigate the annual variation. The results show that the Sr isotope ratio is consistent within these 2 years of investigation. Moreover, the Sr isotope ratio of total Sr in soil was found to be significantly higher than in an NH{sub 4}NO{sub 3} extract, reflecting the mobile (bioavailable) phase. The isotope composition in the latter extract corresponds well to the range found in the asparagus samples in Marchfeld, even though the concentration of Sr in asparagus shows no direct correlation to the concentration of Sr in the mobile phase of the soil. The major question was whether the 'Marchfelder Spargel' can be distinguished from samples from the neighbouring countries of Hungary and Slovakia. According to our findings, they can be clearly (100%) singled out from the Hungarian samples and can be distinguished from the Slovakian asparagus samples with a probability of more than 80%. (orig.)

  10. The Prestudy for Studying Inorganic Nutrient Metabolism in Humans : the Aplication of ICP-MS for Determination of Stable Isotope Ratio of Fe and Zn

    International Nuclear Information System (INIS)

    Rukihati; Sumadjo

    2001-01-01

    A method is described for the determination of isotope ratio of Fe and Zn by means of inductively coupled plasma-mass spectrometry (ICP-MS). The mass spectrometer was operated in low resolution mode to provide maximal sensitivity. Typical conditions for operations were: plasma power 0.85 k W, reflected power 56 Fe/ 54 Fe, 57 Fe/ 54 Fe, 58 Fe/ 54 Fe, dan 64 Zn/ 67 Zn, 66 Zn/ 67 Zn, 68 Zn/ 67 Zn, 70 Zn/ 67 Zn measured by ICP-MS showed a good level of agreement with TIMS (thermal ionization mass spectrometry). This method was prepared for studying the absorption and/or metabolism of inorganic nutrients in humans. (author)

  11. Determination of uranium in natural waters and high-purity aluminum by flow-injection on-line preconcentration and ICP-MS detection

    International Nuclear Information System (INIS)

    Seki, Tatsuya; Oguma, Koichi

    2004-01-01

    A flow injection method has been developed for the determination of uranium is natural waters and high-purity aluminum by use of on-line preconcentration on a U/TEVA TM column and ICP-MS detection. The sample solution prepared as a nitric acid solution in 3 mol l -1 was passed through the U/TEVA TM column to collect uranium and uranium adsorbed was eluted with 0.1 mol l -1 nitric acid. The effluent was introduced directly into the nebulizer of the ICP-MS and 238 U was measured. The detection limit, calculated as 3-times the standard deviation of the background noise, was 3pg and the sample throughput was about 10 per hour. The proposed method was successfully applied to the determination of uranium in river-water reference materials, a seawater reference material and high-purity aluminum reference materials. (author)

  12. Development of a simple extraction cell with bi-directional continuous flow coupled on-line to ICP-MS for assessment of elemental associations in solid samples

    DEFF Research Database (Denmark)

    Buanuam, Janya; Tiptanasup, Kasipa; Shiowatana, Juwadee

    2006-01-01

    A continuous-flow system comprising a novel, custom-built extraction module and hyphenated with inductively coupled plasma-mass spectrometric (ICP-MS) detection is proposed for assessing metal mobilities and geochemical associations in soil compartments as based on using the three step BCR (now...... the Measurements and Testing Programme of the European Commission) sequential extraction scheme. Employing a peristaltic pump as liquid driver, alternate directional flows of the extractants are used to overcome compression of the solid particles within the extraction unit to ensure a steady partitioning flow rate...... and thus to maintain constant operationally defined extraction conditions. The proposed flow set-up is proven to allow for trouble-free handling of soil samples up to 1 g and flow rates ≤ 10 mL min–1. The miniaturized extraction system was coupled to ICP-MS through a flow injection interface in order...

  13. [Effect of the chelator Zn-DTPA on the excretion of lead in lead intoxication mice detected with ICP-MS].

    Science.gov (United States)

    Li, Chen; Lu, Kai-zhi; Zhou, Qi; Wang, Qiong; Zeng, Yu-liang; Yin, Hong-jun; He, Xuan-hui; Tian, Ying; Dong, Jun-Xing

    2014-11-01

    To study the lead excretion effect of the chelator Zn-DTPA on the lead intoxication mice, inductively coupled plasma mass spectrometry (ICP-MS) was applied to detect the lead content of biological samples. The acute lead intoxication mice model was established by injecting lead acetate intraperitoneally with the dose of 1 mg. Zn-DTPA was administered intraperitoneally to mice once daily for five consecutive days 4 h after intoxication. Control group, model group, combination of Zn-DTPA and Ca-DTPA group were evaluated at the same time. The urine was collected every day. The mice were sacrificed in batches in the 2rd, 4th, 6th day. Biological samples including urine, whole blood, femur and brain were prepared and nitrated. Lead concentration was detected by ICP-MS. The result showed that Zn-DTPA could increase lead content in urine markedly and reduce lead content in blood, femur and brain.

  14. Determination of trace impurities in uranium-transition metal alloy fuels by ICP-MS using extended common analyte internal standardization (ECAIS) technique

    International Nuclear Information System (INIS)

    Saha, Abhijit; Deb, S.B.; Nagar, B.K.; Saxena, M.K.

    2015-01-01

    An analytical methodology was developed for the determination of eight trace impurities viz, Al, B, Cd, Co, Cu, Mg, Mn and Ni in three different uranium-transition metal alloy fuels (U-Me; Me = Ti, Zr and Mo) employing inductively coupled plasma mass spectrometry (ICP-MS). The well known common analyte internal standardization (CAIS) chemometric technique was modified and then employed to minimize and account for the matrix effect on analyte intensity. Standard addition of analytes to the pure synthetic U-Me sample solutions and subsequently their ≥ 94% recovery by the ICP-MS measurement validates the proposed methodology. One real sample of each of these alloys was analyzed by the developed analytical methodology and the %RSD observed was in the range of 5-8%. The method detection limits were found to be within 4-10 μg L -1 . (author)

  15. Analysis of inorganic and organic constituents of myrrh resin by GC–MS and ICP-MS: An emphasis on medicinal assets

    Directory of Open Access Journals (Sweden)

    Syed Rizwan Ahamad

    2017-07-01

    Full Text Available The aim of the present investigation was to explore the constituents of the Arabian myrrh resin obtained from Commiphora myrrha. The organic and inorganic composition of the myrrh gum resin has been investigated using gas chromatography-mass spectrometry (GC–MS and inductively coupled plasma-mass spectrometry (ICP-MS. Analysis executed by ICP-MS reveals the presence of various inorganic elements in significant amount in the myrrh resin. The elements that were found to be present in large amounts include calcium, magnesium, aluminum, phosphorus, chlorine, chromium, bromine and scandium. The important organic constituents identified in the myrrh ethanolic extract include limonene, curzerene, germacrene B, isocericenine, myrcenol, beta selinene, and spathulenol,. The present work complements other myrrh associated investigations done in the past and provides additional data for the future researches.

  16. Analysis of inorganic and organic constituents of myrrh resin by GC-MS and ICP-MS: An emphasis on medicinal assets.

    Science.gov (United States)

    Ahamad, Syed Rizwan; Al-Ghadeer, Abdul Rahman; Ali, Raisuddin; Qamar, Wajhul; Aljarboa, Suliman

    2017-07-01

    The aim of the present investigation was to explore the constituents of the Arabian myrrh resin obtained from Commiphora myrrha. The organic and inorganic composition of the myrrh gum resin has been investigated using gas chromatography-mass spectrometry (GC-MS) and inductively coupled plasma-mass spectrometry (ICP-MS). Analysis executed by ICP-MS reveals the presence of various inorganic elements in significant amount in the myrrh resin. The elements that were found to be present in large amounts include calcium, magnesium, aluminum, phosphorus, chlorine, chromium, bromine and scandium. The important organic constituents identified in the myrrh ethanolic extract include limonene, curzerene, germacrene B, isocericenine, myrcenol, beta selinene, and spathulenol,. The present work complements other myrrh associated investigations done in the past and provides additional data for the future researches.

  17. Determination of 129I/127I isotope ratios in liquid solutions and environmental soil samples by ICP-MS with hexapole collision cell

    OpenAIRE

    Izmer, A. V.; Boulyga, S. F.; Becker, J. S.

    2003-01-01

    The determination of I-129 in environmental samples at ultratrace levels is very difficult by ICP-MS due to a high noise caused by Xe impurities in argon plasma gas (interference of Xe-129(+)), possible (IH2+)-I-127 interference and an insufficient abundance ratio sensitivity of the ICP mass spectrometer for I-129/I-127 isotope ratio measurement. A sensitive, powerful and fast analytical technique for iodine isotope ratio measurements in aqueous solutions and contaminated soil samples directl...

  18. Linearity testing and dead-time determination for MC-ICP-MS ion counters using the IRMM-072 series of uranium isotope reference materials

    OpenAIRE

    RICHTER Stephan; KONEGGER-KAPPEL S.; BOULYGA S.; STADELMANN G.; KOEPF A.; SIEGMUND H.

    2016-01-01

    The Environmental Sample Laboratory (ESL) of the International Atomic Energy Agency (IAEA) routinely analyses environmental swipe samples for their bulk U and Pu isotope amounts and ratios using a Neptune Plus™ (Thermo Fisher Scientific) multi collector-inductively coupled plasma mass spectrometer (MC-ICP-MS). The instrument is equipped with the so-called “L5 ion counter package”, which comprises ten Faraday cups, three classical discrete dynode secondary electron multipliers (SEM), and two c...

  19. Determination 230Th by ICP-MS for the control of activities of restoration of an area of land contaminated with uranium mining sterile

    International Nuclear Information System (INIS)

    Yague, L.; Conde, E.; Navarro, N.; Fernandez, M.; Ortiz, M. I.; Noguerales, C.; Gasco, C.

    2013-01-01

    In 2012, within the activities for the Project PIMIC (CIEMAT) took out the first stage of restoration of a contaminated area. This is an area which had a residual contamination due to burial tailings uranium mining. The activities have been: elimination of the arboreal mass, excavation of the ground and earthmoving. The methodology applied is described in this work and is based on the combination of gamma spectrometry technique and development of a method of analysis 230 Th by ICP-MS. (Author)

  20. An investigation by LA-ICP-MS of possum tooth enamel as a model for identifying childhood geographical locations of historical and archaeological human remains from New Zealand

    International Nuclear Information System (INIS)

    Cameron, N.E.; Balks, M.; Littler, R.; Manley-Harris, M.; Te Awekotuku, N.

    2012-01-01

    LA-ICP-MS (laser ablation-inductively coupled plasma-mass spectrometry) has been used to analyse enamel from the teeth of brushtail possum (Trichosurus vulpecula) in order to model a method for identifying the childhood geographical origin of human remains within New Zealand. The model application of the method is promising for establishing locations of historical and archaeological human remains, including preserved heads, upoko tuhi. (author). 30 refs., 5 figs., 6 tabs.

  1. Analytisch-chemische aspecten van de bepaling van As, Ca, Cd, Sb, Sn, Pb, Zn in MVS-filterdestruaten met ICP-MS

    NARCIS (Netherlands)

    Velde-Koerts T van der; Lesquillier AI; Ritsema R; LAC

    1995-01-01

    In dit onderzoek werd een ICP-MS-methode ontwikkeld voor de bepaling van Ca, Zn, As, Cd, Sb, Sn en Pb in filterdestruaten. De onderste analysegrens is 30 ng/l Sb, 60 ng/l Cd, 200 ng/l As, 300 ng/l Sn, 400 ng/l Pb, 4 mug/l Zn en 20 mug/l Ca ; de precisie is beter dan 7% RSD voor Ca, 4% RSD voor

  2. Selective hydride generation- cryotrapping- ICP-MS for arsenic speciation analysis at picogram levels: analysis of river and sea water reference materials and human bladder epithelial cells

    Science.gov (United States)

    Matoušek, Tomáš; Currier, Jenna M.; Trojánková, Nikola; Saunders, R. Jesse; Ishida, María C.; González-Horta, Carmen; Musil, Stanislav; Mester, Zoltán; Stýblo, Miroslav; Dědina, Jiří

    2013-01-01

    An ultra sensitive method for arsenic (As) speciation analysis based on selective hydride generation (HG) with preconcentration by cryotrapping (CT) and inductively coupled plasma- mass spectrometry (ICP-MS) detection is presented. Determination of valence of the As species is performed by selective HG without prereduction (trivalent species only) or with L-cysteine prereduction (sum of tri- and pentavalent species). Methylated species are resolved on the basis of thermal desorption of formed methyl substituted arsines after collection at −196°C. Limits of detection of 3.4, 0.04, 0.14 and 0.10 pg mL−1 (ppt) were achieved for inorganic As, mono-, di- and trimethylated species, respectively, from a 500 μL sample. Speciation analysis of river water (NRC SLRS-4 and SLRS-5) and sea water (NRC CASS-4, CASS-5 and NASS-5) reference materials certified to contain 0.4 to 1.3 ng mL−1 total As was performed. The concentrations of methylated As species in tens of pg mL−1 range obtained by HG-CT-ICP-MS systems in three laboratories were in excellent agreement and compared well with results of HG-CT-atomic absorption spectrometry and anion exchange liquid chromatography- ICP-MS; sums of detected species agreed well with the certified total As content. HG-CT-ICP-MS method was successfully used for analysis of microsamples of exfoliated bladder epithelial cells isolated from human urine. Here, samples of lysates of 25 to 550 thousand cells contained typically tens pg up to ng of iAs species and from single to hundreds pg of methylated species, well within detection power of the presented method. A significant portion of As in the cells was found in the form of the highly toxic trivalent species. PMID:24014931

  3. Sulfate and sulfide sulfur isotopes (δ34S and δ33S) measured by solution and laser ablation MC-ICP-MS: An enhanced approach using external correction

    Science.gov (United States)

    Pribil, Michael; Ridley, William I.; Emsbo, Poul

    2015-01-01

    Isotope ratio measurements using a multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS) commonly use standard-sample bracketing with a single isotope standard for mass bias correction for elements with narrow-range isotope systems measured by MC-ICP-MS, e.g. Cu, Fe, Zn, and Hg. However, sulfur (S) isotopic composition (δ34S) in nature can range from at least − 40 to + 40‰, potentially exceeding the ability of standard-sample bracketing using a single sulfur isotope standard to accurately correct for mass bias. Isotopic fractionation via solution and laser ablation introduction was determined during sulfate sulfur (Ssulfate) isotope measurements. An external isotope calibration curve was constructed using in-house and National Institute of Standards and Technology (NIST) Ssulfate isotope reference materials (RM) in an attempt to correct for the difference. The ability of external isotope correction for Ssulfate isotope measurements was evaluated by analyzing NIST and United States Geological Survey (USGS) Ssulfate isotope reference materials as unknowns. Differences in δ34Ssulfate between standard-sample bracketing and standard-sample bracketing with external isotope correction for sulfate samples ranged from 0.72‰ to 2.35‰ over a δ34S range of 1.40‰ to 21.17‰. No isotopic differences were observed when analyzing Ssulfide reference materials over a δ34Ssulfide range of − 32.1‰ to 17.3‰ and a δ33S range of − 16.5‰ to 8.9‰ via laser ablation (LA)-MC-ICP-MS. Here, we identify a possible plasma induced fractionation for Ssulfate and describe a new method using external isotope calibration corrections using solution and LA-MC-ICP-MS.

  4. Development and validation of an ICP-MS method applied to the determination of uranium in urine

    International Nuclear Information System (INIS)

    Ferreira, Isabela M. de S.; Castro, Marcelo X. de; Fidelis, Valdir dos S.; Santos, Osvaldir P.

    2013-01-01

    The objective of this study is to propose a new methodology for uranium analyses in urine using inductively coupled plasma - mass spectrometry (ICP-MS). The urine samples were provided by nuclear facility workers, specifically, employees of the Industrias Nucleares do Brasil - INB, the company responsible for the production of nuclear fuel in Brazil. At nuclear fuel facility sites, ensure the safety of employees is essential due to the risks involved in such activity, mainly exposure to radiation. On account of that, there are federal laws that limit the ionizing radiation exposure among workers. The verification of compliance with the requirements in technical regulation is performed through monitoring programs. In vitro bioassay is a method to monitor the individual worker by the analysis of radionuclides in excreta samples (urine or feces). The determination of uranium in urine was performed without any sample pretreatment and the method was validated by observing a series of operational parameters set by the INMETRO DOQ-CGCRE-008 guide - Guideline on Validation of Analytical Methods. A limit of detection of 0.9 ng L -1 was achieved. For the evaluation of the trueness/recovery of the method, a NIST Standard Reference Material - SRM 2670a - Toxic Elements in Urine (Freeze-Dried) was used. The calculation of relative error for the Certified Reference Material was 1.96%. The reproducibility of the developed method was confirmed through intercomparison analyses. Through the evaluation of performance parameters, the ability of the developed method of determining uranium with high sensitivity and reproducibility was verified, enabling the use in either environmental or occupational exposures. (author)

  5. Speciation of As(III), As(V), MMA and DMA in contaminated soil extracts by HPLC-ICP/MS

    Energy Technology Data Exchange (ETDEWEB)

    Bissen, M.; Frimmel, F.H. [Engler-Bunte-Institut, Univ. Karlsruhe (Germany)

    2000-05-01

    A method to separate and quantify two inorganic arsenic species As(III) and As(V) and two organic arsenic species, monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA), by HPLC-ICP/MS has been developed. The separation of arsenic species was achieved on the anionic exchange column IonPac {sup trademark} AS11 (Dionex) with NaOH as mobile phase. The technique was successfully applied to analyze extracts of two contaminated soils, sampled at a former tannery site (soil 1) and a former paint production site (soil 2). The soils were extracted at pH values similar to the natural environment. Extractions were performed at different pH values with 0.3 M ammonium oxalate (pH = 3), milli-Q water (pH = 5.8), 0.3 M sodium carbonate (pH = 8) and 0.3 M sodium bicarbonate (pH = 11). No organically bound arsenic was found in the extracts. As(V) was the major component. Only up to 0.04% of the total arsenic contained in soil 1 were mobilized. The highest amount of extracted arsenic was found at the highest pH. In the milli-Q water extract of soil 1 As(III) and As(V) were found. High amounts of As(V) were found in the extracts of soil 2. Up to 20% of the total arsenic bound to soil 2 constituents were released. The results show that the mobilization of arsenic depended on the pH value of the extraction solution and the kind of extracted soil. Dramatic consequences have to be expected for pH changes in the environment especially in cases where soils contain high amounts of mobile arsenic. (orig.)

