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Sample records for icp-ms titanite u-th-pb

  1. U-Th-Pb systematics in zircon and titanite

    International Nuclear Information System (INIS)

    Zartman, R.E.; Kwak, L.M.

    1990-01-01

    U-Th-Pb isotopic analyses of zircon and titanite were made for two core samples of granite from borehole ATK-1 drilled into the Eye-Dashwa Lakes pluton. One of the samples from near the bottom of the hole (990.97 to 996.78 m) yielded zircon and titanite that were slightly to severely disturbed isotopically. Eight fractions of zircon give an upper concordia intercept age of 2625 ± 16 Ma (MSWD = 34), which, based on an evaluation of the more concordant data points and on other geochronological results, is interpreted as being slightly too young. The time of crystallization is probably better approximated by the 207 Pb/ 206 Pb age of 2665 Ma determined on a slightly (∼8 percent) discordant titanite. The other sample from near the surface (3.85 to 9.61 m) generally revealed even more severely disturbed isotopic systematics for both zircon and titanite. The complex nature of the disturbances probably resulted from the penetration of meteoritic water into rock already modified by post-crystallization hydrothermal alteration. Nuclide migration occurred in both minerals -- during the Middle or Late Proterozoic for the zircon and during the modern weathering cycle for the titanite. Material balance calculations are used to demonstrate a recent relative gain of radiogenic Pb and/or loss of Th and U from the freshest-looking, least-altered titanite by exchange with altered, leucoxenite-bearing titanite

  2. Reply to Comment on "Zircon U-Th-Pb dating using LA-ICP-MS: Simultaneous U-Pb and U-Th dating on the 0.1 Ma Toya Tephra, Japan"

    Science.gov (United States)

    Ito, Hisatoshi

    2015-04-01

    Guillong et al. (2015) mentioned that corrections for abundance sensitivity for 232Th and molecular zirconium sesquioxide ions (Zr2O3+) are critical for reliable determination of 230Th abundances in zircon for LA-ICP-MS analyses. There is no denying that more rigorous treatments are necessary to obtain more reliable ages than those in Ito (2014). However, as shown in Fig. 2 in Guillong et al. (2015), the uncorrected (230Th)/(238U) for reference zircons except for Mud Tank are only 5-20% higher than unity. Since U abundance of Toya Tephra zircons that have U-Pb ages Ito (2014) obtained U-Th ages of the Toya Tephra by comparison with Fish Canyon Tuff (FCT) data. Because both the FCT and the Toya Tephra have similar trends of overestimation of 230Th, the effect of overestimation of 230Th to cause overestimation of U-Th age should be cancelled out or negligible. Therefore the pivotal conclusion in Ito (2014) that simultaneous U-Pb and U-Th dating using LA-ICP-MS is possible and useful for Quaternary zircons holds true.

  3. Hydrothermal titanite from the Chengchao iron skarn deposit: temporal constraints on iron mineralization, and its potential as a reference material for titanite U-Pb dating

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    Hu, Hao; Li, Jian-Wei; McFarlane, Christopher R. M.

    2017-09-01

    Uranium-lead isotopes and trace elements of titanite from the Chengchao iron skarn deposit (Daye district, Eastern China), located along the contact zones between Triassic marine carbonates and an early Cretaceous intrusive complex consisting of granite and quartz diorite, were analyzed using laser ablation inductively coupled plasma mass spectrometry to provide temporal constraints on iron mineralization and to evaluate its potential as a reference material for titanite U-Pb geochronology. Titanite grains from mineralized endoskarn have simple growth zoning patterns, exhibit intergrowth with magnetite, diopside, K-feldspar, albite and actinolite, and typically contain abundant primary two-phase fluid inclusions. These paragenetic and textural features suggest that these titanite grains are of hydrothermal origin. Hydrothermal titanite is distinct from the magmatic variety from the ore-related granitic intrusion in that it contains unusually high concentrations of U (up to 2995 ppm), low levels of Th (12.5-453 ppm), and virtually no common Pb. The REE concentrations are much lower, as are the Th/U and Lu/Hf ratios. The hydrothermal titanite grains yield reproducible uncorrected U-Pb ages ranging from 129.7 ± 0.7 to 132.1 ± 2.7 Ma (2σ), with a weighted mean of 131.2 ± 0.2 Ma [mean standard weighted deviation (MSWD) = 1.7] that is interpreted as the timing of iron skarn mineralization. This age closely corresponds to the zircon U-Pb age of 130.9 ± 0.7 Ma (MSWD = 0.7) determined for the quartz diorite, and the U-Pb ages for zircon and titanite (130.1 ± 1.0 Ma and 131.3 ± 0.3 Ma) in the granite, confirming a close temporal and likely genetic relationship between granitic magmatism and iron mineralization. Different hydrothermal titanite grains have virtually identical uncorrected U-Pb ratios suggestive of negligible common Pb in the mineral. The homogeneous textures and U-Pb characteristics of Chengchao hydrothermal titanite suggest that the mineral might be a

  4. 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

  5. LA-ICP-MS and SIMS U-Pb and U-Th zircon geochronological data of Late Pleistocene lava domes of the Ciomadul Volcanic Dome Complex (Eastern Carpathians

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    Réka Lukács

    2018-06-01

    Full Text Available This article provides laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS and secondary ionization mass spectrometry (SIMS U-Pb and U-Th zircon dates for crystals separated from Late Pleistocene dacitic lava dome rocks of the Ciomadul Volcanic Dome Complex (Eastern Carpathians, Romania. The analyses were performed on unpolished zircon prism faces (termed rim analyses and on crystal interiors exposed through mechanical grinding an polishing (interior analyses. 206Pb/238U ages are corrected for Th-disequilibrium based on published and calculated distribution coefficients for U and Th using average whole-rock and individually analyzed zircon compositions. The data presented in this article were used for the Th-disequilibrium correction of (U-Th/He zircon geochronology data in the research article entitled “The onset of the volcanism in the Ciomadul Volcanic Dome Complex (Eastern Carpathians: eruption chronology and magma type variation” (Molnár et al., 2018 [1].

  6. Comment on "Zircon U-Th-Pb dating using LA-ICP-MS: Simultaneous U-Pb and U-Th dating on 0.1 Ma Toya Tephra, Japan" by Hisatoshi Ito

    Science.gov (United States)

    Guillong, M.; Schmitt, A. K.; Bachmann, O.

    2015-04-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) of eight zircon reference materials and synthetic zircon-hafnon end-members indicate that corrections for abundance sensitivity and molecular zirconium sesquioxide ions (Zr2O3+) are critical for reliable determination of 230Th abundances in zircon. Other polyatomic interferences in the mass range 223-233 amu are insignificant. When corrected for abundance sensitivity and interferences, activity ratios of (230Th)/(238U) for the zircon reference materials we used average 1.001 ± 0.010 (1σ error; mean square of weighted deviates MSWD = 1.45; n = 8). This includes the 91500 and Plešovice zircons, which were deemed unsuitable for calibration of (230Th)/(238U) by Ito (2014). Uranium series zircon ages generated by LA-ICP-MS without mitigating (e.g., by high mass resolution) or correcting for abundance sensitivity and molecular interferences on 230Th such as those presented by Ito (2014) are potentially unreliable.

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

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    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)

  8. Integrated Laser Ablation U/Pb and (U-Th)/He Dating of Detrital Accessory Minerals from the Naryani River, Central Nepal

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    Horne, A.; Hodges, K. V.; Van Soest, M. C.

    2015-12-01

    The newly developed 'laser ablation double dating' (LADD) technique, an integrated laser microprobe U/Pb and (U-Th)/He dating method, could be an exceptionally valuable tool in detrital thermochronology for identifying sedimentary provenance and evaluating the exhumation history of a source region. A recent proof-of-concept study has used LADD to successfully date both zircon and titanite crystals from the well-characterized Fish Canyon tuff, but we also believe that another accessory mineral, rutile, could be amenable to dating via the LADD technique. To continue the development of the method, we present an application of LADD to detrital zircon, titanite, and rutile from a sample collected on the lower Naryani River of central Nepal. Preliminary analyses of the sample have yielded zircon U/Pb dates ranging from 31.4 to 2405 Ma; zircon (U-Th)/He from 1.8 to 15.4 Ma; titanite U/Pb between 18 and 110 Ma; titanite (U-Th)/He between 1 and 16 Ma; rutile U/Pb from 6 to 45 Ma; and rutile (U-Th)/He from 2 to 25 Ma. In addition to the initial data, we can use Ti-in-zircon, Zr-in-titanite, and Zr-in-rutile thermometers to determine the range of possible long-term cooling rates from grains with U/Pb ages younger than collision. Thus far our results from zircon analyses imply a cooling rate of approximately 15°C/Myr; titanite analyses imply between 10 and 67°C/Myr; and rutile between 9 and 267°C/Myr. This spread in potential cooling rates, especially in the order of magnitude differences of cooling rates calculated from the rutile grains, suggests that the hinterland source regions of the Naryani river experienced dramatically different exhumation histories during Himalayan orogenisis. Ongoing analyses will expand the dataset such that we can more adequately characterize the range of possibilities represented in the sample.

  9. 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)

  10. 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)

  11. U-Pb ages related to uranium mineralization of Lagoa Real, Bahia - Brazil: tectonic implications

    Energy Technology Data Exchange (ETDEWEB)

    Chaves, Alexandre O.; Rios, Francisco J.; Oliveira, Lucilia A.R.; Alves, James V.; Fuzikawa, Kazuo; Neves, Jose M.C.; Chaves, Adriana M.D.V.; Prates, Sonia P. [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)]. E-mail: aoc@cdtn.br; Tubrett, Michael [Memorial University of Newfoundland, NL (Canada). Inco Innovation Centre. MicroAnalysis Facility; Matos, Evando C. [Industrias Nucleares do Brasil S.A. (INB), Rio de Janeiro, RJ (Brazil)