  6. Lithium and boron analysis by LA-ICP-MS results from a bowed PWR rod with contact

    Directory of Open Access Journals (Sweden)

    Puranen Anders

    2017-01-01

    Full Text Available A previously published investigation of an irradiated fuel rod from the Ringhals 2 PWR, which was bowed to contact with an adjacent rod, identified a significant but highly localised thinning of the clad wall and increased corrosion. Rod fretting was deemed unlikely due to the adhering oxide covering the surfaces. Local overheating in itself was also deemed insufficient to account for the accelerated corrosion. Instead, an enhanced concentration of lithium due to conditions of local boiling was hypothesised to explain the accelerated corrosion. Studsvik has developed a hot cell coupled LA-ICP-MS (Laser Ablation Inductively Coupled Plasma Mass Spectrometer equipment that enables a flexible means of isotopic analysis of irradiated fuel and other highly active surfaces. In this work, the equipment was used to investigate the distribution of lithium (7Li and boron (11B in the outer oxide at the bow contact area. Depth profiling in the clad oxide at the opposite side of the rod to the point of contact, which is considered to have experienced normal operating conditions and which has a typical oxide thickness, evidenced levels of ∼10–20 ppm 7Li and a 11B content reaching hundreds of ppm in the outer parts of the oxide, largely in agreement with the expected range of Li and B clad oxide concentrations from previous studies. In the contact area, the 11B content was similar to the reference condition at the opposite side. The 7Li content in the outermost oxide closest to the contact was, however, found to be strongly elevated, reaching several hundred ppm. The considerable and highly localised increase in lithium content at the area of enhanced corrosion thus offers strong evidence for a case of lithium induced breakaway corrosion during power operation, when rod-to-rod contact and high enough surface heat flux results in a very local increase in lithium concentration.

  7. Multi-elements determination in medical and edible Alpinia oxyphylla and Morinda officinalis and their decoctions by ICP-MS.

    Science.gov (United States)

    Zhao, Xiangsheng; Wei, Jianhe; Shu, Xiaoyan; Kong, Weijun; Yang, Meihua

    2016-12-01

    Contents of twenty elements (Mg, K, Ca, Na, Fe, Al, Zn, Ba, Mn, Cu, Mo, Cr, Ni, As, Se, Cd, Hg, Tl, Pb and V) in two medical and edible plant species, Alpinia oxyphylla and Morinda officinalis were simultaneously determined by inductively coupled plasma-mass spectrometry (ICP-MS) method after microwave digestion with HNO 3 -H 2 O 2 (6:1, v/v) as the digestion solvent. Certified standard reference material Poplar leaf was used to assess the accuracy of the method. The greatest contents of Mg, K, Ca, Al, Fe and Na were found in dried Alpinia oxyphylla and Morinda officinalis samples. The contents of five heavy metals including Pb, Cd, As, Hg and Cu in Alpinia oxyphylla did not exceed the limits. The contents of Pb in 76.67% samples and Cd in two batches of Morinda officinalis samples exceeded the limits set by Chinese Pharmacopeia. The contents of the selected elements in different parts (leaves, stems, roots and fruits) of Alpinia oxyphylla varied considerably. The highest concentrations of Mg, Ca, Mn and Se were found in the leaves of Alpinia oxyphylla, at the same time, while, the contents of 9 elements including Cd, Cr, Cu, As, Pb in the roots were the highest. The transfer ratios of selected elements from both species of herbs into their decoctions were reduced. Especially for the heavy metals, the transfer ratios were below 30% except As (79.73%) in Morinda officinalis. The results showed that decoction of the samples may reduce the intake of heavy metals. Copyright © 2016 Elsevier Ltd. All rights reserved.

  8. Analysis of twenty five impurities in uranium matrix by ICP-MS with iron measurement optimized by using reaction collision cell, cold plasma or medium resolution

    International Nuclear Information System (INIS)

    Quemet, Alexandre; Brennetot, Rene; Chevalier, Emilie; Prian, Edwina; Laridon, Anne-Laure; Fichet, Pascal; Goutelard, Florence; Mariet, Clarisse; Laszak, Ivan

    2012-01-01

    An analytical procedure was developed to determine the concentration of 25 impurities (Li, Be, Ti, V. Cr, Mn, Fe, Co, Ni, Cu, Zn, Zr, Mo, Ag, Cd, In, Sm, Eu, Gd, Dy, W, Pb, Bi and Th) in a uranium matrix using the quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS). The dissolution of U 3 O 8 powder was made with a mixture of hydrochloric acid and nitric acid. Then, a selective separation of uranium using the UTEVA column was used before measurement by Q-ICP-MS. The procedure developed was verified using the Certified Reference Material 'Morille'. The analytical results agree well except for 5 elements where values are underestimated (Li, Be, In, Pb and Bi). Among the list of impurities, iron was particularly investigated because it is well known that this element possesses a polyatomic interference that increases the detection limit. A comparison between iron detection limits obtained with different methods was performed. Iron polyatomic interference was at least reduced, or at best entirely resolved in some cases, by using the cold plasma or the collision/reaction cell with several gases (He, NH 3 and CH 4 ). High-resolution ICP-MS was used to compare the results obtained. A detection limit as low as 8 ng L -1 was achieved. (authors)

  9. Analysis of twenty five impurities in uranium matrix by ICP-MS with iron measurement optimized by using reaction collision cell, cold plasma or medium resolution.

    Science.gov (United States)

    Quemet, Alexandre; Brennetot, Rene; Chevalier, Emilie; Prian, Edwina; Laridon, Anne-Laure; Mariet, Clarisse; Fichet, Pascal; Laszak, Ivan; Goutelard, Florence

    2012-09-15

    An analytical procedure was developed to determine the concentration of 25 impurities (Li, Be, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Zr, Mo, Ag, Cd, In, Sm, Eu, Gd, Dy, W, Pb, Bi and Th) in a uranium matrix using the quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS). The dissolution of U(3)O(8) powder was made with a mixture of hydrochloric acid and nitric acid. Then, a selective separation of uranium using the UTEVA column was used before measurement by Q-ICP-MS. The procedure developed was verified using the Certified Reference Material "Morille". The analytical results agree well except for 5 elements where values are underestimated (Li, Be, In, Pb and Bi). Among the list of impurities, iron was particularly investigated because it is well known that this element possesses a polyatomic interference that increases the detection limit. A comparison between iron detection limits obtained with different methods was performed. Iron polyatomic interference was at least reduced, or at best entirely resolved in some cases, by using the cold plasma or the collision/reaction cell with several gases (He, NH(3) and CH(4)). High-resolution ICP-MS was used to compare the results obtained. A detection limit as low as 8 ng L(-1) was achieved. Copyright © 2012 Elsevier B.V. All rights reserved.

  10. Quantification of trace amounts of rare earth elements in high purity gadolinium oxide by sector field inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Pedreira, W.R.; Silva Queiroz, C.A. da; Abrao, A.; Pimentel, M.M.

    2004-01-01

    In recent years, rare earth elements (REEs) have received much attention in the fields of geochemistry and industry. Gadolinium oxide is used for many different high technology applications such as infrared absorbing automotive glass, petroleum cracking catalyst, gadolinium-yttrium garnets, microwave applications, and color TV tube phosphors. It can also be used in optical glass manufacturing and in the electronic industry. Rapid and accurate determinations of the rare earth elements are increasingly required as industrial demands expand. In general, the inductively coupled plasma mass spectrometry (ICP-MS) presents some advantages for trace element analysis, due to high sensitivity and resolution, when compared with other analytical techniques. In this work, sector field inductively coupled plasma mass spectrometry was used. Sixteen elements (Sc, Y, and 14 lanthanides) were determined selectively with the ICP-MS system using a concentration gradient method. The detection limits with the ICP-MS system were about 0.2-8 pg ml -1 . The recovery percentage ranged from 95 to 100% for different rare earth elements. The %R.S.D. of the methods varying between 1.5 and 2.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two high pure gadolinium oxides samples (IPEN and JMC) was performed. IPEN's material is highly pure (>99.99%) and was successfully analyzed without spectral interference

  11. Ultra-sensitive speciation analysis of mercury by CE-ICP-MS together with field-amplified sample stacking injection and dispersive solid-phase extraction.

    Science.gov (United States)

    Chen, YiQuan; Cheng, Xian; Mo, Fan; Huang, LiMei; Wu, Zujian; Wu, Yongning; Xu, LiangJun; Fu, FengFu

    2016-04-01

    A simple dispersive solid-phase extraction (DSPE) used to extract and preconcentrate ultra-trace MeHg, EtHg and Hg(2+) from water sample, and a sensitive method for the simultaneous analysis of MeHg, EtHg and Hg(2+) by using capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) with field-amplified sample stacking injection (FASI) were first reported in this study. The DSPE used thiol cotton particles as adsorbent, and is simple and effective. It can be used to extract and preconcentrate ultra-trace mercury compounds in water samples within 30 min with a satisfied recovery and no mercury species alteration during the process. The FASI enhanced the sensitivity of CE-ICP-MS with 25-fold, 29-fold and 27-fold for MeHg, EtHg and Hg(2+) , respectively. Using FASI-CE-ICP-MS together with DSPE, we have successfully determined ultra-trace MeHg, EtHg and Hg(2+) in tap water with a limits of quantification (LOQs) of 0.26-0.45 pg/mL, an RSD (n = 3) mercury. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Precision and accuracy of ST-EDXRF performance for As determination comparing with ICP-MS and evaluation of As deviation in the soil media.

    Science.gov (United States)

    Akbulut, Songul; Cevik, Ugur; Van, Aydın Ali; De Wael, Karolien; Van Grieken, Rene

    2014-02-01

    The present study was conducted to (i) determine the precision and accuracy of arsenic measurement in soil samples using ST-EDXRF by comparison with the results of ICP-MS analyses and (ii) identify the relationship of As concentration with soil characteristics. For the analysis of samples, inductively coupled plasma mass spectrometry (ICP-MS) and energy dispersive X-ray fluorescence spectrometry (EDXRF) were performed. According to the results found in the soil samples, the addition of HCl to HNO3, used for the digestion gave significant variations in the recovery of As. However, spectral interferences between peaks for As and Pb can affect detection limits and accuracy for XRF analysis. When comparing the XRF and ICP-MS results a correlation was observed with R(2)=0.8414. This means that using a ST-EDXRF spectrometer, it is possible to achieve accurate and precise analysis by the calibration of certified reference materials and choosing an appropriate secondary target. On the other hand, with regard to soil characteristics analyses, the study highlighted that As is mostly anthropogenically enriched in the studied area. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Metal-doped inorganic nanoparticles for multiplex detection of biomarkers by a sandwich-type ICP-MS immunoassay.

    Science.gov (United States)

    Ko, Jung Aa; Lim, H B

    2016-09-28

    Metal-doped inorganic nanoparticles were synthesized for the multiplex detection of biomarkers by a sandwich-type inductively coupled plasma mass spectrometry (ICP-MS) immunoassay. The synthesized Cs-doped multicore magnetic nanoparticles (MMNPs) were used not only for magnetic extraction of targets but also for ratiometric measurement in ICP-MS. In addition, three different metal/dye-doped silica nanoparticles (SNPs) were synthesized as probes for multiplex detection: Y/RhBITC (rhodamine B isothiocyanate)-doped SNPs for CRP (cardiovascular disease), Cd/RhBITC-doped SNPs for AFP (tumor), and Au/5(6)-XRITC (X-rhodamine-5-(and-6)-isothiocyanate)-doped SNPs for NSE (heart disease). For quantification, the doped metals of SNPs were measured by ICP-MS and then the signal ratio to Cs of MMNPs was plotted with respect to the concentration of targets by a ratiometry. Limits of detection (LOD) of 0.35 ng/mL to 77 ng mL(-1) and recoveries of 83%-125% were obtained for serum samples spiked with the biomarkers. Since no sample treatment was necessary prior to the extraction, the proposed method provided short analysis time and convenience for the multiplex determination of biomarkers, which will be valuable for clinical application. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. An exploration hydrogeochemical study at the giant Pebble porphyry Cu-Au-Mo deposit, Alaska, USA, using high-resolution ICP-MS

    Science.gov (United States)

    Eppinger, Robert G.; Fey, David L.; Giles, Stuart A.; Kelley, Karen D.; Smith, Steven M.

    2012-01-01

    A hydrogeochemical study using high resolution ICP-MS was undertaken at the giant Pebble porphyry Cu-Au-Mo deposit and surrounding mineral occurrences. Surface water and groundwater samples from regional background and the deposit area were collected at 168 sites. Rigorous quality control reveals impressive results at low nanogram per litre (ng/l) levels. Sites with pH values below 5.1 are from ponds in the Pebble West area, where sulphide-bearing rubble crop is thinly covered. Relative to other study area waters, anomalous concentrations of Cu, Cd, K, Ni, Re, the REE, Tl, SO42− and F− are present in water samples from Pebble West. Samples from circum-neutral waters at Pebble East and parts of Pebble West, where cover is much thicker, have anomalous concentrations of Ag, As, In, Mn, Mo, Sb, Th, U, V, and W. Low-level anomalous concentrations for most of these elements were also found in waters surrounding nearby porphyry and skarn mineral occurrences. Many of these elements are present in low ng/l concentration ranges and would not have been detected using traditional quadrupole ICP-MS. Hydrogeochemical exploration paired with high resolution ICP-MS is a powerful new tool in the search for concealed deposits.

  15. Multielement determination and speciation of major-to-ultratrace elements in green tea leaves by ICP-AES and ICP-MS

    International Nuclear Information System (INIS)

    Matsuura, Hirotaka; Hokura, Akiko; Haraguchi, Hiroki

    2000-01-01

    In order to investigate the multi-elemental composition of green tea leaves as well as chemical species in tea infusions, inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) were used for elemental analysis and elemental speciation with the aid of size exclusion chromatography (SEC). As a result, the multielement determination of major-to-ultratrace elements in green tea leaves and green tea infusions was carried out by ICP-AES and ICP-MS. About 40 elements in these tea samples could be determined in a wide concentration range of over 8 orders of magnitude. The extraction efficiency of each element was estimated as the ratio of its concentration in tea infusion to that in tea leaves. It was found from the experimental results that the elements in tea leaves could be classified into three characteristic groups, depending on their extraction efficiencies. Furthermore, tea infusions were analyzed by a combined system of SEC, UV absorption detector, and ICP-AES (or ICP-MS) for the speciation of major-to-ultratrace elements. Most of the elements in tea infusions were found to be present as associated complexes with large organic molecules. (author)

  16. Measurement of isotopic composition of lanthanides in reprocessing process solutions by high-performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC/ICP-MS)

    International Nuclear Information System (INIS)

    Okano, Masanori; Jitsukata, Shu; Kuno, Takehiko; Yamada, Keiji

    2011-01-01

    Isotopic compositions of fission products in process solutions and wastes in a reprocessing plant are valuable to proceed safety study of the solutions and research/development concerning treatment/disposal of the wastes. The amount of neodymium-148 is a reliable indication to evaluate irradiation history. The isotopic compositions of samarium and gadolinium in high radioactive wastes are referred to as essential data to evaluate environmental impact in geological repositories. However, pretreatment of analysis must be done with complicated chemical separation such as solvent extraction and ion exchange. The actual measurement data of isotopic compositions of lanthanides comparable to the one of actinides in spent fuel reprocessing process has not been obtained enough. Rapid and high sensitive analytical technique based on high-performance liquid chromatography (HPLC) with an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the measurement of isotopic compositions of lanthanides in spent fuel reprocessing solutions. HPLC/ICP-MS measurement system was customized for a glove-box to be applied to the radioactive solutions. The cation exchange chromatographic columns (Shim-pack IC-C1) and injection valve (20μL) were located inside of the glove-box except the chromatographic pump. The elements of lanthanide group were separated by a gradient program of HPLC with α-hydroxyisobutyric acid. Isotopic compositions of lanthanides in eluate was sequentially analyzed by a quadruple ICP-MS. Optimization of parameter of HPLC and ICP-MS measurement system was examined with standard solutions containing 14 lanthanide elements. The elements of lanthanides were separated by HPLC and detected by ICP-MS within 25 minutes. The detection limits of Nd-146, Sm-147 and Gd-157 were 0.37 μg L -1 , 0.69 μg L -1 and 0.47 μg L -1 , respectively. The analytical precision of the above three isotopes was better than 10% for standard solutions of 100 μg L -1 with

  17. A novel quantification strategy of transferrin and albumin in human serum by species-unspecific isotope dilution laser ablation inductively coupled plasma mass spectrometry (ICP-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Feng, Liuxing, E-mail: fenglx@nim.ac.cn; Zhang, Dan; Wang, Jun; Shen, Dairui; Li, Hongmei