    2007-07-01

    The uranium from Lagoa Real (Bahia/Brazil) is associated with syenitic magmatism (1904 {+-}44 Ma minimum age from upper intercept of zircon U-Pb discordia by LA-ICP-MS) belonging to a mafic/ felsic lithologic association linked to the final stages of 2.05-1.80 Ga Orosirian Orogeny, which acted in the Paramirim Block. These syenitic rocks are rich not only in albite, but also in U-rich titanite (source of uranium). In association with the development of the Orosirian ductile shear zones, the syenites were crystallized and deformed. The metamorphic reactions, which include intense recrystallization of magmatic minerals, led uraninite to precipitate (1868 {+-} 69 Ma; U-Pb by LA-ICP MS) under Redox control. A second population of uraninites was also generated by shear zones reactivation during 0.6-0.5 Ga Brasiliano Orogeny (605 {+-} 170 Ma; U-Pb by LA-ICP-MS). The geotectonic implications are: a) the importance of the Orosirian event in the Paramirim Block during paleoproterozoic Sao Francisco/Congo Craton edification and b) the influence of the Brasiliano event in the Paramirim Block during the West-Gondwana assembly processes, indicated by the 605 {+-} 170 Ma uraninite (second population) age and by the 483 {+-} 100 Ma lower intercept of the metamorphosed syenite U-Pb discordia. (author)

  12. Age of the emerald mineralization from the Itabira-Nova Era District, Minas Gerais, Brazil, based on LA-ICP-MS geochronology of cogenetic titanite

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    Hanna Jordt-Evangelista

    Full Text Available ABSTRACT: In the Itabira-Nova Era Emerald District, southeast Brazil, gemological emerald is extracted from underground mines found in schist-type deposits at the contact zone of the Archean Metavolcanosedimentary Sequence of the Guanhães Complex and Paleoproterozoic anorogenic granites of the Borrachudos Suite. Schist-type deposits are commonly generated by reactions enhanced by deformation and heat during regional metamorphism. The age of the mineralization in the region has been a matter of debate for decades: Ages ranging from the Archean to the Neoproterozoic are mentioned in the literature. In the mineralized zone from the Piteiras mine fluorine-aluminum-bearing titanite is found in metamafic rocks. The fluorine content was probably derived from the Borrachudos granites and pegmatites like the beryllium for emerald, thus both minerals could have been generated during the same event. U-Pb titanite geochronology via laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS was performed on a thin section of a phlogopite-plagioclase-hornblende schist from the Piteiras mine. The determined age of 576 ± 7 Ma is also the probable age for emerald generation during the Brasiliano cycle, which was the only tectonometamorphic event postdating the intrusion of the granites. This event provided heat and fluids necessary for reactions between the Be- and the Cr-bearing rocks, thus enabling the formation of emeralds.

  13. 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.

  14. LA-ICP-MS U-Th-Pb Dating and Trace Element Geochemistry of Allanite: Implications on the Different Skarn Metallogenesis between the Giant Beiya Au and Machangqing Cu-Mo-(Au Deposits in Yunnan, SW China

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    Yu Fu

    2017-12-01

    Full Text Available The giant Beiya Au skarn deposit and Machangqing porphyry Cu-Mo-(Au deposit are located in the middle part of the Jinshajiang–Ailaoshan alkaline porphyry metallogenic belt. The Beiya deposit is the largest Au skarn deposit in China, whilst the Machangqing deposit comprises a well-developed porphyry-skarn-epithermal Cu-Mo-(Au mineral system. In this paper, we present new allanite U-Th-Pb ages and trace element geochemical data from the two deposits and discuss their respective skarn metallogenesis. Based on the mineral assemblage, texture and Th/U ratio, the allanite from the Beiya and Machangqing deposits are likely hydrothermal rather than magmatic. Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS allanite U-Th-Pb dating has yielded Th-Pb isochron ages of 33.4 ± 4.6 Ma (MSWD = 0.22 (Beiya and 35.4 ± 9.8 Ma (MSWD = 0.26 (Machangqing, representing the retrograde alteration and magnetite skarn mineralization age of the two deposits. The Beiya and Machangqing alkali porphyry-related mineralization are synchronous and genetically linked to the magmatic hydrothermal activities of the Himalayan orogenic event. Major and trace element compositions reveal that the Beiya allanite has higher Fe3+/(Fe3+ + Fe2+ ratios, U content and Th content than the Machangqing allanite, which indicate a higher oxygen fugacity and F content for the ore-forming fluids at Beiya. Such differences in the ore-forming fluids may have contributed to the different metallogenic scales and metal types in the Beiya and Machangqing deposit.