    2015-07-16

    Highlights: • Species-unspecific ID-PAGE-LA-ICP-MS was used to quantify Alb and Tf in human serum. • Addition methods of species-unspecific {sup 34}S spike were evaluated. • Isotope change conditions were investigated to reach satisfactory “isotope equilibration”. • Human serum CRM (ERM-DA470k/IFCC) was used to validate the new arrangements. • The developed method offers potential for accurate quantification of protein by ID-PAGE-LA-ICP-MS. - Abstract: Species-specific (SS) isotope dilution analysis with gel electrophoresis (GE)-laser ablation (LA)-ICP-MS is a promising technique for the quantification of particular metal-binding proteins in biological samples. However, unavailable isotopically enriched spike and metal losses in GE separation are main limitations for SS-isotope dilution PAGE-LA-ICP-MS. In this study, we report for the first time the absolute quantification of transferrin (Tf) and albumin (Alb) in human serum by non-denaturing (native) GE combined with species-unspecific isotope dilution mass spectrometry (IDMS). In order to achieve a homogeneous distribution of both protein and isotope-enriched spike (simulated isotope equilibration), immersing the protein strips with {sup 34}S spike solution after gel electrophoresis was demonstrated to be an effective way of spike addition. Furthermore, effects of immersion time and {sup 34}S spike concentration were investigated to obtain optimal conditions of the post-electrophoresis isotope dilution method. The relative mass of spike and ablated sample (m{sub sp}/m{sub sam}) in IDMS equation was calculated by standard Tf and Alb proteins, which could be applied to the quantification of Tf and Alb in ERM-DA470k/IFCC for method confirmation. The results were in agreement with the certified value with good precision and small uncertainty (1.5–3%). In this method, species-specific spike protein is not necessary and the integrity of the heteroatom-protein could be maintained in sample preparation

  18. A novel quantification strategy of transferrin and albumin in human serum by species-unspecific isotope dilution laser ablation inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Feng, Liuxing; Zhang, Dan; Wang, Jun; Shen, Dairui; Li, Hongmei

    2015-01-01

    Highlights: • Species-unspecific ID-PAGE-LA-ICP-MS was used to quantify Alb and Tf in human serum. • Addition methods of species-unspecific 34 S spike were evaluated. • Isotope change conditions were investigated to reach satisfactory “isotope equilibration”. • Human serum CRM (ERM-DA470k/IFCC) was used to validate the new arrangements. • The developed method offers potential for accurate quantification of protein by ID-PAGE-LA-ICP-MS. - Abstract: Species-specific (SS) isotope dilution analysis with gel electrophoresis (GE)-laser ablation (LA)-ICP-MS is a promising technique for the quantification of particular metal-binding proteins in biological samples. However, unavailable isotopically enriched spike and metal losses in GE separation are main limitations for SS-isotope dilution PAGE-LA-ICP-MS. In this study, we report for the first time the absolute quantification of transferrin (Tf) and albumin (Alb) in human serum by non-denaturing (native) GE combined with species-unspecific isotope dilution mass spectrometry (IDMS). In order to achieve a homogeneous distribution of both protein and isotope-enriched spike (simulated isotope equilibration), immersing the protein strips with 34 S spike solution after gel electrophoresis was demonstrated to be an effective way of spike addition. Furthermore, effects of immersion time and 34 S spike concentration were investigated to obtain optimal conditions of the post-electrophoresis isotope dilution method. The relative mass of spike and ablated sample (m sp /m sam ) in IDMS equation was calculated by standard Tf and Alb proteins, which could be applied to the quantification of Tf and Alb in ERM-DA470k/IFCC for method confirmation. The results were in agreement with the certified value with good precision and small uncertainty (1.5–3%). In this method, species-specific spike protein is not necessary and the integrity of the heteroatom-protein could be maintained in sample preparation process. Moreover, the

  19. Comparative evaluation of ICP sample introduction systems to be used in the metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS.

    Science.gov (United States)

    Klencsár, Balázs; Sánchez, Carlos; Balcaen, Lieve; Todolí, José; Lynen, Frederic; Vanhaecke, Frank

    2018-05-10

    A systematic evaluation of four different ICP sample introduction systems to be used in the context of metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS was carried out using diclofenac and its major metabolite, 4'-hydroxy-diclofenac, as model compounds. The strict requirements for GMP validation of chromatographic methods in the pharmaceutical industry were adhered to in this context. The final aim of this investigation is an extension of the applicability and validatability of HPLC-ICP-MS in the field of pharmaceutical R&D. Five different gradient programmes were tested while the baseline peak width (w b ), peak capacity (P), USP tailing factor (A s ) and USP signal-to-noise ratio (USP S/N) were determined as major indicators of the chromatographic performance and the values obtained were compared to the corresponding FDA recommendations (if applicable). Four different ICP-MS sample introductions systems were investigated involving two units typically working at higher flow rates (∼1.0 mL min -1 ) and another two systems working at lower flow rates (∼0.1 mL min -1 ). Optimal conditions with potential for applicability under GMP conditions were found at a mobile phase flow rate of 1.0 mL min -1 by using a pneumatic micro-flow LC nebulizer mounted onto a Peltier-cooled cyclonic spray chamber cooled to -1 °C for sample introduction. Under these conditions, HPLC-ICP-MS provided a chromatographic performance similar to that of HPLC with UV detection. The peak shape (USP tailing factor = 1.1-1.4) was significantly improved compared to that obtained with the Peltier-cooled Scott-type spray chamber. Two alternative sample introduction systems - a POINT ® and a High-Temperature Torch-Integrated Sample Introduction System (hTISIS) - were also tested at a flow rate of 0.1 mL min -1 using a chromatographic column with 1.0 mm ID. Although these systems allowed the peak shape to be improved compared to that obtained with

  20. Determination of the platinum - group elements (PGE) and gold (Au) in the manganese nodule reference samples by nickel sulfide fire-assay and Te coprecipitation with ICP-MS

    Digital Repository Service at National Institute of Oceanography (India)

    Balaram, V.; Mathur, R.; Banakar, V.K.; Hein, J.R.; Rao, C.R.M.; Rao, T.G.; Dasaram, B.

    Platinum group elements (PGE) and Au data in polymetallic oceanic ferromanganese nodule reference samples and crust samples obtained by inductively coupled plasma mass spectrometry (ICP-MS), after separation and pre-concentration by nickel sulfide...

  1. [A comparative study of cadmium, lead, mercury, arsenic, selenium, manganese, copper and zinc in brown rice and fish by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic absorption spectrometry].

    Science.gov (United States)

    Oshima, Harumi; Ueno, Eiji; Saito, Isao; Matsumoto, Hiroshi

    2004-10-01

    A study was conducted to evaluate the applicability of ICP-MS techniques for determination of metals in brown rice and fish. Cadmium, lead, mercury, arsenic, selenium, manganese, copper and zinc were determined by this method. An open digestion with nitric acid (Method A) and a rapid open digestion with nitric acid and hydrochloric acid (Method B) were used to solubilize analytes in samples, and these procedures were followed by ICP-MS analysis. Recovery of certified elements from standard reference materials by Method A and Method B ranged from 92 to 110% except for mercury (70 to 100%). Analytical results of brown rice and fish samples obtained by this ICP-MS agreed with those obtained by atomic absorption spectrometry (AAS). The results of this study demonstrate that quadrupole ICP-MS provides precise and accurate measurements of the elements tested in brown rice and fish samples.

  2. Experimental design for TBT quantification by isotope dilution SPE-GC-ICP-MS under the European water framework directive.

    Science.gov (United States)

    Alasonati, Enrica; Fabbri, Barbara; Fettig, Ina; Yardin, Catherine; Del Castillo Busto, Maria Estela; Richter, Janine; Philipp, Rosemarie; Fisicaro, Paola

    2015-03-01

    In Europe the maximum allowable concentration for tributyltin (TBT) compounds in surface water has been regulated by the water framework directive (WFD) and daughter directive that impose a limit of 0.2 ng L(-1) in whole water (as tributyltin cation). Despite the large number of different methodologies for the quantification of organotin species developed in the last two decades, standardised analytical methods at required concentration level do not exist. TBT quantification at picogram level requires efficient and accurate sample preparation and preconcentration, and maximum care to avoid blank contamination. To meet the WFD requirement, a method for the quantification of TBT in mineral water at environmental quality standard (EQS) level, based on solid phase extraction (SPE), was developed and optimised. The quantification was done using species-specific isotope dilution (SSID) followed by gas chromatography (GC) coupled to inductively coupled plasma mass spectrometry (ICP-MS). The analytical process was optimised using a design of experiment (DOE) based on a factorial fractionary plan. The DOE allowed to evaluate 3 qualitative factors (type of stationary phase and eluent, phase mass and eluent volume, pH and analyte ethylation procedure) for a total of 13 levels studied, and a sample volume in the range of 250-1000 mL. Four different models fitting the results were defined and evaluated with statistic tools: one of them was selected and optimised to find the best procedural conditions. C18 phase was found to be the best stationary phase for SPE experiments. The 4 solvents tested with C18, the pH and ethylation conditions, the mass of the phases, the volume of the eluents and the sample volume can all be optimal, but depending on their respective combination. For that reason, the equation of the model conceived in this work is a useful decisional tool for the planning of experiments, because it can be applied to predict the TBT mass fraction recovery when the

  3. Application of ICP-MS and AMS for determination of Pu- and U-isotope ratios for source identification

    Energy Technology Data Exchange (ETDEWEB)

    Skipperud, L. (Norwegian Univ. of Life Sciences, Isotope Lab.. Dept. of Plant and Environmental Sciences, AAs (Norway))

    2010-03-15

    the Pu-240/Pu-239 ratio offers a reliable way of distinguishing weapon's grade sources from global fallout. Since these two isotopes are not separated easily by conventional alfa spectrometry techniques, mass spectrometry is required for an assessment of the isotope ratios. Because of the low levels of plutonium in the Arctic area, plutonium concentrations and 240/239 ratios have been determined using accelerator mass spectrometry (AMS), which has proved a useful and reliable method for analysis of plutonium. ICP-MS has proven to be a good tool together with traditional alfa spectrometry when it comes to analysing plutonium and its isotope ratios in more contaminated areas. (author)

  4. Assessment of drinking water quality using ICP-MS and microbiological methods in the Bholakpur area, Hyderabad, India.

    Science.gov (United States)

    Abdul, Rasheed M; Mutnuri, Lakshmi; Dattatreya, Patil J; Mohan, Dayal A

    2012-03-01

    A total of 16 people died and over 500 people were hospitalized due to diarrhoeal illness in the Bholakpur area of Hyderabad, India on 6th May 2009. A study was conducted with immediate effect to evaluate the quality of municipal tap water of the Bholakpur locality. The study consists of the determination of physico-chemical properties, trace metals, heavy metals, rare earth elements and microbiological quality of drinking water. The data showed the variation of the investigated parameters in samples as follows: pH 7.14 to 8.72, EC 455 to 769 μS/cm, TDS 303.51 to 515.23 ppm and DO 1.01 to 6.83 mg/L which are within WHO guidelines for drinking water quality. The water samples were analyzed for 27 elements (Li, Be, B, Na, Mg, Al, Si, K, Ca, V, Cr, Mn, Fe, Ni, Co, Cu, Zn, As, Se, Rb, Sr, Mo, Ag, Cd, Sb, Ba and Pb) using inductively coupled plasma-mass spectrometry (ICP-MS). The concentrations of Fe (0.12 to 1.13 mg/L), Pb (0.01 to 0.07 mg/L), Cu (0.01 to 0.19 mg/L), Ni (0.01 to 0.15 mg/L), Al (0.16 to 0.49 mg/L), and Na (38.36 to 68.69 mg/L) were obtained, which exceed the permissible limits of the World Health Organization (WHO) for drinking water quality guidelines. The remaining elements were within the permissible limits. The microbiological quality of water was tested using standard plate count, membrane filtration technique, thermotolerant coliform (TTC), and most probable number (MPN) methods. The total heterotrophic bacteria ranged from 1.0 × 10(5) to 18 × 10(7 )cfu/ml. Total viable bacteria in all the water samples were found to be too numerable to count and total number of coliform bacteria in all water samples were found to be of order of 1,100 to >2,400 MPN index/100 ml. TTC tested positive for coliform bacteria at 44.2°C. All the water samples of the study area exceeded the permissible counts of WHO and that (zero and minimal counts) of the control site (National Geophysical Research Institute) water samples. Excessively high colony numbers indicate

  5. High-Precision Measurement of Eu/Eu* in Geological Glasses via LA-ICP-MS Analysis

    Science.gov (United States)

    Tang, Ming; McDonough, William F.; Arevalo, Ricardo, Jr.

    2014-01-01

    Elemental fractionation during laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) analysis has been historically documented between refractory and volatile elements. In this work, however, we observed fractionation between light rare earth elements (LREEs) and heavy rare earth elements (HREEs) when using ablation strategies involving large spot sizes (greater than 100 millimeters) and line scanning mode. In addition: (1) ion yields decrease when using spot sizes above 100 millimeters; (2) (Eu/Eu*)(sub raw) (i.e. Europium anomaly) positively correlates with carrier gas (He) flow rate, which provides control over the particle size distribution of the aerosol reaching the ICP; (3) (Eu/Eu*)(sub raw) shows a positive correlation with spot size, and (4) the changes in REE signal intensity, induced by the He flow rate change, roughly correlate with REE condensation temperatures. The REE fractionation is likely driven by the slight but significant difference in their condensation temperatures. Large particles may not be completely dissociated in the ICP and result in preferential evaporation of the less refractory LREEs and thus non-stoichiometric particle-ion conversion. This mechanism may also be responsible for Sm-Eu-Gd fractionation as Eu is less refractory than Sm and Gd. The extent of fractionation depends upon the particle size distribution of the aerosol, which in turn is influenced by the laser parameters and matrix. Ablation pits and lines defined by low aspect ratios produce a higher proportion of large particles than high aspect ratio ablation, as confirmed by measurements of particle size distribution in the laser induced aerosol. Therefore, low aspect ratio ablation introduces particles that cannot be decomposed and/or atomized by the ICP and thus results in exacerbated elemental fractionation. Accurate quantification of REE concentrations and Eu/Eu* requires reduction of large particle production during laser ablation. For the reference

  6. Exploiting dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) for sequential determination of trace elements in blood using a dilute-and-shoot procedure

    International Nuclear Information System (INIS)

    Lemos Batista, Bruno; Lisboa Rodrigues, Jairo; Andrade Nunes, Juliana; Oliveira Souza, Vanessa Cristina de; Barbosa, Fernando

    2009-01-01

    Inductively coupled plasma mass spectrometry with quadrupole (q-ICP-MS) and dynamic reaction cell (DRC-ICP-MS) were evaluated for sequential determination of As, Cd, Co, Cr, Cu, Mn, Pb, Se, Tl, V and Zn in blood. The method requires as little as 100 μL of blood. Prior to analysis, samples (100 μL) were diluted 1:50 in a solution containing 0.01% (v/v) Triton X-100 and 0.5% (v/v) nitric acid. The use of the DRC was only mandatory for Cr, Cu, V and Zn. For the other elements the equipment may be operated in a standard mode (q-ICP-MS). Ammonia was used as reaction gas. Selection of best flow rate of ammonium gas and optimization of the quadrupole dynamic band-pass tuning parameter (RPq) were carried out, using a ovine base blood for Cr and V and a synthetic matrix solution (SMS) for Zn and Cu diluted 1:50 and spiked to contain 1 μg L -1 of each element. Method detection limits (3 s) for 75 As, 114 Cd, 59 Co, 51 Cr, 63 Cu 55 Mn, 208 Pb, 82 Se, 205 Tl, 51 V, and 64 Zn were 14.0, 3.0, 11.0, 7.0, 280, 9.0, 3.0, 264, 0.7, 6.0 and 800 ng L -1 , respectively. Method validation was accomplished by the analysis of blood Reference Materials produced by the L'Institut National de Sante Publique du Quebec (Canada).

  7. Usefulness of laser ablation ICP-MS for analysis of metallic particles released to oral mucosa after insertion of dental implants.

    Science.gov (United States)

    Sajnóg, Adam; Hanć, Anetta; Koczorowski, Ryszard; Makuch, Krzysztof; Barałkiewicz, Danuta

    2018-03-01

    Despite the fact that titanium is considered highly biocompatible, its presence in the oral cavity (an environment of frequently changing pH and temperature) may result in the release of titanium from intraosseous implants into the oral mucosa, causing a range of reactions from the human body. Fragments of oral mucosa collected from patients after dental implant insertion were analyzed by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The study revealed an elevated content of elements (Ti, Al, V) which are components of the metal implants and temporary cover screws. Dynamic ablation of the tissue surface was used in order to obtain maps of the content and distribution of analyzed elements. The material consisted of 30 oral mucosa tissue fragments collected 3-5 months after implantation and 10 samples collected before implantation (control group). The application of optical microscope allowed for indication and confirmation of the location of metal particles prior to LA-ICP-MS analysis. The so-obtained map permitted location of regions containing metal particles. LA-ICP-MS analysis revealed groups of samples with similar properties of metal particles, thus confirming that those metal particles were the main source of the elevated content of metals (Ti, Al, V) in the tissue after implantation. A calibration strategy based on matrix matched solid standards with powdered egg white proteins as matrix material was applied with 34 S as an internal standard. The accuracy of the analytical method was verified by ablating pellets of certified reference material ERM-BB422 Fish muscle. Copyright © 2017 Elsevier GmbH. All rights reserved.