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

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    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

  16. Combined U-Pb and Lu-Hf isotope analyses by laser ablation MC-ICP-MS: methodology and applications

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    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)

  17. Zircon, titanite, and apatite (U-Th)/He ages and age-eU correlations from the Fennoscandian Shield, southern Sweden

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    Guenthner, William R.; Reiners, Peter W.; Drake, Henrik; Tillberg, Mikael

    2017-07-01

    Craton cores far from plate boundaries have traditionally been viewed as stable features that experience minimal vertical motion over 100-1000 Ma time scales. Here we show that the Fennoscandian Shield in southeastern Sweden experienced several episodes of burial and exhumation from 1800 Ma to the present. Apatite, titanite, and zircon (U-Th)/He ages from surface samples and drill cores constrain the long-term, low-temperature history of the Laxemar region. Single grain titanite and zircon (U-Th)/He ages are negatively correlated (104-838 Ma for zircon and 160-945 Ma for titanite) with effective uranium (eU = U + 0.235 × Th), a measurement proportional to radiation damage. Apatite ages are 102-258 Ma and are positively correlated with eU. These correlations are interpreted with damage-diffusivity models, and the modeled zircon He age-eU correlations constrain multiple episodes of heating and cooling from 1800 Ma to the present, which we interpret in the context of foreland basin systems related to the Neoproterozoic Sveconorwegian and Paleozoic Caledonian orogens. Inverse time-temperature models constrain an average burial temperature of 217°C during the Sveconorwegian, achieved between 944 Ma and 851 Ma, and 154°C during the Caledonian, achieved between 366 Ma and 224 Ma. Subsequent cooling to near-surface temperatures in both cases could be related to long-term exhumation caused by either postorogenic collapse or mantle dynamics related to the final assembly of Rodinia and Pangaea. Our titanite He age-eU correlations cannot currently be interpreted in the same fashion; however, this study represents one of the first examples of a damage-diffusivity relationship in this system, which deserves further research attention.

  18. Magmatic Longevity Constrained by ID-TIMS U-Pb Dating of Zircon and Titanite

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    Szymanowski, D.; Wotzlaw, J. F.; Ellis, B. S.; Bachmann, O.; Von Quadt, A.

    2016-12-01

    Clues about the timescales and thermal conditions associated with the growth and evacuation of large silicic magma reservoirs are frequently drawn from radiometric dating, diffusion modelling, or thermomechanical modelling. A growing amount of petrological and geochronological evidence, supported by thermal modelling, suggests that many silicic magma reservoirs may exist for some 104-106 years in the form of high-crystallinity mushes at relatively low temperatures ( 700-750°C; [1-3]). Geochronological studies addressing this issue typically utilise the U-Pb system in zircon capable of recording extended periods of crystallisation, particularly in evolved calc-alkaline systems that spend most of their lifetime zircon-saturated. In this study, we integrate U-Pb dating of zircon and titanite to investigate the longevity of the magma reservoir that produced the Kneeling Nun Tuff, a 35 Ma, >900 km3 crystal-rich rhyolitic super-eruption from the Mogollon-Datil volcanic field in New Mexico (USA). High-precision ID-TIMS U-Pb dates of single crystals of both zircon and titanite independently record a continuous crystallisation history over >400,000 years. We combine the dating of both accessory phases with textural, major, trace element and isotopic studies of single crystals, placing tight constraints on the thermal conditions of magma accumulation and storage while recording differentiation and rejuvenation processes within the magma reservoir. The results suggest a protracted `cool' upper-crustal storage of magma prior to the Kneeling Nun Tuff eruption followed by a melting event which reduced the magma crystallinity and conditioned it for eruption. [1] Bachmann & Bergantz (2004), J. Petrol. 45, 1565-1582. [2] Gelman et al. (2013), Geology 41, 759-762. [3] Cooper & Kent (2014), Nature 506, 480-483.

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

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    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...

  20. Titanite chronology, thermometry, and speedometry of ultrahigh-temperature (UHT) calc-silicates from south Madagascar: U-Pb dates, Zr temperatures, and lengthscales of trace-element diffusion

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    Holder, R. M.; Hacker, B. R.

    2017-12-01

    Calc-silicate rocks are often overlooked as sources of pressure-temperature-time data in granulite-UHT metamorphic terranes due to the strong dependence of calc-silicate mineral assemblages on complex fluid compositions and a lack of thermodynamic data on common high-temperature calc-silicate minerals such as scapolite. In the Ediacaran-Cambrian UHT rocks of southern Madagascar, clinopyroxene-scapolite-feldspar-quartz-zircon-titanite calc-silicate rocks are wide-spread. U-Pb dates of 540-520 Ma from unaltered portions of titanite correspond to cooling of the rocks through upper-amphibolite facies and indicate UHT metamorphism occurred before 540 Ma. Zr concentrations in these domains preserve growth temperatures of 900-950 °C, consistent with peak temperatures calculated by pseudosection modeling of nearby osumilite-bearing gneisses. Younger U-Pb dates (510-490 Ma) correspond to fluid-mediated Pb loss from titanite grains, which occurred below their diffusive Pb-closure temperature, along fractures. The extent of fluid alteration is seen clearly in back-scattered electron images and Zr-, Al-, Fe-, Ce-, and Nb-concentration maps. Laser-ablation depth profiling of idioblastic titanite grains shows preserved Pb diffusion profiles at grain rims, but there is no evidence for Zr diffusion, indicating that it was effectively immobile even at UHT.

  1. U-Pb systematics of zircon and titanite from the Gardnos impact structure, Norway: Evidence for impact at 546 Ma?

    Science.gov (United States)

    Kalleson, E.; Corfu, F.; Dypvik, H.

    2009-05-01

    Zircon and titanite were investigated in impactites of the Gardnos structure, a crater formed in Sveconorwegian (ca. 1 Ga) crust, which was then overridden in the Devonian by Caledonian nappes. Observed deformation features in zircons are granular texture, planar microstructures, and likely the incorporation of organic carbon during impact causing black staining of the zircon grains. The grains were studied by scanning electron microscopy (SEM) and cathode luminescence (CL) and dated by U-Pb isotope dilution - thermo-ionization mass spectrometry (ID-TIMS). Zircon grains without impact related features have U-Pb data showing moderate discordance (5-13%) and indicating formation ages mostly in the range of 1600-1000 Ma, except detrital zircon ages as old as >2481 Ma, reflecting the diversity of target rocks in the area. Titanite with concordant ages of 995-999 Ma dates metamorphism during final juxtaposition of the Telemarkia on the Idefjorden terrane to the east. Zircon grains with demonstrated or presumed shock features yield highly discordant (14-40%) U-Pb data, with a majority of them plotting along an array with a lower intercept of about 340 Ma reflecting the influence of the Caledonian orogeny and recent Pb-loss. One zircon grain was totally reset at 379 Ma during late Caledonian metamorphism, which also caused local growth of new titanite. A specific group of zircon grains yields data with relatively high discordance for moderate U contents, and five of these analyses, including that of a grain with proven granular or aggregate texture, fit a discordia line with an upper intercept of 546 ± 5 Ma. These features are interpreted as indicating zircon break-down to an amorphous state during impact, with subsequent recrystallization into microcrystalline aggregates causing extensive to complete Pb loss. We further suggest that their crystallinity prevented Pb loss during the Caledonian orogeny, while the small subgrain size and increasing metamictisation allowed

  2. Laser Ablation in situ (U-Th-Sm)/He and U-Pb Double-Dating of Apatite and Zircon: Techniques and Applications

    Science.gov (United States)

    McInnes, B.; Danišík, M.; Evans, N.; McDonald, B.; Becker, T.; Vermeesch, P.

    2015-12-01

    We present a new laser-based technique for rapid, quantitative and automated in situ microanalysis of U, Th, Sm, Pb and He for applications in geochronology, thermochronometry and geochemistry (Evans et al., 2015). This novel capability permits a detailed interrogation of the time-temperature history of rocks containing apatite, zircon and other accessory phases by providing both (U-Th-Sm)/He and U-Pb ages (+trace element analysis) on single crystals. In situ laser microanalysis offers several advantages over conventional bulk crystal methods in terms of safety, cost, productivity and spatial resolution. We developed and integrated a suite of analytical instruments including a 193 nm ArF excimer laser system (RESOlution M-50A-LR), a quadrupole ICP-MS (Agilent 7700s), an Alphachron helium mass spectrometry system and swappable flow-through and ultra-high vacuum analytical chambers. The analytical protocols include the following steps: mounting/polishing in PFA Teflon using methods similar to those adopted for fission track etching; laser He extraction and analysis using a 2 s ablation at 5 Hz and 2-3 J/cm2fluence; He pit volume measurement using atomic force microscopy, and U-Th-Sm-Pb (plus optional trace element) analysis using traditional laser ablation methods. The major analytical challenges for apatite include the low U, Th and He contents relative to zircon and the elevated common Pb content. On the other hand, apatite typically has less extreme and less complex zoning of parent isotopes (primarily U and Th). A freeware application has been developed for determining (U-Th-Sm)/He ages from the raw analytical data and Iolite software was used for U-Pb age and trace element determination. In situ double-dating has successfully replicated conventional U-Pb and (U-Th)/He age variations in xenocrystic zircon from the diamondiferous Ellendale lamproite pipe, Western Australia and increased zircon analytical throughput by a factor of 50 over conventional methods

  3. 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

  4. 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.

  5. Characterization of titanite generations from Gameleira-I deposit (U-anomaly 35) Lagoa Real Uranium Province (LRUP), Bahia state, Brazil

    International Nuclear Information System (INIS)

    Santos, Camila M. dos; Rios, Francisco Javier; Amorim, Lucas E.D.; Palmieri, Helena E.

    2017-01-01

    The Lagoa Real Uranium Province (LRUP) is located in northwest of Bahia state and is the major uranium deposit of Brazil. Titanite is a common accessory mineral in rocks of LRUP and usually is part of uranium ore assemblage. Thirty three polished thin sections of F10 drill-hole located in Gameleira I deposit (anomaly 35) were petrographically studied and used for mineral chemistry study. Petrographically, titanite can be differentiated according to texture between granular and prismatic. Granular titanite is generally associated with magmatic assemblage (alkali feldspar hypersolvus granite) and it is present in some albitites (barren magnetite albitite). Prismatic titanite is restricted to albitite (garnet and mineralized magnetite albitite) and is associated with metamorphic assemblage. Microprobe analyses shows a trend from granites to mineralized albitites and do not cluster titanite by its texture, but by its host rocks. On the other hand, trace elements can distinguish titanite generation according to texture. Granular titanite is characterized by some highest high field strength elements (HFSE) values, like Hf, Pb, Th, U and HREE+Y, and the lowest V content. Vanadium has positive correlation with Zr/Hf ratio and inverse with U. Vanadium versus U relationship is inverse to the previously found by literature in LRUP what indicates that titanite was submitted to complexes processes of uranium loss after its crystallization. In addition, hafnium loss can be related to precipitation of hydrothermal zircon as it is strongly partitioned to this mineral. (author)