  8. Rapid actinide analysis method coupling liquid chromatography/ICP-MS and "9"0Sr gas proportional counter in post-accidental situation environmental samples

    International Nuclear Information System (INIS)

    Habibi, Azza

    2015-01-01

    The present study follows the Fukushima power plant accident and aimed to develop an analytical method to achieve, during an emergency situation, a rapid identification and quantification of alpha and beta emitters in environmental samples. The first step of this study allowed us to list the alpha and beta emitters which can be released in the environment in case of a nuclear accident. The second step aimed towards the development of a rapid analysis method to quantify 17 radionuclides of U, Th, Pu, Am, Np and Sr. The main objective was the automation of the radiochemical separation step and its coupling for the measurement. The separation is performed using columns containing extraction resins, namely TEVA, TRU and Sr. The measurement is performed using an ICP-MS (inductively coupled plasma mass spectrometry) and in some cases a gas proportional counter to quantify radiostrontium ("8"9Sr and "9"0Sr). Excellent figures of merit were obtained, off line, with water (tap, river and sea water) and solid matrices (soil and aerosol filters), after a micro-wave digestion or an alkaline fusion dissolution followed by a Ca_3(PO_4)_2 coprecipitation. The proposed analytical strategy showed yields between 70 % and 100 % and standard deviations between 5 % and 10 %. The newly developed separation method was then automated and coupled on-line to ICP-MS. The operating parameters were optimized using a design of experiments and the results were processed with Minitab. The optimized automated separation coupled on-line to the ICP-MS allows the rapid quantification, in 1.5 h per sample, of U, Th, Pu, Am, Np and Sr with detection limits gain as high as 20 times for artificial radionuclide. (author)

  9. A validated inductively coupled plasma mass spectrometry (ICP-MS) method for the quantification of total platinum content in plasma, plasma ultrafiltrate, urine and peritoneal fluid.

    Science.gov (United States)

    Lemoine, Lieselotte; Thijssen, Elsy; Noben, Jean-Paul; Adriaensens, Peter; Carleer, Robert; Speeten, Kurt Van der

    2018-04-15

    Oxaliplatin is a platinum (Pt) 1 containing antineoplastic agent that is applied in current clinical practice for the treatment of colon and appendiceal neoplasms. A fully validated, highly sensitive, high throughput inductively coupled plasma mass spectrometry (ICP-MS) method is provided to quantify the total Pt content in plasma, plasma ultrafiltrate, urine and peritoneal fluid. In this ICP-MS approach, the only step of sample preparation is a 1000-fold dilution in 0.5% nitric acid, allowing the analysis of 17 samples per hour. Detection of Pt was achieved over a linear range of 0.01-100 ng/mL. The limit of quantification was 18.0 ng/mL Pt in plasma, 8.0 ng/mL in ultrafiltrate and 6.1 ng/mL in urine and peritoneal fluid. The ICP-MS method was further validated for inter-and intraday precision and accuracy (≤15%), recovery, robustness and stability. Short-term storage of the biofluids, for 14 days, can be performed at -4 °C, -24 °C and -80 °C. As to long-term stability, up to 5 months, storage at -80 °C is encouraged. Furthermore, a timeline assessing the total and unbound Pt fraction in plasma and ultrafiltrate over a period of 45 h is provided. Following an incubation period of 5 h at 37 °C, 19-21% of Pt was recovered in the ultrafiltrate, emphasizing the extensive and rapid binding of oxaliplatin-derived Pt to plasma proteins. The described method can easily be implemented in a routine setting for pharmacokinetic studies in patients treated with oxaliplatin-based hyperthermic intraperitoneal perioperative chemotherapy. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Tissue gadolinium deposition in hepatorenally impaired rats exposed to Gd-EOB-DTPA: evaluation with inductively coupled plasma mass spectrometry (ICP-MS).

    Science.gov (United States)

    Sato, Tomohiro; Tamada, Tsutomu; Watanabe, Shigeru; Nishimura, Hirotake; Kanki, Akihiko; Noda, Yasufumi; Higaki, Atsushi; Yamamoto, Akira; Ito, Katsuyoshi

    2015-06-01

    This study was undertaken to quantify tissue gadolinium (Gd) deposition in hepatorenally impaired rats exposed to gadolinium ethoxybenzyl diethylenetriamine pentaacetic acid (Gd-EOB-DTPA) by means of inductively coupled plasma mass spectrometry (ICP-MS) and to compare differences in Gd distribution among major organs as possible triggers for nephrogenic systemic fibrosis. Five hepatorenally impaired rats (5/6-nephrectomized, with carbon-tetrachloride-induced liver fibrosis) were injected with Gd-EOB-DTPA. Histological assessment was conducted and Gd content of the skin, liver, kidneys, lungs, heart, spleen, diaphragm, and femoral muscle was measured by inductively coupled plasma mass spectrometry (ICP-MS) at 7 days after last injection. In addition, five renally impaired rats were injected with Gd-EOB-DTPA and the degree of tissue Gd deposition was compared with that in the hepatorenally impaired rats. ICP-MS analysis revealed significantly higher Gd deposition in the kidneys, spleen, and liver (p = 0.009-0.047) in the hepatorenally impaired group (42.6 ± 20.1, 17.2 ± 6.1, 8.4 ± 3.2 μg/g, respectively) than in the renally impaired group (17.2 ± 7.7, 5.4 ± 2.1, 2.8 ± 0.7 μg/g, respectively); no significant difference was found for other organs. In the hepatorenally impaired group, Gd was predominantly deposited in the kidneys, followed by the spleen, liver, lungs, skin, heart, diaphragm, and femoral muscle. Histopathological investigation revealed hepatic fibrosis in the hepatorenally impaired group. Compared with renally impaired rats, tissue Gd deposition in hepatorenally impaired rats exposed to Gd-EOB-DTPA was significantly increased in the kidneys, spleen, and liver, probably due to the impairment of the dual excretion pathways of the urinary and biliary systems.

  11. Contribution to the understanding of ion-gas reactions in ICP-MS collision reaction cells: application to the resolution of isobaric and polyatomic interferences

    International Nuclear Information System (INIS)

    Quemet, A.

    2012-01-01

    Inductively Coupled Plasma Mass Spectrometry (ICP-MS) emerged as the most essential technique in inorganic analytical chemistry thanks to its numerous assets, particularly its flexibility, its sensitivity and its reproducibility. As part of the elementary and isotopic analysis of irradiated fuel and transmutation target, the analyst is faced with a complex mass spectrum, due to the presence of many radionuclides. ICP-MS can not differentiate ions with the same mass, which induces isobaric and polyatomic interferences when the ions at the same mass are different chemical species. Last generations of ICP-MS have introduced collision reaction cells. It can in situ reduce these isobaric or polyatomic interferences. The cell is a multipole (quadrupole, hexapole or octupole) device filled with a collision and/or reaction gas. The gas molecules collide or possibly react with the ion beam, which eliminates or reduces interferences. Such resolution of interferences is based on the difference of chemical behaviours between the analyte and the interfering species: the choice of the gas is crucial. A better understanding of the 'ion - gas' reaction should help choosing the reacting gases. Three ICP-MS, with the different cell geometries, were used for this study: Perkin Elmer Elan DRC e (quadrupole), Thermo Fischer X serie II (hexapole) and Agilent Technologies 7700x (octupole). The effects of the cell geometry on different experimental parameters and on the resolution of the 56 Fe + / 40 Ar 16 O + polyatomic interferences were examined to measure iron at trace or ultra-trace level. This preliminary study was applied to measure iron as impurities in uranium oxide, the method was then validated with a Certified Reference Material. The reactivities of transition metals (Zr, Ru, Pd, Ag, Cd, Sn), lanthanides (La, Ce, Nd, Sm, Eu, Gd, Dy, Er and Yb) and actinides (U, Np, Pu, Am and Cm), elements of interest in the nuclear field, are studied with numerous gases (O 2 , CO, CO 2 , N 2

  12. Trace elements in landfill calcite: a comparison of solution & laser ablation ICP-MS and calibration to different standard material (SRM NIST glass and USGS MACS carbonate)

    Czech Academy of Sciences Publication Activity Database

    Strnad, L.; Ettler, V.; Mihaljevič, M.; Hladil, Jindřich

    2008-01-01

    Roč. 9, - (2008), s. 235-236 ISSN 1885-7264. [Reunión de la Sociedad Española de Mineralogía /28./ ; Reunión de la Sociedad Española de Arcillas /21./. Zaragoza, 16.09.2008-19.09.2008] R&D Projects: GA AV ČR IAA300130702 Institutional research plan: CEZ:AV0Z30130516 Keywords : trace elements * reference material * carbonate * ICP-MS * laser ablation Subject RIV: DB - Geology ; Mineralogy http://www.ehu.es/sem/macla_pdf/macla9/macla9_235.pdf

  13. Boron analyses in the reactor coolant system of French PWR by acid-base titration ([B]) and ICP-MS (10B atomic %): key to NPP safety

    International Nuclear Information System (INIS)

    Jouvet, Fabien; Roux, Sylvie; Carabasse, Stephanie; Felgines, Didier

    2012-09-01

    Boron is widely used by Nuclear Power Plants and especially by EDF Pressurized Water Reactors to ensure the control of the neutron rate in the reactor coolant system and, by this way, the fission reaction. The Boron analysis is thus a major factor of safety which enables operators to guarantee the permanent control of the reactor. Two kinds of analyses carried out by EDF on the Boron species, recently upgraded regarding new method validation standards and developed to enhance the measurement quality by reducing uncertainties, will be discussed in this topic: Acid-Base titration of Boron and Boron isotopic composition by Inductively Coupled Plasma Mass Spectrometer - ICP MS. (authors)

  14. ICP-MS as the method of the determination of gallium, indium and thallium isotope ratios in the studies of isotope effects in the chromatography systems

    International Nuclear Information System (INIS)

    Herdzik, I.

    2006-01-01

    The procedure of the determination of gallium, indium and thallium isotope ratios and its application to the studies of the isotope effects in chromatography systems by the ICP-MS method (inductively coupled plasma-mass spectrometry) are presented. It was shown that it is possible to determine the isotope ratios of gallium ( 69/71 Ga), indium ( 113/115 In) and thallium ( 203/205 Tl) with the relative standard deviation 0.03-0.07%. Such precision appeared to be sufficient to calculate the unit separation factors in the column chromatographic processes. (author) [pl

  15. Analysis of geochemical "twins" A1/Ga and Si/Ge in rock-forming silicate minerals in granitoides using LA-ICP-MS

    Czech Academy of Sciences Publication Activity Database

    Gardenová, N.; Kanický, V.; Breiter, Karel; Vaculovič, T.

    2011-01-01

    Roč. 75, č. 3 (2011), s. 894-894 ISSN 0026-461X. [Goldschmidt Conference. 14.08.2011-19.08.2011, Prague] R&D Projects: GA ČR GAP210/10/1309 Institutional research plan: CEZ:AV0Z30130516 Keywords : granite * galium * germanicum * trace elements * LA- ICP -MS Subject RIV: DD - Geochemistry http://docserver.ingentaconnect.com/deliver/connect/minsoc/0026461x/v75n3/s7.pdf?expires=1325850744&id=66551597&titleid=895&accname=Geological+institute+ASCR+library&checksum=1BA3818E3E01A68BC628566398A6E8CA

  16. Detection and characterization of silver nanoparticles in chicken meat by asymmetric flow field flow fractionation with detection by conventional or single particle ICP-MS

    DEFF Research Database (Denmark)

    Löschner, Katrin; Navratilova, Jana; Købler, Carsten

    2013-01-01

    of the AgNPs took place during the sample preparation stage. The digestate was injected into the asymmetric flow field flow fractionation (AF(4)) -ICP-MS system, which enabled fractionation of nanoparticles from the remaining meat matrix, and resulted in one large peak in the fractograms as well as two...... smaller peaks eluting close to the void volume. The recovery of silver contained in the large AgNP peak was around 80 %. Size determination of AgNPs in the meat matrix, based on external size calibration of the AF(4) channel, was hampered by non-ideal (early elution) behavior of the AgNPs. Single particle...

  17. Application of SEC-ICP-MS for comparative analyses of metal-containing species in cancerous and healthy human thyroid samples.

    Science.gov (United States)

    Boulyga, Sergei F; Loreti, Valeria; Bettmer, Jörg; Heumann, Klaus G

    2004-09-01

    Size exclusion chromatography (SEC) was coupled on-line to inductively coupled plasma mass spectrometry (ICP-MS) for speciation study of trace metals in cancerous thyroid tissues in comparison to healthy thyroids aimed to estimation of changes in metalloprotein speciation in pathological tissue. The study showed a presence of species binding Cu, Zn, Cd and Pb in healthy thyroid tissue with a good reproducibility of chromatographic results, whereas the same species could not be detected in cancerous tissues. Thus, remarkable differences with respect to metal-binding species were revealed between healthy and pathological thyroid samples, pointing out a completely different distribution of trace metals in cancerous tissues. The metal-binding species could not be identified in the frame of this work because of a lack of appropriate standards. Nevertheless, the results obtained confirm the suitability of SEC-ICP-MS for monitoring of changes in trace metal distribution in cancerous tissue and will help to better understand the role of metal-containing species in thyroid pathology.

  18. Multielement determination of major-to-ultratrace elements in vegetable samples by ICP-MS and ICP-AES after acid digestion

    International Nuclear Information System (INIS)

    Hokura, Akiko; Oguri, Sachiko; Matsuura, Hirotaka; Haraguchi, Hiroki

    2000-01-01

    A multielement determination of major-to-ultratrace elements in vegetable samples was carried out by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Spinach samples (0.5 g) were digested with nitric acid and hydrofluoric acid in a Teflon beaker on a hot plate. The decomposed samples were dissolved in a 1 M ( = mol dm -3 ) HNO 3 solution containing internal standard elements (Ge, In, and Re, 10 ppb each), and were subjected to multielement analyses by ICP-AES and ICP-MS. As a result, about 40 elements were successfully determined over a wide concentration range from % to ppb level. Spinach samples grown in different production areas were also analyzed in order to understand the influences of the environmental conditions on growth. Among the major and minor elements, the values of the coefficient of variance (CV) for B, Mg, P, and K were < 20%, and those for Ca, Na, Al, and Mn were higher than 50%. On the other hand, the values of CV for trace and ultratrace elements were significantly high. Furthermore, the present analytical method was also applied to the determination of major-to-ultratrace elements in various vegetable samples (23 species in 11 families); the similarities and differences of the elemental distributions in vegetables were found in the experimental results. (author)

  19. Isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS) for the certification of lead and cadmium in environmental standard reference materials.

    Science.gov (United States)

    Murphy, K E; Beary, E S; Rearick, M S; Vocke, R D

    2000-10-01

    Lead (Pb) and cadmium (Cd) have been determined in six new environmental standard reference materials (SRMs) using isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS). The SRMs are the following: SRM 1944, New York-New Jersey Waterway Sediment, SRMs 2583 and 2584, Trace Elements in Indoor Dust, Nominal 90 mg/kg and 10,000 mg/kg Lead, respectively, SRMs 2586 and 2587, Trace Elements in Soil Containing Lead from Paint, Nominal 500 mg/kg and 3,000 mg/kg Lead, respectively, and SRM 2782, Industrial Sludge. The capabilities of ID ICP-MS for the certification of Pb and Cd in these materials are assessed. Sample preparation and ratio measurement uncertainties have been evaluated. Reproducibility and accuracy of the established procedures are demonstrated by determination of gravimetrically prepared primary standard solutions and by comparison with isotope dilution thermal ionization mass spectrometry (ID TIMS). Material heterogeneity was readily demonstrated to be the dominant source of uncertainty in the certified values.

  20. A fast and feasible method for Br and I determination in whole egg powder and its fractions by ICP-MS.

    Science.gov (United States)

    Toralles, Isis Gonçalves; Coelho, Gilberto Silva; Costa, Vanize Cadeira; Cruz, Sandra Meinen; Flores, Erico Marlon Moraes; Mesko, Marcia Foster

    2017-04-15

    A method for Br and I determination in whole egg powder and its fractions (egg white and yolk) was developed by combining microwave-induced combustion (MIC) and inductively coupled plasma mass spectrometry (ICP-MS). Using the MIC method, 350mg of whole egg powder and its fractions were efficiently digested using 50mmolL -1 NH 4 OH as an absorbing solution. The limits of detection for Br and I using the MIC method followed by ICP-MS determination were 0.039 and 0.015μgg -1 , respectively. Using the proposed method, agreements with the reference values between 97 and 104% for Br and I were obtained by analysis of reference material NIST 8435. Finally, it was possible to observe that Br concentration (4.59-5.29μgg -1 ) was higher than I (0.150-2.28μgg -1 ) for all the evaluated samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  1. Method validation for determination of metals in Vitis labrusca L. grapevine leaf extracts by inductively coupled plasma mass spectrometry (ICP-MS

    Directory of Open Access Journals (Sweden)

    LIANE V.V. BOKOWSKI

    Full Text Available ABSTRACT Vitis labrusca L. is the main species used for wine and juice production in Brazil. The grapevine leaves can be used both as functional foods and as cheapest sources for the extraction of phenolic compounds. Besides the antioxidant activity, grapevine leaves exhibited significant anti-inflammatory activity. Therefore, the aim of this study was to develop and validate an analytical methodology to determine the metals selenium (96Se, chromium (53Cr, nickel (62Ni, cadmium (111Cd and lead (206Pb in 30 samples of grapevine leaf extracts (Vitis labrusca, Bordo cultivar using inductively coupled plasma mass spectrometry (ICP-MS. To obtain the grapevine leaf extracts the samples were milled, weighed and digested in microwave oven with nitric acid. The method showed linearity, precision, accuracy and limits of quantification and detection acceptable for INMETRO protocol validation of analytical methods. Therefore, the method using ICP-MS was developed and validated to determine metals concentrations in grapevine leaves of Vitis labrusca L. and the proposed method could be applied in routine analytical laboratory.

  2. Determination of lanthanum and rare earth elements in bovine whole blood reference material by ICP-MS after coprecipitation preconcentration with heme-iron as coprecipitant

    International Nuclear Information System (INIS)

    Fujimori, Eiji; Hayashi, Tatsuya; Inagaki, Kazumi; Haraguchi, H.

    1999-01-01

    An analytical method for the determination of lanthanide elements in the bovine whole blood reference material (IAEA A-13) has been investigated by inductively coupled plasma mass spectrometry (ICP-MS). The bovine whole blood reference material was digested with HNO 3 and HClO 4 , and then the pH of the digested solution was adjusted to 12 with 3 M sodium hydroxide aqueous solution. In this experimental procedure, lanthanide elements in the blood sample were coprecipitated with iron mainly derived from heme-iron in blood itself. In order to minimize matrix effects due to iron, excess iron in the analysis solution was removed by solvent extraction using methyl isobutyl ketone (MIBK) prior to the determination of lanthanide elements by ICP-MS. The recoveries of all lanthanide elements were almost quantitative in the recovery test. In consequence, it has been found that all lanthanide elements in bovine whole blood reference material are at the wide concentration range of 0.90 pg/g for Tm ∝1880 pg/g for Ce. (orig.)

  3. Study of composition and provenance of ancient Mamluk-Ayyubid potteries in Jordan using ICP-MS and synchrotron radiation XRF techniques

    International Nuclear Information System (INIS)

    Aldrabee, A.; Wriekat, A.; Abusaleem, K.; Radtke, M.

    2012-12-01

    Multielement analysis of thirty two Ayubid-Mamluk glazed pottery shards were analyzed for determining chemical composition in order to study their provenance. The shards lasted in the present research come from the historical site of Khirbt Far is on the Karat plateau in Jordan. The chemical analysis for sixteen samples was carried out by inductively coupled plasma mass spectroscopy (ICP-MS) and by synchrotron radiation x-rays fluorescence spectrometry (SR-X RF) for all samples. The quantitative analysis for elements Mg, Al, Ti, V, Cr, Mn, Ni, Cu, Mo, Bi, and U has been determined by ICP-MS and the semi-quantitative analysis for the elements Fe, Cu, Zu, Br, Rb, Sr, Y, Zr, Nb, Mo, Pd, Ag, Cd, and Pd has been conducted for all samples by SR-X RF. The data were analyzed by using principal component analysis PCA and hierarchical cluster analysis with Bray-Curtis in order to define grouping of different glazed pottery by obtain information about their similarity and clustering. The results of chemical analysis provided persuasive evidence that the Khirbet faribet Faris pottery shards have at least three different sources of provenance. (Author)

  4. Synthesis of novel chitosan resin derivatized with serine moiety for the column collection/concentration of uranium and the determination of uranium by ICP-MS

    International Nuclear Information System (INIS)

    Oshita, Koji; Oshima, Mitsuko; Gao Yunhua; Lee, Kyue-Hyung; Motomizu, Shoji

    2003-01-01

    A chitosan resin derivatized with serine moiety (serine-type chitosan) was newly developed by using the cross-linked chitosan as a base material. The adsorption behavior of trace amounts of metal ions on the serine-type chitosan resin was systematically examined by packing it in a mini-column, passing a metal solution through it and measuring metal ions in the effluent by ICP-MS. The resin could adsorb a number of metal cations at pH from neutral to alkaline region, and several oxoanionic metals at acidic pH region by an anion exchange mechanism. Uranium and Cu could be adsorbed selectively at pH from acidic to alkaline region by a chelating mechanism; U could be adsorbed quantitatively even at pH 3-4. Uranium adsorbed on the resin was easily eluted with 1 M nitric acid: the preconcentration (5-, 10-, 50- and 100-fold) of U was possible. The column treatment method was used prior to the ICP-MS measurement of U in natural river, sea and tap waters; R.S.D. were 2.63, 1.13 and 1.37%, respectively. Uranium in tap water could be determined by 10-fold preconcentration: analytical result was 1.46±0.02 ppt. The resin also was applied to the recovery of U in sea water: the recovery tests for artificial and natural sea water were 97.1 and 93.0%, respectively

  5. Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives

    DEFF Research Database (Denmark)

    Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente

    2006-01-01

    Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material, t...... analysis of bromine-containing preservatives in commercially available cosmetic products.......Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material...... at an intermediate and at a high linear velocity. The precision was better than 2.2% R.S.D. and regression analysis showed that a linear response was achieved at both flow rates (R2 > 0.9993, n = 36). The analysis time was less than 4.5 min at a flow rate of 50 microL min(-1) and limits of detection...

  6. Multielement determination of major-to-ultratrace elements in vegetable samples by ICP-MS and ICP-AES after acid digestion

    Energy Technology Data Exchange (ETDEWEB)

    Hokura, Akiko; Oguri, Sachiko; Matsuura, Hirotaka; Haraguchi, Hiroki [Dept. of Applied Chemistry, Graduate School of Engineering, Nagoya Univ. (Japan)

    2000-06-01

    A multielement determination of major-to-ultratrace elements in vegetable samples was carried out by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Spinach samples (0.5 g) were digested with nitric acid and hydrofluoric acid in a Teflon beaker on a hot plate. The decomposed samples were dissolved in a 1 M ( = mol dm{sup -3}) HNO{sub 3} solution containing internal standard elements (Ge, In, and Re, 10 ppb each), and were subjected to multielement analyses by ICP-AES and ICP-MS. As a result, about 40 elements were successfully determined over a wide concentration range from % to ppb level. Spinach samples grown in different production areas were also analyzed in order to understand the influences of the environmental conditions on growth. Among the major and minor elements, the values of the coefficient of variance (CV) for B, Mg, P, and K were < 20%, and those for Ca, Na, Al, and Mn were higher than 50%. On the other hand, the values of CV for trace and ultratrace elements were significantly high. Furthermore, the present analytical method was also applied to the determination of major-to-ultratrace elements in various vegetable samples (23 species in 11 families); the similarities and differences of the elemental distributions in vegetables were found in the experimental results. (author)

  7. Comparison of MP AES and ICP-MS for analysis of principal and selected trace elements in nitric acid digests of sunflower (Helianthus annuus).

    Science.gov (United States)

    Karlsson, Stefan; Sjöberg, Viktor; Ogar, Anna

    2015-04-01

    The use of nitrogen as plasma gas for microwave plasma atomic emission spectroscopy (MP AES) is an interesting development in analytical science since the running cost can be significantly reduced in comparison to the inductively coupled argon plasma. Here, we evaluate the performance of the Agilent 4100 MP AES instrument for the analysis of principal metals (Ca, K, Mg, and Na), lithogenic metals (Al, Fe, and Mn) and selected trace metals (As, Ba, Cd, Co, Cr, Cu, Mo, Ni, Pb, V, and Zn) in nitric acid plant digests. The digests were prepared by microwave-assisted dissolution of dry plant material from sunflower (Helianthus annuus) in concentrated nitric acid. Comparisons are made with analysis of the same solutions with ICP-MS (Agilent 7500cx) using the octopole reaction system (ORS) in the collision mode for As, Fe, and V. The limits of detection were usually in the low µg L(-1) range and all principal and lithogenic metals were successfully determined with the MP AES and provided almost identical results with the ICP-MS. The same applies for the selected trace metals except for As, Co and Mo where the concentrations were below the detection limit with the MP AES. For successful analysis we recommend that (i) only atom lines are used, (ii) ionization is minimized (e.g. addition of CsNO3) and (iii) the use of internal standards should be considered to resolve spectral interferences. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Ion-pair chromatography coupled to inductively coupled plasma-mass spectrometry (IPC-ICP-MS) as a method for thiomolybdate speciation in natural waters.

    Science.gov (United States)

    Lohmayer, Regina; Reithmaier, Gloria Maria Susanne; Bura-Nakić, Elvira; Planer-Friedrich, Britta

    2015-03-17

    Molybdenum precipitates preferentially under reducing conditions; therefore, its occurrence in sediment records is used as an indicator of paleoredox conditions. Although thiomolybdates (MoO4-xSx(2-) with x = 1-4) supposedly are necessary intermediates in the process of molybdenum precipitation under anoxic conditions, there is no information about their abundance in natural environments, because of a lack of element-specific methods with sufficiently low detection limits. Here, we optimized ion-pair chromatographic separation for coupling to an inductively coupled plasma-mass spectrometry detector (IPC-ICP-MS). 2-Propanol (10%-25% gradient) replaced the previously used acetonitrile (25%-75%) as the solvent, to reduce the carbon load into the plasma. In synthetic solutions, formation of thiomolybdates was found to occur spontaneously in the presence of excess sulfide and the degree of thiolation was highest at pH 7. Excess hydroxyl led to a transformation of thiomolybdates to molybdate. Under acidic to neutral conditions, precipitation of molybdenum and hydrolysis of tetrathiomolybdate were observed. Flash-freezing was found to be suitable to stabilize tetrathiomolybdate, with 2 mM) negatively affected the detection of molybdate, which eluted mainly in the dead volume, but had no negative effect on higher thiolated molybdates. Detection limits were ∼10 nM. With the newly developed IPC-ICP-MS method, thiomolybdates were found to form spontaneously in euxinic marine waters after adding a molybdate spike and occur naturally in sulfidic geothermal waters.

  9. Laser ablation - inductive coupled plasma - mass spectrometer (LA-ICP-MS) geochemistry characterization of albitites associated to uranium in Lagoa da Rabicha deposit, Lagoa Real, BA (Brazil)

    International Nuclear Information System (INIS)

    Oliveira, Lucilia A. Ramos de; Rios, Francisco Javier; Amorim, Lucas Eustaquio Dias; Souza, Aurelio da Silva; Prates, Sonia Pinto; Yardley, Bruce; Matos, Evando Carele

    2009-01-01

    The LA-ICP-MS technique is a good tool for mineral geochemical characterization. The technique has high spatial resolution, elevated sensibility, low detection limits and multi-elementary analysis possibility. Almost all chemistry elements can be analyzed by this methodology. Briefly, this methodology consists in vaporize the sample by Laser Ablation, which is dragged by argon into the Plasma where are created and accelerated the ions. They are separated by their mass/charge ratio into the Mass Spectrometer, being conveyed to a detector that convert the signals in specters. In this work LA-ICP-MS analyses were performed in two albitites thin sections, a mineralized and a non mineralized sample. Both samples are from the Lagoa da Rabicha Deposit, Uranium Lagoa Real Province, BA. From these analysis it was possible to chemically characterize the minerals present in the samples and better understand the trace elements on them. The results for plagioclase in both samples show that it is albite (NaAlSi 3 O 8 ). The albite from sample 200907-20 shows traces of strontium, lanthanum, cerium, neodymium, samarium and thorium in one crystal. The albite from sample 200907-23 has strontium with uranium, yttrium and lead in smaller quantities. The results obtained in this work are very important and contribute to a better understanding of the uranium origin in Lagoa Real deposits. (author)

  10. LA-ICP-MS Pb-U Dating of Young Zircons from the Kos-Nisyros Volcanic Centre, SE Aegean Arc (Greece)

    Science.gov (United States)

    Guillong, M.; Von Quadt, A.; Peytcheva, I.; Bachmann, O.

    2014-12-01

    Zircon Pb-U dating has become a key technique for answering many important questions in geosciences. This paper describes a new LA-ICP-MS approach. We show, using previously dated samples of a large quaternary rhyolitic eruption in the Kos-Nisyros volcanic centre (the 161 ka Kos Plateau Tuff), that the precision of our LA-ICP-MS method is as good as via SHRIMP, while ID-TIMS measurements confirm the accuracy. Gradational age distribution over >140 ka of the Kos zircons and the near-absence of inherited cores indicate near-continuous crystallisation in a growing magma reservoir with little input from wall rocks. Previously undated silicic eruptions from Nisyros volcano (Lower Pumice, Nikia Flow, Upper Pumice), which are stratigraphically constrained to have happened after the Kos Plateau Tuff, are dated to be younger than respectively 124 ± 35 ka, 111 ± 42 ka and 70 ± 24 ka. Samples younger than 1 Ma were corrected for initial thorium disequilibrium using a new formula that also accounts for disequilibrium in 230Th decay. Guillong, M. et al., 2014, JAAS, 29, p. 963-967; doi: 10.1039/c4ja00009a.

  11. Automation of sample processing for ICP-MS determination of 90Sr radionuclide at ppq level for nuclear technology and environmental purposes.

    Science.gov (United States)

    Kołacińska, Kamila; Chajduk, Ewelina; Dudek, Jakub; Samczyński, Zbigniew; Łokas, Edyta; Bojanowska-Czajka, Anna; Trojanowicz, Marek

    2017-07-01

    90 Sr is a widely determined radionuclide for environmental purposes, nuclear waste control, and can be also monitored in coolants in nuclear reactor plants. In the developed method, the ICP-MS detection was employed together with sample processing in sequential injection analysis (SIA) setup, equipped with a lab-on-valve with mechanized renewal of sorbent bed for solid-phase extraction. The optimized conditions of determination included preconcentration of 90 Sr on cation-exchange column and removal of different type of interferences using extraction Sr-resin. The limit of detection of the developed procedure depends essentially on the configuration of the employed ICP-MS spectrometer and on the available volume of the sample to be analyzed. For 1L initial sample volume, the method detection limit (MDL) value was evaluated as 2.9ppq (14.5BqL -1 ). The developed method was applied to analyze spiked river water samples, water reference materials, and also simulated and real samples of the nuclear reactor coolant. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Trace Element Determination and Cardioprotection of Terminalia pallida Fruit Ethanolic Extract in Isoproterenol Induced Myocardial Infarcted Rats by ICP-MS.

    Science.gov (United States)

    Althaf Hussain, Shaik; Kareem, Mohammed Abdul; Rasool, Shaik Nayab; Al Omar, Suliman Yousef; Saleh, Alwasel; Al-Fwuaires, Manal Abdulrahman; Daddam, Jayasimha Rayalu; Devi, Kodidhela Lakshmi

    2018-01-01

    The trace elements and minerals in Terminalia pallida fruit ethanolic extract (TpFE) were determined by the instrument inductively coupled plasma-mass spectrometry (ICP-MS), and the cardioprotection of TpFE against isoproterenol (ISO)-administered rats was studied. Rats were pretreated with TpFE (100, 300, and 500 mg/kg bw) for 30 days, with concurrent administration of ISO (85 mg/kg bw) for two consecutive days. The levels of trace elements and minerals in TpFE were below the permitted limits of World Health Organization standards. ISO administration significantly increased the heart weight and cardiac marker enzymes in serum, xanthine oxidase, sodium, and calcium in the heart, whereas significantly decreased body weight, reduced glutathione, glutathione-S-transferase, superoxide dismutase, and potassium in the heart. Oral pretreatment of TpFE significantly prevented the ISO-induced alterations. This is the first report that revealed the determination of trace elements and mineral nutrients of TpFE by ICP-MS which plays a principal role in the herbal drug discovery for the treatment of cardiovascular diseases.

  13. The impact of whole human blood on the kinetic inertness of platinum(iv) prodrugs - an HPLC-ICP-MS study.

    Science.gov (United States)

    Theiner, Sarah; Grabarics, Márkó; Galvez, Luis; Varbanov, Hristo P; Sommerfeld, Nadine S; Galanski, Markus; Keppler, Bernhard K; Koellensperger, Gunda

    2018-04-17

    The potential advantage of platinum(iv) complexes as alternatives to classical platinum(ii)-based drugs relies on their kinetic stability in the body before reaching the tumor site and on their activation by reduction inside cancer cells. In this study, an analytical workflow has been developed to investigate the reductive biotransformation and kinetic inertness of platinum(iv) prodrugs comprising different ligand coordination spheres (respectively, lipophilicity and redox behavior) in whole human blood. The distribution of platinum(iv) complexes in blood pellets and plasma was determined by inductively coupled plasma-mass spectrometry (ICP-MS) after microwave digestion. An analytical approach based on reversed-phase (RP)-ICP-MS was used to monitor the parent compound and the formation of metabolites using two different extraction procedures. The ligand coordination sphere of the platinum(iv) complexes had a significant impact on their accumulation in red blood cells and on their degree of kinetic inertness in whole human blood. The most lipophilic platinum(iv) compound featuring equatorial chlorido ligands showed a pronounced penetration into blood cells and a rapid reductive biotransformation. In contrast, the more hydrophilic platinum(iv) complexes with a carboplatin- and oxaliplatin-core exerted kinetic inertness on a pharmacologically relevant time scale with notable amounts of the compound accumulated in the plasma fraction.

  14. Application of CE-ICP-MS and CE-ESI-MS/MS for identification of Zn-binding ligands in Goji berries extracts.

    Science.gov (United States)

    Ruzik, Lena; Kwiatkowski, Piotr

    2018-06-01

    The identification of groups of ligands binding metals is a crucial issue for the better understanding of their bioaccessibility. In the current study, we have intended an approach for identification of Zn-binding ligands based on using capillary electrophoresis combined with inductively coupled plasma mass spectrometry (CE-ICP-MS) and tandem electrospray ionization mass spectrometry (CE-ESI-MS/MS). The approach, which featured the use of the coupling of capillary electrophoresis with inductively coupled plasma mass spectrometry allows to separate and observe zinc ions present in complexes with respect to their size and charge and to identify nine compounds with zinc isotopic profile. CE-ICP-MS provides us with information about presence of zinc species and elemental information about zinc distribution. CE-ESI-MS/MS provide us with information about the most favorable Zn binding ligands: amino acids, flavonols, stilbenoids, fenolic acids and carotenoids. The presented work is the continuation of previous studies based on using LC-ESI-MS/MS, though, now we presented a new solutions with the possibility of changing detectors without changing the separation techniques, what is important without re-optimizing the method. The new presented method allows to identify the zinc-binding ligands in shorter time. Copyright © 2018 Elsevier B.V. All rights reserved.

  15. Gold nanoparticle labeling with tyramide signal amplification for highly sensitive detection of alpha fetoprotein in human serum by ICP-MS.