  6. Characterization of titanite generations from Gameleira-I deposit (U-anomaly 35) Lagoa Real Uranium Province (LRUP), Bahia state, Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Santos, Camila M. dos; Rios, Francisco Javier; Amorim, Lucas E.D.; Palmieri, Helena E., E-mail: cms@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2017-11-01

    The Lagoa Real Uranium Province (LRUP) is located in northwest of Bahia state and is the major uranium deposit of Brazil. Titanite is a common accessory mineral in rocks of LRUP and usually is part of uranium ore assemblage. Thirty three polished thin sections of F10 drill-hole located in Gameleira I deposit (anomaly 35) were petrographically studied and used for mineral chemistry study. Petrographically, titanite can be differentiated according to texture between granular and prismatic. Granular titanite is generally associated with magmatic assemblage (alkali feldspar hypersolvus granite) and it is present in some albitites (barren magnetite albitite). Prismatic titanite is restricted to albitite (garnet and mineralized magnetite albitite) and is associated with metamorphic assemblage. Microprobe analyses shows a trend from granites to mineralized albitites and do not cluster titanite by its texture, but by its host rocks. On the other hand, trace elements can distinguish titanite generation according to texture. Granular titanite is characterized by some highest high field strength elements (HFSE) values, like Hf, Pb, Th, U and HREE+Y, and the lowest V content. Vanadium has positive correlation with Zr/Hf ratio and inverse with U. Vanadium versus U relationship is inverse to the previously found by literature in LRUP what indicates that titanite was submitted to complexes processes of uranium loss after its crystallization. In addition, hafnium loss can be related to precipitation of hydrothermal zircon as it is strongly partitioned to this mineral. (author)

  7. Bioaccessibility of U, Th and Pb in particulate matter from an abandoned uranium mine

    Science.gov (United States)

    Millward, Geoffrey; Foulkes, Michael; Henderson, Sam; Blake, William

    2016-04-01

    Currently, there are approximately 150 uranium mines in Europe at various stages of either operation, development, decommissioning, restoration or abandonment (wise-uranium.com). The particulate matter comprising the mounds of waste rock and mill tailings poses a risk to human health through the inadvertent ingestion of particles contaminated with uranium and thorium, and their decay products, which exposes recipients to the dual toxicity of heavy elements and their radioactive emissions. We investigated the bioaccessibility of 238U, 232Th and 206,214,210Pb in particulate samples taken from a contaminated, abandoned uranium mine in South West England. Sampling included a mine shaft, dressing floor and waste heap, as well as soils from a field used for grazing. The contaminants were extracted using the in-vitro Unified Bioaccessibility Research Group of Europe Method (UBM) in order to mimic the digestion processes in the human stomach (STOM) and the combined stomach and gastrointestinal tract (STOM+INT). Analyses of concentrations of U, Th and Pb in the extracts were by ICP-MS and the activity concentrations of radionuclides were determined on the same particles, before and after extraction, using gamma spectroscopy. 'Total' concentrations of U, Th and Pb for all samples were in the range 57 to 16,200, 0.28 to 3.8 and 69 to 4750 mg kg-1, respectively. For U and Pb the concentrations in the STOM fraction were lower than the total and STOM+INT fractions were even lower. However, for Th the STOM+INT fractions were higher than the STOM due to the presence of Th carbonate species within the gastrointestinal fluid. Activity concentrations for 214Pb and 210Pb, including total, STOM and STOM+INT, were in the range 180 to samples were 39% and 8% in the STOM and STOM+INT, respectively, whereas the respective BAFs for 232Th were 3% and 9%. For stable 206Pb the STOM and STOM+INT BAFs were 16% and 3% for the most contaminated samples, whereas those from the field had 44% in the

  8. Two modes of orogenic collapse of the Pamir plateau recorded by titanite

    Science.gov (United States)

    Stearns, M. A.; Hacker, B. R.; Ratschbacher, L.; Rutte, D.; Kylander-Clark, A. R.