    Science.gov (United States)

    Li, Xiaoting; Chen, Beibei; He, Man; Xiao, Guangyang; Hu, Bin

    2018-01-01

    In this work, we developed an immunoassay based on tyramide signal amplification (TSA) and gold nanoparticles (Au NPs) labeling for highly sensitive detection of alpha fetoprotein (AFP) by inductively coupled plasma mass spectrometry (ICP-MS). AFP was captured by anti-AFP1 coating on the 96-well plate and labeled by anti-AFP2-horseradish peroxidase (HRP), in which the HRP can catalyze the deposition of biotinylated tyramine on the nearby protein. Then the streptavidin (SA)-Au NPs was labeled on the deposited biotinylated tyramine as the intensive signal probe for ICP-MS measurement. Under the optimal experimental conditions, the limit of detection of the developed method for AFP was 1.85pg/mL and the linear range was 0.005-2ng/mL. The relative standard deviation for seven replicate detections of 0.01ng/mL AFP was 5.2%. The proposed method was successfully applied to the detection of AFP in human serum with good recoveries. This strategy is highly sensitive and easy to operate, and can be extended to the sensitive detection of other biomolecules in human serum. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Speciation of the oxidation states of plutonium in aqueous solutions by UV/Vis spectroscopy, CE-ICP-MS and CE-RIMS

    International Nuclear Information System (INIS)

    Buerger, S.; Banik, N.L.; Buda, R.A.; Kratz, J.V.; Kuczewski, B.; Trautmann, N.

    2007-01-01

    For the speciation of the plutonium oxidation states in aqueous solutions, the online coupling of capillary electrophoresis (CE) with inductively coupled plasma mass spectrometry (ICP-MS) has been developed. Depending on the radius/electrical charge ratio, the oxidation states III, IV, V, and VI of plutonium are separated by CE, based on the different migration times through the capillary and are detected by ICP-MS. The detection limit is 20 ppb, i.e. 10 9 -10 10 atoms (10 -12 -10 -13 g) for one oxidation state with an uncertainty of the reproducibility of the migration times of ≤ 1% and ≤ 5% for the peak area. The redox kinetics of the different plutonium oxidation states in the presence of humic substances (humic and fulvic acid) have been studied. A relatively rapid reduction of Pu(VI) (10 to 1000 h) in contact with Gorleben fulvic or Aldrich humic acid could be observed, depending on the pH of the solution. Furthermore, at pH=1, a reduction to Pu(III) and Pu(IV) in a mixture of all four oxidation states in contact with Gorleben fulvic acid after one month has been observed. In order to improve the sensitivity of the CE method, the offline coupling of CE to resonance ionization mass spectrometry (RIMS) has been explored. First applications of this new speciation method are presented. (orig.)

  17. Multielement determination of major-to-ultratrace elements in deep-seawater salts by ICP-AES and ICP-MS

    International Nuclear Information System (INIS)

    Sakai, Takeshi; Nakagawa, Koji; Nakajima, Hiroshi; Itoh, Akihide; Ji, Shan; Haraguchi, Hiroki

    2002-01-01

    Major-to-ultratrace elements in deep-seawater salts were determined by ICP-AES and ICP-MS, after they were separated into the water-soluble, acid-soluble, and insoluble particle components. Deep-seawater salts were prepared from seawater collected at 344 m deep near the off-shore of Cape Muroto in Kochi Prefecture. The major and minor elements in salts were determined by ICP-AES after appropriate dilution with pure water. Trace and ultratrace elements in the water-soluble and acid-soluble components were preconcentrated by a chelating resin preconcentration method. In addition, the major to-ultratrace elements in the insoluble particle component were determined by ICP-AES and ICP-MS, after acid-digestion using HNO 3 /HF/HClO 4 . As a result, 21-35 elements in deep-seawater salts could be determined over the wide concentration range. It was found that the elements, such as Al, V, Fe, Mn, Co, Cu, Zn, and rare earth elements, were more abundant in the acid-soluble component of deep-seawater salts, which may play some essential roles in physiological effectiveness for intake of salt. (author)

  18. Multielement analytical procedure coupling INAA, ICP-MS and ICP-AES: Application to the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco)

    International Nuclear Information System (INIS)

    Bounouira, H.; CEA - CNRS/UMR, Centre de Saclay, 91 - Gif sur Yvette; Choukri, A.; Hakam, O.K.; Cherkaoui, R.; Gaudry, A.; Delmas, R.; Mariet, C.; Chakiri, S.

    2008-01-01

    Instrumental neutron activation analysis (INAA), inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) were used for the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco). The reliability of the results was checked, by using IAEA Soil-7 certified reference material. Results obtained by the three techniques were compared to control digestions efficiencies. A general good agreement was found between INAA and both ICP-MS and ICP-AES after alkaline fusion (ICPf). The ICP-MS technique used after acid attack (ICPa) was satisfactory for a few elements. A principal component analysis (PCA) has been used for analyzing the variability of concentrations, and defining the most influential sites with respect to the general variation trends. Three groups of elements could be distinguished. For these groups a normalization of concentrations to the central element concentration (that means Mn, Si or Al) is proposed. (author)

  19. Determining the isotopic compositions of uranium and fission products in radioactive environmental microsamples using laser ablation ICP-MS with multiple ion counters

    International Nuclear Information System (INIS)

    Boulyga, Sergei F.; Prohaska, Thomas

    2008-01-01

    This paper presents the application of a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS) - a Nu Plasma HR - equipped with three ion-counting multipliers and coupled to a laser ablation system (LA) for the rapid and sensitive determination of the 235 U/ 238 U, 236 U/ 238 U, 145 Nd/ 143 Nd, 146 Nd/ 143 Nd, 101 Ru/( 99 Ru+ 99 Tc) and 102 Ru/( 99 Ru+ 99 Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred μm to about 1 mm and with surface alpha activities of 3-38 mBq were first identified using nuclear track radiography. U, Nd and Ru isotope systems were then measured sequentially for the same microsample by LA-MC-ICP-MS. The application of a zoom ion optic for aligning the ion beams into the ion counters allows fast switching between different isotope systems, which enables all of the abovementioned isotope ratios to be measured for the same microsample within a total analysis time of 15-20 min (excluding MC-ICP-MS optimization and calibration). The 101 Ru/( 99 Ru+ 99 Tc) and 102 Ru/( 99 Ru+ 99 Tc) isotope ratios were measured for four microsamples and were found to be significantly lower than the natural ratios, indicating that the microsamples were contaminated with the corresponding fission products (Ru and Tc). A slight depletion in 146 Nd of about 3-5% was observed in the contaminated samples, but the Nd isotopic ratios measured in the contaminated samples coincided with natural isotopic composition within the measurement uncertainty, as most of the Nd in the analyzed samples originates from the natural soil load of this element. The 235 U/ 238 U and 236 U/ 238 U isotope ratios were the most sensitive indicators of irradiated uranium. The present work yielded a significant variation in uranium isotope ratios in microsamples, in contrast with previously published results from the bulk analysis of contaminated samples originating from the vicinity of Chernobyl. Thus

  20. Determining the isotopic compositions of uranium and fission products in radioactive environmental microsamples using laser ablation ICP-MS with multiple ion counters.

    Science.gov (United States)

    Boulyga, Sergei F; Prohaska, Thomas

    2008-01-01

    This paper presents the application of a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS)--a Nu Plasma HR--equipped with three ion-counting multipliers and coupled to a laser ablation system (LA) for the rapid and sensitive determination of the 235U/238U, 236U/238U, 145Nd/143Nd, 146Nd/143Nd, 101Ru/(99Ru+99Tc) and 102Ru/(99Ru+99Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred mum to about 1 mm and with surface alpha activities of 3-38 mBq were first identified using nuclear track radiography. U, Nd and Ru isotope systems were then measured sequentially for the same microsample by LA-MC-ICP-MS. The application of a zoom ion optic for aligning the ion beams into the ion counters allows fast switching between different isotope systems, which enables all of the abovementioned isotope ratios to be measured for the same microsample within a total analysis time of 15-20 min (excluding MC-ICP-MS optimization and calibration). The 101Ru/(99Ru+99Tc) and 102Ru/(99Ru+99Tc) isotope ratios were measured for four microsamples and were found to be significantly lower than the natural ratios, indicating that the microsamples were contaminated with the corresponding fission products (Ru and Tc). A slight depletion in 146Nd of about 3-5% was observed in the contaminated samples, but the Nd isotopic ratios measured in the contaminated samples coincided with natural isotopic composition within the measurement uncertainty, as most of the Nd in the analyzed samples originates from the natural soil load of this element. The 235U/238U and 236U/238U isotope ratios were the most sensitive indicators of irradiated uranium. The present work yielded a significant variation in uranium isotope ratios in microsamples, in contrast with previously published results from the bulk analysis of contaminated samples originating from the vicinity of Chernobyl. Thus, the 235U/238U ratios measured in ten

  1. Establishment of methodology for determination of 93Zr in radioactive wastes by Liquid Scintillation Counting (LSC) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Oliveira, Thiago Cesar de

    2014-01-01

    The zirconium-93 is a long-lived pure β-particle-emitting radionuclide produced from 235 U fission and from neutron activation of the stable isotope 92 Zr and thus occurring as one of the radionuclides found in nuclear reactors. Due to its long half life, 93 Zr is one of the radionuclides of interest for the performance of assessment studies of waste storage or disposal. Measurement of 93 Zr is difficult owing to its trace level concentration and its low activity in nuclear wastes and further because its certified standards are not frequently available. The aim of this work was to develop a selective radiochemical separation methodology for the determination of 93 Zr in nuclear waste and analyze it by Liquid Scintillation Counting (LSC) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). To set up the radiochemical separation procedure for zirconium, a tracer solution of 95 Zr and its 724 keV γ-ray measurements by γ- spectrometry were used in order to follow the behavior of zirconium during the radiochemical separation. For the LSC technique a 55 Fe solution, which is one of the major interfering measures zirconium, was used to verify the decontamination factor during the separation process. The efficiency detection for 63 Ni was used to determination of 93 Zr activity in the matrices analyzed. The limit of detection of the 0.05 Bq 1 −1 was obtained for 63 Ni standard solutions by using a sample:cocktail ratio of 3:17 mL for Optiphase Hisafe 3 cocktail. For the ICP-MS technique a zirconium stable solution was used to verify the zirconium behavior and recovery during radiochemical separation and a solution of Ba, Co, Eu, Fe, Mn, Nb, Sr and Y was used to verify the decontamination factor during the separation process. A standard solution 93 Nb as isotope for determining the 93 Zr by ICP-MS was used for calibration and analysis. The detection limit of 0.039 ppb was obtained for the standard solution of zirconium. Then, the protocol was applied to low level

  2. Quantification of plasmid DNA reference materials for Shiga toxin-producing Escherichia coli based on UV, HR-ICP-MS and digital PCR.

    Science.gov (United States)

    Liang, Wen; Xu, Li; Sui, Zhiwei; Li, Yan; Li, Lanying; Wen, Yanli; Li, Chunhua; Ren, Shuzhen; Liu, Gang

    2016-01-01

    The accuracy and metrology traceability of DNA quantification is becoming a critical theme in many fields, including diagnosis, forensic analysis, microorganism detection etc. Thus the research of DNA reference materials (RMs) and consistency of DNA quantification methods has attracted considerable research interest. In this work, we developed 3 plasmid candidate RMs, containing 3 target genes of Escherichia coli O157:H7 (E. coli O157:H7) and other Shiga toxin-producing Escherichia coli (STEC): stx1, stx2, and fliC (h7) respectively. Comprehensive investigation of the plasmid RMs was performed for their sequence, purity, homogeneity and stability, and then the concentration was quantified by three different methods: ultraviolet spectrophotometer (UV), high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) and digital PCR. As a routinely applied method for DNA analysis, UV was utilized for the quantification (OD260) and purity analysis for the plasmids. HR-ICP-MS quantified the plasmid DNA through analysing the phosphorus in DNA molecules. Digital PCR distributed the DNA samples onto a microarray chip containing thousands of reaction chambers, and quantified the DNA copy numbers by analysing the number of positive signals without any calibration curves needed. Based on the high purification of the DNA reference materials and the optimization of dPCR analysis, we successfully achieved good consistency between UV, HR-ICP-MS and dPCR, with relative deviations lower than 10 %. We then performed the co-quantification of 3 DNA RMs with three different methods together, and the uncertainties of their concentration were evaluated. Finally, the certified values and expanded uncertainties for 3 DNA RMs (pFliC, pStx1 and pStx2) were (1.60 ± 0.10) × 10(10) copies/μL, (1.53 ± 0.10) × 10(10) copies/μL and (1.70 ± 0.11) × 10(10) copies/μL respectively.Graphical abstractWe developed 3 plasmid candidate RMs, containing 3 target genes of

  3. Direct lead isotope analysis in Hg-rich sulfides by LA-MC-ICP-MS with a gas exchange device and matrix-matched calibration

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Wen [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China); Hu, Zhaochu, E-mail: zchu@vip.sina.com [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China); Günther, Detlef, E-mail: guenther@inorg.chem.ethz.ch [ETH Zurich, Laboratory for Inorganic Chemistry, CH-8093, Zurich (Switzerland); Liu, Yongsheng; Ling, Wenli; Zong, Keqing; Chen, Haihong; Gao, Shan [State Key Laboratory of Geological Processes and Mineral Resources, Faculty of Earth Sciences, China University of Geosciences, Wuhan, 430074 (China)

    2016-12-15

    In situ Pb isotope data of sulfide samples measured by LA-MC-ICP-MS provide valuable geochemical information for studies of the origin and evolution of ore deposits. However, the severe isobaric interference of {sup 204}Hg on {sup 204}Pb and the lack of matrix-matched sulfide reference materials limit the precision of Pb isotopic analyses for Hg-rich sulfides. In this study, we observe that Hg forms vapor and can be completely removed from sample aerosol particles produced by laser ablation using a gas exchange device. Additionally, this device does not influence the signal intensities of Pb isotopes. The within-run precision, the external reproducibility and the analytical accuracy are significantly improved for the Hg-rich sulfide samples using this mercury-vapor-removing device. Matrix effects are observed when using silicate glass reference materials as the external standards to assess the relationship of mass fractionation factors between Tl and Pb in sulfide samples, resulting in a maximum deviation of ∼0.20% for {sup 20x}Pb/{sup 204}Pb. Matrix-matched reference materials are therefore required for the highly precise and accurate Pb isotope analyses of sulfide samples. We investigated two sulfide samples, MASS-1 (the Unites States Geological Survey reference materials) and Sph-HYLM (a natural sphalerite), as potential candidates. Repeated analyses of the two proposed sulfide reference materials by LA-MC-ICP-MS yield good external reproducibility of <0.04% (RSD, k = 2) for {sup 20x}Pb/{sup 206}Pb and <0.06% (RSD, k = 2) for {sup 20x}Pb/{sup 204}Pb with the exception of {sup 20x}Pb/{sup 204}Pb in MASS-1, which provided an external reproducibility of 0.24% (RSD, k = 2). Because the concentration of Pb in MASS-1 (76 μg g{sup −1}) is ∼5.2 times lower than that in Sph-HYLM (394 ± 264 μg g{sup −1}). The in situ analytical results of MASS-1 and Sph-HYLM are consistent with the values obtained by solution MC-ICP-MS, demonstrating the reliability

  4. Operationally defined species characterization and bioaccessibility evaluation of cobalt, copper and selenium in Cape gooseberry (Physalis Peruviana L.) by SEC-ICP MS.

    Science.gov (United States)

    Wojcieszek, Justyna; Ruzik, Lena

    2016-03-01

    Physalis peruviana could attract great interest because of its nutritional and industrial properties. It is an excellent source of vitamins, minerals, essential fatty acids and carotenoids. Physalis Peruviana is also known to have a positive impact on human health. Unfortunately, still little is known about trace elements present in Physalis Peruviana and their forms available for the human body. Thus, the aim of this study was to estimate bioaccessibility and characterization of species of cobalt, copper and selenium in Physalis Peruviana fruits. Total and extractable contents of elements were determined by mass spectrometer with inductively coupled plasma (ICP MS). In order to separate the different types of metal complexes Physalis peruviana fruits were treated with the following solvents: Tris-HCl (pH 7.4), sodium dodecyl sulfate (SDS) (pH 7.4) and ammonium acetate (pH 5.5). The best efficiency of extraction of: cobalt was obtained for ammonium acetate (56%) and Tris-HCl (60%); for copper was obtained for SDS (66%), for selenium the best extraction efficiency was obtained after extraction with SDS (48%). To obtain information about bioaccessibility of investigated elements, enzymatic extraction based on in vitro simulation of gastric (pepsin) and intestinal (pancreatin) digestion was performed. For copper and selenium the simulation of gastric digestion leads to the extraction yield above 90%, while both steps of digestion method were necessary to obtain satisfactory extraction yield in the case of cobalt. Size exclusion chromatography (SEC) coupled to on-line ICP MS detection was used to investigate collected metal species. The main fraction of metal compounds was found in the 17 kDa region. Cobalt and copper create complexes mostly with compounds extracted by means of ammonium acetate and SDS, respectively. Cobalt, copper and selenium were found to be highly bioaccessible from Physalis Peruviana. Investigation of available standards of cobalt and selenium

  5. Analysis of glass from the post-Roman settlement Tonovcov grad (Slovenia) by PIXE–PIGE and LA-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Šmit, Ž., E-mail: ziga.smit@fmf.uni-lj.si [Faculty of Mathematics and Physics, University of Ljubljana, Jadranska 19, SI-1000 Ljubljana (Slovenia); Jožef Stefan Institute, Jamova 39, SI-1001 Ljubljana (Slovenia); Milavec, T. [Department of Archaeology, Faculty of Arts, University of Ljubljana, Zavetiška 5, SI-1000 Ljubljana (Slovenia); Fajfar, H. [Jožef Stefan Institute, Jamova 39, SI-1001 Ljubljana (Slovenia); Rehren, Th. [UCL Qatar, Education City, P.O. Box 23689, Doha (Qatar); Lankton, J.W. [UCL Institute of Archaeology, 31-34 Gordon Square, London WC1H 0PY (United Kingdom); Gratuze, B. [IRAMAT-Centre Ernest-Babelon, CNRS Université d’Orléans, 3D rue de la Ferollerie, 45071 Orléans Cedex 2 (France)

    2013-09-15

    The combined PIXE–PIGE method was used for the analysis of 43 glass fragments from the archaeological site Tonovcov grad in western Slovenia, with 10 of these additionally being analysed by LA-ICP-MS. The glass objects were attributed to the Late Antique production of the 4th–7th c. AD, with two examples of early Roman glass and three glass beads, one of them presumably of oriental origin. The analysis showed typical natron-type glass, produced in the Levantine region around the river Belus, and a few examples of HIMT glass, which could be recognized also in several other recycled objects. Only one glass bead, found in Early Medieval context, was made of the ash of halophytic plants.

  6. Determination of lead by hydride generation inductively coupled plasma mass spectrometry (HG-ICP-MS): On-line generation of plumbane using potassium hexacyanomanganate(III)

    Energy Technology Data Exchange (ETDEWEB)

    Yilmaz, Vedat [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States); Erciyes University, Faculty of Pharmacy, Department of Analytical Chemistry, 38039 Kayseri (Turkey); Arslan, Zikri, E-mail: zikri.arslan@jsums.edu [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States); Rose, LaKeysha [Jackson State University, Department of Chemistry and Biochemistry, Jackson, MS 39217 (United States)

    2013-01-25

    Highlights: Black-Right-Pointing-Pointer Potassium hexacyanomanganate(III), (K{sub 3}Mn(CN){sub 6}, was utilized first time for hydride generation (HG). Black-Right-Pointing-Pointer Hexacyanomanganate(III) promoted generation of lead hydride (PbH{sub 4}) remarkably. Black-Right-Pointing-Pointer The HG method using K{sub 3}Mn(CN){sub 6} enhanced sensitivity by at least 40-fold. Black-Right-Pointing-Pointer The method detection limits for Pb were as low as 8 ng L{sup -1} by ICP-MS. Black-Right-Pointing-Pointer The method is highly suitable for quantitative determination of Pb in various samples and salt matrices by ICP-MS. - Abstract: A hydride generation (HG) procedure has been described for determination of Pb by ICP-MS using potassium hexacyanomanganate(III), K{sub 3}Mn(CN){sub 6}, as an additive to facilitate the generation of plumbane (PbH{sub 4}). Potassium hexacyanomanganate(III) was prepared in acidic medium as it was unstable in water. The stability of hexacyanomanganate(III) was examined in dilute solutions of HCl, HNO{sub 3} and H{sub 2}SO{sub 4}. The solutions prepared in 1% v/v H{sub 2}SO{sub 4} were found to be stable for over a period of 24 h. The least suitable medium was 1% v/v HNO{sub 3}. For generation of plumbane, acidic hexacyanomanganate(III) and sample solutions were mixed on-line along a 5-cm long tygon tubing (1.14 mm i.d.) and then reacted with 2% m/v sodium borohydride (NaBH{sub 4}). A concentration of 0.5% m/v K{sub 3}Mn(CN){sub 6} facilitated the generation of PbH{sub 4} remarkably. In comparison to H{sub 2}SO{sub 4}, HCl provided broader working range for which optimum concentration was 1% v/v. No significant interferences were noted from transition metals and hydride forming elements, up to 0.5 {mu}g mL{sup -1} levels, except Cu which depressed the signals severely. The depressive effects in the presence of 0.1 {mu}g mL{sup -1} Cu were alleviated by increasing the concentration of K{sub 3}Mn(CN){sub 6} to 2% m/v. Under these conditions

  7. Accurate technetium-99 determination using the combination of TEVA resin pretreatment and ICP-MS measurement and its influence on the Tc-99/Cs-137 scaling factor calculation

    International Nuclear Information System (INIS)

    Lian-Song Chen; Tsing-Hai Wang; Yi-Kong Hsieh; Li-Wei Jian; Wie-Han Chen; Chu-Fang Wang; Tsuey-Lin Tsai

    2014-01-01

    Accurate determination of technetium-99 (Tc-99) is very important because any overestimation will cause the examined radioactive wastes to be categorized into super C class, which dramatically increases the cost of waste management. Herein, we demonstrated that by adopting the analytical method comprising TEVA resin pretreatment and ICP-MS measurement, the determined Tc-99 concentrations in representative waste stream samples from the Lan-Yu low-level radioactive waste temporary storage site in Taiwan were approximately two orders of magnitude lower than those determined from the beta radiation measurement using a low background liquid scintillation counter. Two important concerns emerged from our results. First, severe interferences from other nuclides residing in the matrix considerably affect the determination of Tc-99, even when a low background liquid scintillation counter was used. Second, the currently used Tc-99/Cs-137 scaling factor should be carefully revised, or it might lead to a considerable overestimation of the Tc-99 concentration. (author)

  8. Determination of organic and inorganic mercury species in Sungai Kinta, Perak by reversed-phase high performance liquid chromatography (HPLC) on-line coupled with ICP-MS

    International Nuclear Information System (INIS)

    Norshidah Baharuddin; Norashikin Saim; Rozita Osman; Sharifuddin Mohd Zain

    2012-01-01

    This paper describes a simple method for mercury speciation in river water samples of Sungai Kinta, Perak. Separation and measurement were done by high-performance liquid chromatography on-line with inductively coupled plasma mass spectrometry (HPLC/ ICP-MS). Separation of mercury species was accomplished within 6 minutes on an AQ C18 4.6 mm i.d x 150 mm, 5 μm reversed phase column with 0.1 % (w/ v) L-cysteine as mobile phase. Under the optimum instrumental conditions, recoveries of 101-104 % for MeHg + and 96 - 104 % for Hg 2+ were obtained with experimental detection limits of 1ngL -1 for inorganic mercury and 1.5 μgL -1 for organic mercury. (author)

  9. Analysis of molybdenum, tungsten, and vanadium in surface water of the Atlantic Ocean using solid phase extraction with 8-hydroxyquinoline and ICP MS determination

    Science.gov (United States)

    Rimskaya-Korsakova, M. N.; Berezhnaya, E. D.; Dubinin, A. V.

    2017-07-01

    An analytical technique is proposed to determine ultratrace concentrations of Mo, V, and W found in seawater using mass spectrometry with inductively coupled plasma (ICP MS) after preliminary concentration by solid-phase extraction of metal complexes with 8-hydroxyquinoline (8-HQ) on C18 octadecyl silica. The technique utilizes 150 mL of a water sample. A preconcentration factor 50 is obtained. The detection limits are 0.25 nmol/kg, 0.041 nmol/kg, and 5 pmol/kg for Mo, V, and W, respectively. Dissolved Mo, V, and Wconcentrations in surface seawater from Atlantic Ocean transect were determined. The concentrations ranges along the transect were: 91-108 nmol/kg for Mo, 28-35 nmol/kg for V, and 55-75 pmol/kg for W. The Mo/W ratio varied from 1300 to 1800.

  10. Determination of trace level thorium and uranium in high purity gadolinium sulfate using ICP-MS with solid-phase chromatographic extraction resins

    Science.gov (United States)

    Ito, S.; Takaku, Y.; Ikeda, M.; Kishimoto, Y.

    2018-01-01

    The Super Kamiokand-Gadolinium (SK-Gd) project is the upgrade of the Super-Kamiokande (SK) detector in order to discover Supernova Relic Neutrinos (SRNs) by loading 0.2% of Gd2(SO4)3 into a 50 kton of the SK water tank. In order to continue solar neutrino measurement with low energy threshold at ˜3.5 MeV, main radioactive contamination, U and Th in Gd2(SO4)3, should be purified before loading. We developed solid-phase extraction technique to measure low concentration of U and Th in Gd2(SO4)3 by ICP-MS. The extraction technique and current status will be presented.

  11. Comparison of direct injection nebulizer and desolvating microconcentric nebulizer for analysis of chlorine-, bromine- and iodine-containing compounds by reversed phase HPLC with ICP-MS detection

    DEFF Research Database (Denmark)

    Jensen, B.P.; Gammelgaard, Bente; Hansen, S.H.

    2003-01-01

    the direct injection nebulizer at flow rates of 25 and 50 mul min(-1), the influence of 0-50% methanol and 0-25% acetonitrile on the sensitivity was studied. For chlorine and bromine, the relative sensitivity decreased with increasing amounts of organic solvent. For iodine, the relative sensitivity reached...... structure. Many chlorine-, bromine-, and iodine-containing compounds were partially lost in the desolvating unit. For those chlorine- and iodine-containing compounds that were not lost, the sensitivity was independent of methanol concentration in the solvent when a 0-100% methanol gradient was applied......With the purpose of finding ways to combine micro-bore reversed phase HPLC with ICP-MS detection for analysis of drug substances containing chlorine, bromine and iodine, the suitability of a direct injection nebulizer and an Aridus desolvating microconcentric nebulizer was compared. Using...

  12. Simultaneous measurement of 239Pu, 240Pu, 241Pu, and 242Pu by high resolution inductively coupled plasma mass spectrometer (HR ICP-MS) in marine sediments

    International Nuclear Information System (INIS)

    Bruneau, F.

    1999-01-01

    Transuranics elements are of particular interest in radioecological studies because of their radiotoxicity and their potential use to decipher source fingerprints and transport processes. The simultaneous measurement of 239 Pu, 240 Pu, 241 Pu, and 242 Pu in environmental samples requires a specific chemical procedure. This work deals with an analytical procedure which yields a very high grade of purification of Pu suitable for ultra low level detection by HR ICP-MS, from marine sediments. After the elimination of major elements (Fe, Al, Mg...) by a first chromatographic separation, a new device of purification by solvent extraction and concentration by a second chromatographic separation is used to obtain a concentrated and high purified solution of plutonium. The chemical procedure have been validated on IAEA certified sediment samples and on sediment samples collected in the roads of Cherbourg which had been previously analysed by other techniques (a spectrometry and thermo-ionisation mass spectrometer). (author)

  13. Isotopic compositions of Sr in waters and of Pb in sediments and ashes from an urban incinerator using an ICP-MS

    International Nuclear Information System (INIS)

    Fillion, N.; Clauer, N.; Samuen, J.

    1996-01-01

    The analytical precision of the Sr and the Pb isotopic compositions of natural samples obtained with a conventional ICP-MS is of 3 to 7 x 10 -3 (internal 2 σ) for the 87 Sr/ 86 Sr ratio, 6 to 8 x 10 -3 for the 206 Pb/ 207 Pb and 1 to 4 x 10 -1 for the 206 Pb/ 204 Pb and 207 Pb/ 204 Pb ratios. Such accuracy is obtained with a procedure including a resin-chromatographic purification, a correction with respect to standard values (NBS 987 and 981) and a routine of four determinations for each sample. This procedure should allow rapid geochemical investigations ahead of more precise determinations by thermo-ionization mass spectrometry. (authors). 8 refs., 6 figs., 5 tabs

  14. The use of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of toxic and essential elements in different types of food samples

    Science.gov (United States)

    Voica, C.; Dehelean, A.; Kovacs, M. H.

    2012-02-01

    Food is the primary source of essential elements for humans and it is an important source of exposure to toxic elements. In this context, levels of essential and toxic elements must be determined routinely in consumed food products. The content of trace elements (As, Pb, Cu, Cd, Zn, Sn, Hg) in different types of food samples (e.g. rice, bread, sugar, cheese, milk, butter, wheat, coffee, chocolate, biscuits pasta, etc.) was determined, using inductively coupled plasma mass spectrometry (ICP-MS). Trace element contents in some foods were higher than maximum permissible levels of toxic metals in human food (Cd in bread, Zn in cheese, Cu in coffee, Hg in carrots and peppers).

  15. Quality control considerations for size exclusion chromatography with online ICP-MS: a powerful tool for evaluating the size dependence of metal-organic matter complexation.

    Science.gov (United States)

    McKenzie, Erica R; Young, Thomas M

    2013-01-01

    Size exclusion chromatography (SEC), which separates molecules based on molecular volume, can be coupled with online inductively coupled plasma mass spectrometry (ICP-MS) to explore size-dependent metal-natural organic matter (NOM) complexation. To make effective use of this analytical dual detector system, the operator should be mindful of quality control measures. Al, Cr, Fe, Se, and Sn all exhibited columnless attenuation, which indicated unintended interactions with system components. Based on signal-to-noise ratio and peak reproducibility between duplicate analyses of environmental samples, consistent peak time and height were observed for Mg, Cl, Mn, Cu, Br, and Pb. Al, V, Fe, Co, Ni, Zn, Se, Cd, Sn, and Sb were less consistent overall, but produced consistent measurements in select samples. Ultrafiltering and centrifuging produced similar peak distributions, but glass fiber filtration produced more high molecular weight (MW) peaks. Storage in glass also produced more high MW peaks than did plastic bottles.

  16. Investigation of metallodrug-protein interactions by size-exclusion chromatography coupled with inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Szpunar, J.; Makarov, A.; Pieper, T.; Keppler, B.K.; Lobinski, R.

    1999-01-01

    The coupling of size-exclusion HPLC with ICP-MS was developed for the studies of the kinetics of metallodrug binding to human serum proteins. Two platinum- and three ruthenium-based drugs were investigated. Various SEC columns (of different lengths and with different packings) were compared for the separation of the protein-bound and unbound fractions of a metallodrug prior to on-line detection of the metal (Ru or Pt). The approach developed offers considerable advantages over the methods based on ultrafiltration followed by the off-line metal determination in terms of speed, simplicity, precision and selectivity regarding the molecular weight of the complexes involved. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  17. Application of inductively coupled plasma mass spectrometry (ICP/MS) to detection of trace elements, heavy metals and radioisotopes in scalp hair

    International Nuclear Information System (INIS)

    Ozturk, Yildirim; Benderli, Cihan

    2010-01-01

    Trace element analysis of human hair has the potential to reveal retrospective information about an individual's nutritional status and exposure. As trace elements are incorporated into the hair during the growth process, longitudinal segments of the hair may reflect the body burden during the growth period. it was evaluated the potential of human hair to indicate exposure or nutritional status over time by analysing trace element profiles in single strands of human hair. By using inductively coupled plasma mass spectrometry (ICP-MS), it was achieved profiles of 43 elements in single strands of human hair. It was shown that trace element analysis along single strands of human hair can yield information about essential and toxic elements and for some elements, can be correlated with seasonal changes in diet and exposure. The information obtained from the trace element profiles of human hair in this study substantiates the potential of hair as a biomarker

  18. Meso-optical Fourier transform microscope with double focusing

    International Nuclear Information System (INIS)

    Batusov, Yu.A.; Soroko, L.M.; Tereshchenko, V.V.

    1992-01-01

    The meso-optical Fourier transform microscope (MFTM) with double focusing for particle tracks of low ionization level in the nuclear emulsion is described. It is shown experimentally that this device enables one to get high concentration of information about the position of the particle track in the nuclear emulsion and thus to increase the signal-to-noise ratio. It is shown that spreading of the meso-optical image of the particle track in the sagittal section of the MFTM can be eliminated completely in the frame of the diffraction limit. The number of the additional degrees of freedom in this new MFTM system along depth coordinate is equal to 20 in comparison to single degree of freedom in the Fourier transform microscope of the direct observation. 10 refs.; 15 figs

  19. ICP-MS analysis of lanthanide-doped nanoparticles: A quantitative and multiplexing approach to investigate biodistribution, blood clearance, and targeting

    Science.gov (United States)

    Crayton, Samuel

    The rapidly progressing field of nanotechnology promises to revolutionize healthcare in the 21st century, with applications in the prevention, diagnosis, and treatment of a wide range of diseases. However, before nanoparticulate agents can be brought into clinical use, they must first be developed, optimized, and evaluated in animal models. In the typical pre-clinical paradigm, almost all of the optimization is done at the in vitro level, with only a few select agents reaching the level of animal studies. Since only one experimental nanoparticle formulation can be investigated in a single animal, and in vivo experiments have relatively higher complexity, cost, and time requirements, it is not feasible to evaluate a very large number of agents at the in vivo stage. A major drawback of this approach, however, is that in vitro assays do not always accurately predict how a nanoparticle will perform in animal studies. Therefore, a method that allows many agents to be evaluated in a single animal subject would allow for much more efficient and predictive optimization of nanoparticles. We have found that by incorporating lanthanide tracer metals into nanoparticle formulations, we are successfully able to use inductively coupled plasma mass spectrometry (ICP-MS) to quantitatively determine a nanoparticle's blood clearance kinetics, biodistribution, and tumor delivery. This approach was applied to evaluate both passive and active tumor targeting, as well as metabolically directed targeting of nanoparticles to low pH tumor microenvironments. Importantly, we found that these in vivo measurements could be made for many nanoparticle formulations simultaneously, in single animals, due to the high-order multiplexing capability of mass spectrometry. This approach allowed for efficient and reproducible comparison of performance between different nanoparticle formulations, by eliminating the effects of subject-to-subject variability. In the future, we envision that this "higher

  20. Determination of Metal Levels in Shamma (Smokeless Tobacco) with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) in Najran, Saudi Arabia

    Science.gov (United States)

    Brima, Eid Ibrahim

    2016-10-01

    Objective: The use of Shamma (smokeless tobacco) by certain groups is giving rise to health problems, including cancer, in parts of Saudi Arabia. Our objective was to determine metals levels in Shamma using inductively coupled plasma mass spectrometry (ICP-MS). Methods: Thirty-three samples of Shamma (smokeless tobacco) were collected, comprising four types: brown Shamma (n = 14.0), red Shamma (n = 9.0), white Shamma (n = 4.0), and yellow Shamma (n = 6.0). All samples were collected randomly from Shamma users in the city of Najran. Levels of 11 elements (Al, As, Cd, Co, Cr, Cu, Li, Mn, Ni, Pb, and Zn) were determined by ICP-MS. Results: A mixed standard (20 ppb) of all elements was used for quality control, and average recoveries ranged from 74.7% to 112.2%. The highest average concentrations were found in the following order: Al (598.8–812.2 μg/g), Mn (51.0–80.6 μg/g), and Ni (23.2–53.3 μg/g) in all four Shamma types. The lowest concentrations were for As (0.7–1.0 μg/g) and Cd (0.0–0.06 μg/g). Conclusions: The colour of each Shamma type reflects additives mixed into the tobacco. Cr and Cu were showed significant differences (P awareness about the safety and health effects of Shamma, which is clearly a source of oral exposure to metals. Creative Commons Attribution License

  1. Determination of reduced homocysteine in human serum by elemental labelling and liquid chromatography with ICP-MS and ESI-MS detection.