    2013-12-01

    Processes that operate in the mid- to lower crust during and following continent-continent collision are important for understanding how orogenic plateaux transition from thickening to collapse. In the central and southern Pamir, mid- to lower crustal rocks crop out in two belts of extensional domes. The central Pamir domes were exhumed by symmetrical N-S extension. In contrast, the southern Pamir domes were exhumed by asymmetrical top to the south (NNW-SSE) extension via a rolling-hinge detachment. To investigate the high-temperature exhumation history, titanites were dated using LASS (laser ablation split stream-ICP-MS). A multi-collector ICP was used to collect U-Pb isotopic ratios and a single collector ICP-MS was used to measure trace-element abundances. The data indicate that the central Pamir domes began exhumation synchronously at ~17 Ma. Titanite from the southern Pamir record two periods of protracted (re)crystallization: older metamorphic dates ranging from ~35-18 Ma and younger igneous and metamorphic dates from ~15-7 Ma. Samples with single populations of titanite dates are present throughout both groups. Samples with more-complex date populations typically have distinct trace-element (e.g., Sr, Y, Zr, and Nb) groups that can be used to distinguish different date populations (e.g., older dates may have higher Zr and younger dates lower Zr). The distinct early exhumation histories of the north and south Pamir require either a diachronous single process or two semi-independent processes. The N to S sequence of exhumation, ranges of dates, and overall extension directions may be related to two important plate-tectonic events inferred from seismic data: 1) breakoff of the northward subducting Indian slab around ~20 Ma, and 2) southward subduction and northwestward rollback of the Asian lithosphere between ~15-10 Ma based on geodetic convergence rates and Benioff zone length. We interpret these two lithospheric-detachment events to have driven the

  9. 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)

  10. LA-ICP-MS U-Pb apatite dating of Lower Cretaceous rocks from teschenite-picrite association in the Silesian Unit (southern Poland

    Directory of Open Access Journals (Sweden)

    Szopa Krzysztof

    2014-08-01

    Full Text Available The main products of volcanic activity in the teschenite-picrite association (TPA are shallow, sub-volcanic intrusions, which predominate over extrusive volcanic rocks. They comprise a wide range of intrusive rocks which fall into two main groups: alkaline (teschenite, picrite, syenite, lamprophyre and subalkaline (dolerite. Previous 40Ar/39Ar and 40K/40Ar dating of these rocks in the Polish Outer Western Carpathians, performed on kaersutite, sub-silicic diopside, phlogopite/biotite as well as on whole rock samples has yielded Early Cretaceous ages. Fluorapatite crystals were dated by the U-Pb LA-ICP-MS method to obtain the age of selected magmatic rocks (teschenite, lamprophyre from the Cieszyn igneous province. Apatite-bearing samples from Boguszowice, Puńców and Lipowa yield U-Pb ages of 103± 20 Ma, 119.6 ± 3.2 Ma and 126.5 ± 8.8 Ma, respectively. The weighted average age for all three samples is 117.8 ± 7.3 Ma (MSWD = 2.7. The considerably smaller dispersion in the apatite ages compared to the published amphibole and biotite ages is probably caused by the U-Pb system in apatite being less susceptible to the effects of hydrothermal alternation than the 40Ar/39Ar or 40K/40Ar system in amphibole and/or biotite. Available data suggest that volcanic activity in the Silesian Basin took place from 128 to 103 Ma with the the main magmatic phase constrained to 128-120 Ma.

  11. Standard practice for the determination of 237Np, 232Th, 235U and 238U in urine by inductively coupled plasma-Mass spectrometry (ICP-MS) and gamma ray spectrometry.

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2005-01-01

    1.1 This practice covers the separation and preconcentration of neptunium-237 (237Np), thorium-232 (232Th), uranium-235 (235U) and uranium-238 (238U) from urine followed by quantitation using ICP-MS. 1.2 This practice can be used to support routine bioassay programs. The minimum detectable concentrations (MDC) for this method, taking the preconcentration factor into account, are approximately 1E-2Bq for 237Np (0.38ng), 2E-6Bq for 232Th (0.50ng), 4E-5Bq for 235U (0.50ng) and 6E-6Bq for 238U (0.48ng). 1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

  12. Determination of trace element concentrations and stable lead, uranium and thorium isotope ratios by quadrupole-ICP-MS in NORM and NORM-polluted sample leachates

    International Nuclear Information System (INIS)

    Mas, J.L.; Villa, M.; Hurtado, S.; García-Tenorio, R.

    2012-01-01

    Highlights: ► Polluted sediment and NORM samples. ► An efficient yet fast process allowing multi-parametric determinations in 206 Pb/ 207 Pb/ 208 Pb, 238 U/ 234 U and 232 Th/ 230 Th isotope ratios using a single sample aliquot and a single instrument (ICP-QMS). Eichrom UTEVA ® 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.

  13. Textures, trace element compositions, and U-Pb ages of titanite from the Mangling granitoid pluton, East Qinling Orogen: Implications for magma mixing and destruction of the North China Craton

    Science.gov (United States)