    Science.gov (United States)

    Espina, Juan Gómez; Montes-Bayón, Maria; Blanco-González, Elisa; Sanz-Medel, Alfredo

    2015-10-01

    Analytical methods allowing sensitive determination of reduced homocysteine (rHcy), one of the so-called biothiols, in human serum is a topic of growing interest due to its close relation to several human disorders, mainly cardiovascular diseases. Although most widely used analytical strategies to determine total Hcy involve derivatization by means of fluorescent labels, this work proposes the use of ebselen, a Se-containing labelling agent to derivatize the reactive sulfhydryl group of the Hcy molecule in its "free" reduced form, which is more likely to play different roles in disease pathogenesis. Optimization of the derivatization and separation conditions by high-performance liquid chromatography (HPLC) to isolate the excess of derivatizing reagent is carried out here using UV/VIS detection. Further, the study of the Se labelling reaction by electrospray ionization tandem mass spectrometry (ESI-MS/MS) provides a stoichiometry of the derivative of 1:1. The main advantage of using ebselen as a labelling agent is the presence of the Se atom in the molecule that allows the use of inductively coupled plasma mass spectrometry (ICP-MS) as a sensitive and selective Se detector. The coupling of HPLC with ICP-MS provided excellent features for the determination of Se-derivatized rHcy (detection limit of 9.6 nM) in real samples. Quantification was accomplished by using post-column isotope dilution (ID) of Se in serum samples, after precipitation of the main serum proteins. Quantitative results for "free" rHcy turned out to be around 0.18-0.22 μM in serum samples from healthy individuals that could be directly analyzed without sample preconcentration.

  2. Trace element profiles in modern horse molar enamel as tracers of seasonality: Evidence from micro-XRF, LA-ICP-MS and stable isotope analysis

    Science.gov (United States)

    de Winter, Niels; Goderis, Steven; van Malderen, Stijn; Vanhaecke, Frank; Claeys, Philippe

    2016-04-01

    A combination of laboratory micro-X-ray Fluorescence (μXRF) and stable carbon and oxygen isotope analysis shows that trace element profiles from modern horse molars reveal a seasonal pattern that co-varies with seasonality in the oxygen isotope records of enamel carbonate from the same teeth. A combination of six cheek teeth (premolars and molars) from the same individual yields a seasonal isotope and trace element record of approximately three years recorded during the growth of the molars. This record shows that reproducible measurements of various trace element ratios (e.g., Sr/Ca, Zn/Ca, Fe/Ca, K/Ca and S/Ca) lag the seasonal pattern in oxygen isotope records by 2-3 months. Laser Ablation-ICP-Mass Spectrometry (LA-ICP-MS) analysis on a cross-section of the first molar of the same individual is compared to the bench-top tube-excitation μXRF results to test the robustness of the measurements and to compare both methods. Furthermore, trace element (e.g. Sr, Zn, Mg & Ba) profiles perpendicular to the growth direction of the same tooth, as well as profiles parallel to the growth direction are measured with LA-ICP-MS and μXRF to study the internal distribution of trace element ratios in two dimensions. Results of this extensive complementary line-scanning procedure shows the robustness of state of the art laboratory micro-XRF scanning for the measurement of trace elements in bioapatite. The comparison highlights the advantages and disadvantages of both methods for trace element analysis and illustrates their complementarity. Results of internal variation within the teeth shed light on the origins of trace elements in mammal teeth and their potential use for paleo-environmental reconstruction.

  3. The micro-scale synthesis of (117)Sn-enriched tributyltin chloride and its characterization by GC-ICP-MS and NMR techniques.

    Science.gov (United States)

    Peeters, Kelly; Iskra, Jernej; Zuliani, Tea; Ščančar, Janez; Milačič, Radmila

    2014-07-01

    Organotin compounds (OTCs) are among the most toxic substances ever introduced to the environment by man. They are common pollutants in marine ecosystems, but are also present in the terrestrial environment, accumulated mainly in sewage sludge and landfill leachates. In investigations of the degradation and methylation processes of OTC in environmental samples, the use of enriched isotopic tracers represents a powerful analytical tool. Sn-enriched OTC are also necessary in application of the isotope dilution mass spectrometry technique for their accurate quantification. Since Sn-enriched monobutyltin (MBT), dibutyltin (DBT) and tributyltin (TBT) are not commercially available as single species, "in house" synthesis of individual butyltin-enriched species is necessary. In the present work, the preparation of the most toxic butyltin, namely TBT, was performed via a simple synthetic path, starting with bromination of metallic Sn, followed by butylation with butyl lithium. The tetrabutyltin (TeBT) formed was transformed to tributyltin chloride (TBTCl) using concentrated hydrochloric acid (HCl). The purity of the synthesized TBT was verified by speciation analysis using the techniques of gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS) and nuclear magnetic resonance (NMR). The results showed that TBT had a purity of more than 97%. The remaining 3% corresponded to DBT. TBT was quantified by reverse isotope dilution GC-ICP-MS. The synthesis yield was around 60%. The advantage of this procedure over those previously reported lies in its possibility to be applied on a micro-scale (starting with 10mg of metallic Sn). This feature is of crucial importance, since enriched metallic Sn is extremely expensive. The procedure is simple and repeatable, and was successfully applied for the preparation of (117)Sn-enriched TBTCl from (117)Sn-enriched metal. Copyright © 2014 Elsevier Ltd. All rights reserved.

  4. Results of LA-ICP-MS sulfide mapping from Algoma-type BIF gold systems with implications for the nature of mineralizing fluids, metal sources, and deposit models

    Science.gov (United States)

    Gourcerol, B.; Kontak, D. J.; Thurston, P. C.; Petrus, J. A.

    2018-01-01

    Quantitative laser ablation inductively coupled plasma-mass spectrometry (LA-ICP-MS) element distribution maps combined with traverse mode analyses have been acquired on various sulfides (pyrite, pyrrhotite, arsenopyrite) from three Canadian Algoma-type BIF-hosted gold deposits ( 4 Moz Au Meadowbank, ≥ 2.8 Moz Au Meliadine district, 6 Moz Au Musselwhite). These data, in conjunction with detailed petrographic and SEM-EDS observations, provide insight into the nature and relative timing of gold events, the presence and implication of trace element zoning regarding crystallization processes, and elemental associations that fingerprint gold events. Furthermore, the use of an innovative method of processing the LA-ICP-MS data in map and traverse modes, whereby the results are fragmented into time-slice data, to generate various binary plots (Ag versus Ni) provides a means to identify elemental associations (Te, Bi) not otherwise apparent. This integrated means of treating geochemical data, along with petrography, allows multiple gold events and remobilization processes to be recognized and their elemental associations determined. The main gold event in each of these deposits is characterized by the coupling of an As-Se-Te-Ag element association coincident with intense stratabound sulfide-replacement of the Fe-rich host rock. Additionally, the data indicate presence of a later remobilization event, which upgraded the Au tenor, as either non-refractory or refractory type, along fracture networks due to the ingress of subsequent base metal-bearing metamorphic fluids (mainly a Pb-Bi association). Furthermore, the data reveal a stratigraphic influence, as reflected in the elemental associations and the elemental enrichments observed and the nature of the sulfide phase hosting the gold mineralization (arsenopyrite versus pyrite).

  5. Evaluating the capabilities of aerosol-to-liquid particle extraction system (ALPXS)/ICP-MS for monitoring trace metals in indoor air.

    Science.gov (United States)

    Jayawardene, Innocent; Rasmussen, Pat E; Chenier, Marc; Gardner, H David

    2014-09-01

    This study investigates the application of the Aerosol-to-Liquid Particle Extraction System (ALPXS), which uses wet electrostatic precipitation to collect airborne particles, for multi-element indoor stationary monitoring. Optimum conditions are determined for capturing airborne particles for metal determination by inductively coupled plasma-mass spectrometry (ICP-MS), for measuring field blanks, and for calculating limits of detection (LOD) and quantification (LOQ). Due to the relatively high flow rate (300 L min(-1)), a sampling duration of 1 hr to 2 hr was adequate to capture airborne particle-bound metals under the investigated experimental conditions. The performance of the ALPXS during a building renovation demonstrated signal-to-noise ratios appropriate for sampling airborne particles in environments with elevated metal concentrations, such as workplace settings. The ALPXS shows promise as a research tool for providing useful information on short-term variations (transient signals) and for trapping particles into aqueous solutions where needed for subsequent characterization. As the ALPXS does not provide size-specific samples, and its efficiency at different flow rates has yet to be quantified, the ALPXS would not replace standard filter-based protocols accepted for regulatory applications (e.g., exposure measurements), but rather would provide additional information if used in conjunction with filter based methods. Implications: This study investigates the capability of the Aerosol-to-Liquid Particle Extraction System (ALPXS) for stationary sampling of airborne metals in indoor workplace environments, with subsequent analysis by ICP-MS. The high flow rate (300 L/min) permits a short sampling duration (< 2 hr). Results indicated that the ALPXS was capable of monitoring short-term changes in metal emissions during a renovation activity. This portable instrument may prove to be advantageous in occupational settings as a qualitative indicator of elevated

  6. Chemical speciation of arsenic species in human blood serum by liquid chromatography using a phosphatidylcholine-coated ODS column with detection by ICP-MS

    International Nuclear Information System (INIS)

    Hasegawa, Takuya; Ishise, Jotaro; Fukumoto, Yasuharu; Matsuura, Hirotaka; Zhu, Yanbei; Umemura, Tomonari; Haraguchi, Hiroki; Yamamoto, Kazuhito; Naoe, Tomoki

    2007-01-01

    Chemical speciation of arsenic species in human blood serum was performed by high-performance liquid chromatography/inductively coupled plasma mass spectrometry (HPLC/ICP-MS) with direct sample injection, where an octadecylsilyl silica (ODS) column coated with phosphatidylcholine (PC) (hereafter known as 'PC-coated ODS column') was used as the separation column. In arsenic species analysis, a citrate buffer solution (pH 4.0) was used as the mobile phase, in which the following reagents were added: sodium 1-dodecanesulfonate (SDS), tetramethylammonium hydroxide (TMAH), which are ion-pair reagents to separate inorganic and organic arsenic species, and 3-[(3-cholamidopropyl)-dimethylammonio]-1-propane sulfonate (CHAPS), which is a protein-solubilizing agent to prevent adsorption of proteins on the column. As a result of optimization, five representative arsenic species spiked in human blood serum reference material could be separated from each other within 5 min on the PC-coated ODS column by elution with a 5 mM citrate buffer (pH 4.0) containing 5 mM SDS, 5 mM THAH, and 0.2 mM CHAPS. The detection limits obtained by ICP-MS were 3.1, 2.7, 4.5, 2.5, and 2.5 ng of As g -1 for arsenate (iAs V ), arsenite (iAs III ), monomethylarsonic acid (MMA), dimethylarsenic acid (DMA), and arsenobetaine (AB), respectively, when the injection volume was 20 μL. The present separation system was also applied to speciation analysis of arsenic species in human blood serum collected from a leukemia patient after therapeutic treatment with arsenic. (author)

  7. Direct spectral analysis of tea samples using 266 nm UV pulsed laser-induced breakdown spectroscopy and cross validation of LIBS results with ICP-MS.

    Science.gov (United States)

    Gondal, M A; Habibullah, Y B; Baig, Umair; Oloore, L E

    2016-05-15

    Tea is one of the most common and popular beverages spanning vast array of cultures all over the world. The main nutritional benefits of drinking tea are its anti-oxidant properties, presumed protection against certain cancers, inhibition of inflammation and possible protective effects against diabetes. Laser induced breakdown spectrometer (LIBS) was assembled as a powerful tool for qualitative and quantitative analysis of various brands of tea samples using 266 nm pulsed UV laser. LIBS spectra for six brands of tea samples in the wavelength range of 200-900 nm was recorded and all elements present in our tea samples were identified. The major toxic elements detected in several brands of tea samples were bromine, chromium and minerals like iron, calcium, potassium and silicon. The spectral assignment was conducted prior to the determination of concentration of each element. For quantitative analysis, calibration curves were drawn for each element using standard samples prepared in known concentration in the tea matrix. The plasma parameters (electron temperature and electron density) were also determined prior to the tea samples spectroscopic analysis. The concentration of iron, chromium, potassium, bromine, copper, silicon and calcium detected in all tea samples was between 378-656, 96-124, 1421-6785, 99-1476, 17-36, 2-11 and 92-130 mg L(-1) respectively. The limits of detection estimated for Fe, Cr, K, Br, Cu, Si, Ca in tea samples were 22, 12, 14, 11, 6, 1 and 12 mg L(-1) respectively. To further confirm the accuracy of our LIBS results, we determined the concentration of each element present in tea samples by using standard analytical technique like ICP-MS. The concentrations detected with our LIBS system are in excellent agreement with ICP-MS results. The system assembled for spectral analysis in this work could be highly applicable for testing the quality and purity of food and also pharmaceuticals products. Copyright © 2016 Elsevier B.V. All rights reserved.

  8. Quantification of 226Ra at environmental relevant levels in natural waters by ICP-MS: Optimization, validation and limitations of an extraction and preconcentration approach.

    Science.gov (United States)

    Lagacé, François; Foucher, Delphine; Surette, Céline; Clarisse, Olivier

    2017-05-15

    Radium (Ra) at environmental relevant levels in natural waters was determined by ICP-MS after an off-line pre-concentration procedure. The latter consisted of Ra selective elution from potential interfering elements (i.e. other alkaline earth cations: Ba 2+ , Sr 2+ , Ca 2+ , Mg 2+ ) on a series of two different ion exchange resins (AG50W-X8 and Sr-resin). The overall analytical method was optimized according to the instrumental performance, the volume of water sample loaded on resins, and the sample salinity. Longer acquisition time (up to 150 s) was required to ensure stable measurement of Ra by ICP-MS at ultra trace level (1.0pgL -1 ). For a synthetic groundwater spiked with Ra at 10.0pgL -1 , the analytical procedure demonstrated efficient separation of the analyte from its potential interfering elements and a complete recovery, independent of the sample volume tested from 10 up to 100mL. For synthetic seawater spiked at a level of 10.0pgL -1 of Ra, the total load of salts on the two resins should not exceed 0.35g in order to ensure a complete separation and recovery of Ra. The method was validated on natural waters (i.e. groundwater, freshwater and seawater samples) spiked with Ra at different levels (0.0, 0.5, 1.0 and 5.0pgL -1 ). Absolute Ra detection limits were determined at 0.020pgL -1 (0.73mBqL -1 ) and 0.12pgL -1 (4.4mBqL -1 ) respectively for 60.0mL of freshwater sample and for 10.0mL of seawater. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Analysis of corrosions-products in tissue samples near surgical implants by means of LAMMA (Laser Microprobe Mass Analyzer) and ICP-MS (Inductively Coupled Plasma Mass Spectrometer)

    International Nuclear Information System (INIS)

    Schlagenhaufen, C.

    1996-08-01

    In this work corrosion products of surgical implants in tissue samples were identified. For the characterization of the corrosion products the LAMMA 500 (Laser Microprobe Mass Analyzer) was used. Additional analysis were made with the ICP-MS (Inductively Coupled Plasma Mass Spectrometer) to determine the concentration of chromium, cobalt, nickel, and molybdenum in the tissues. In the first part several synthetic chromium- and molybdenum compounds were investigated with LAMMA. With the anionic mass spectra of the chromium-compounds it is possible to the oxidation state of chromium. The mass spectra of the synthetic compounds were used to identify, the compounds in the corrosion products. In the second part thin sections prepared from the tissue samples from the surrounding of the implants were analyzed. Several embedding and cutting methods were tested. Histological staining methods and LAMMA spectra were used to characterize the deposits in the tissue. Three different deposits were found in the tissue. In all tissues metal splinters from the implant were found. In most of the tissues iron-rich deposits were found, that were identified as iron-phosphate. As definitive corrosion products of the implant mixtures of chromium(III)phosphate, calcium molybdate, calcium phosphate and chromium(III) molybdate were identified. The ICP-MS results show in comparison to normal values, very high concentrations for chromium, nickel, cobalt and molybdenum. These results support the conclusions based on LAMMA results. The results of these investigations clearly indicate, that stainless steel implants, are not corrosion-resistant in the body. Relatively high amounts of the constituents, of the implant dissolved, and are deposited as solid compounds in the tissue next to the implant. (author)

  10. Determination of Arsenic Species in Ophiocordyceps sinensis from Major Habitats in China by HPLC-ICP-MS and the Edible Hazard Assessment.

    Science.gov (United States)

    Guo, Lian-Xian; Zhang, Gui-Wei; Wang, Jia-Ting; Zhong, Yue-Ping; Huang, Zhi-Gang

    2018-04-26

    This study sought to determine the concentration and distribution of arsenic (As) species in Ophiocordyceps sinensis ( O. sinensis ), and to assess its edible hazard for long term consumption. The total arsenic concentrations, measured through inductively coupled plasma mass spectrometry (ICP-MS), ranged from 4.00 mg/kg to 5.25 mg/kg. As determined by HPLC-ICP-MS, the most concerning arsenic species—AsB, MMA V , DMA V , As V , and As Ш —were either not detected (MMA V and DMA V ) or were detected as minor As species (AsB: 1.4⁻2.9%; As V : 1.3⁻3.2%, and As Ш : 4.1⁻6.0%). The major components were a cluster of unknown organic As (uAs) compounds with As Ш , which accounted for 91.7⁻94.0% of the As content. Based on th