    Hu, Hao; Li, Jian-Wei; McFarlane, Christopher R. M.; Luo, Yan; McCarron, Travis

    2017-07-01

    The Mangling granitoid pluton, located along the southern margin of the North China Craton, consists mainly of monzogranite with minor amounts of diorite. The monzogranite contains abundant mafic microgranular enclaves (MMEs) and is intruded by numerous mafic dikes, providing an opportunity to study magma mixing and its role in the formation of the granitioid pluton. In this paper, we present in situ analysis of U-Pb isotopes and trace element compositions of titanite from the MMEs and the host monzogranite using Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry to document the role of magma mixing in the formation of the Mangling granitoid pluton. Titanite grains from the MMEs (type 1) are euhedral with patchy zoning, whereas the varieties from the closely associated host monzogranite are euhedral and consist of two types (type 2 and type 3). Type 2 titanite is more abundant and has oscillatory zoning without Fe-Ti oxide inclusions, whereas type 3 grains commonly have Fe-Ti oxide inclusions in the core that is rimmed by inclusion-free overgrowths with weak oscillatory zoning. Titanite from monzogranite without MMEs (type 4) is euhedal and has weak oscillatory zoning, with rare ilmenite inclusions in the core. Titanite from a mafic dike intruding the monzogranite (type 5) is anhedral and has sector zoning. Titanite grains from MMEs and the monzogranite (type 1, 2 and 3) have U-Pb ages that are indistinguishable (149 ± 1 Ma, 148 ± 1 Ma and 148 ± 2 Ma, respectively). These ages agree well with zircon U-Pb ages of 150 ± 1 Ma, 150 ± 1 Ma and 149 ± 1 Ma for the MMEs, host monzogranite, and mafic dike, respectively. The age consistency thus confirms coeval formation of the MMEs, the host monzogranite, and the mafic dikes, demonstrating a mafic magmatic, rather than extraneous or restitic origin for the MMEs. Titanite grains from the MMEs (type 1) and mafic dike (type 5) have much lower Al2O3, REE, Nb/Zr, Y/Zr, and Lu/Hf, but higher (Ce + Nd)/Y and La

  14. Relics of continental lithosphere in the atlantic by data of (Th/U)th, (Th/U)pb, and K/Ti systematics

    International Nuclear Information System (INIS)

    Titayeva, N.A.; Mironov, Y.

    1996-01-01

    The problem of mantle heterogeneity of the Atlantic Ocean has been investigated. Th/U ratio is a sensitive geochemical tracer. This ratio can be calculated from 232Th/230Th or from 208Pb/206Pb since 230Th and 206Pb are decay product of 238U and 208Pb is a product of 232Th decay. The former way to get Th/U ratio is valid for quaternary volcanic rocks because of the relatively short 230Th half life (80000 years), the latter way gives an integral quantity characterizing the pre-oceanic history beginning from the onset of earth formation and ending about 150 million years ago. Clear distinctions between ''depleted oceanic'' and ''enriched continental'' reservoirs have been drawn from comparative analysis of rocks. (A.C.)

  15. 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

  16. 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.

  17. 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.

  18. From opening to subduction of an oceanic domain constrained by LA-ICP-MS U-Pb zircon dating (Variscan belt, Southern Armorican Massif, France)

    Science.gov (United States)

    Paquette, J.-L.; Ballèvre, M.; Peucat, J.-J.; Cornen, G.

    2017-12-01

    In the Variscan belt of Western Europe, the lifetime and evolution of the oceanic domain is poorly constrained by sparse, outdated and unreliable multigrain ID-TIMS U-Pb zircon dating. In this article, we present a complete in situ LA-ICP-MS dataset of about 300 U-Pb zircon analyses obtained on most of the ophiolitic and eclogitic outcrops of Southern Brittany, comprising new dating of previously published zircon populations and newly discovered rock samples. In situ dating and cathodo-luminescence imaging of each zircon grain yields new absolute time-constraints on the evolution of the Galicia-Moldanubian Ocean. The new results confirm that the opening of this oceanic domain is well defined at about 490 Ma. In contrast, the generally-quoted 400-410 Ma-age for the high-pressure event related to the subduction of the oceanic crust is definitely not recorded in the zircons of the eclogites. In light of these new data, we propose that the obduction of oceanic rocks occurred at about 370-380 Ma while the high-pressure event is recorded at 355 Ma in only a few zircon grains of some eclogite samples. Additionally, this large scale dating project demonstrates that the zircons from eclogites do not systematically recrystallise during the high pressure event and consequently their U-Pb systems do not record that metamorphism systematically. These zircons rather preserve the isotopic memory of the magmatic crystallization of their igneous protolith. Another example of an eclogite sample from the French Massif Central illustrates the frequent mistake in the interpretation of the ages of the early hydrothermal alteration of zircons in the oceanic crust versus partial or complete recrystallization during eclogite facies metamorphism.

  19. 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)

  20. 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.

  1. An integrated automatic system to evaluate U and Th dynamic lixiviation from solid matrices, and to extract/pre-concentrate leached analytes previous ICP-MS detection.

    Science.gov (United States)

    Ceballos, Melisa Rodas; García-Tenorio, Rafael; Estela, José Manuel; Cerdà, Víctor; Ferrer, Laura

    2017-12-01

    Leached fractions of U and Th from different environmental solid matrices were evaluated by an automatic system enabling the on-line lixiviation and extraction/pre-concentration of these two elements previous ICP-MS detection. UTEVA resin was used as selective extraction material. Ten leached fraction, using artificial rainwater (pH 5.4) as leaching agent, and a residual fraction were analyzed for each sample, allowing the study of behavior of U and Th in dynamic lixiviation conditions. Multivariate techniques have been employed for the efficient optimization of the independent variables that affect the lixiviation process. The system reached LODs of 0.1 and 0.7ngkg -1 of U and Th, respectively. The method was satisfactorily validated for three solid matrices, by the analysis of a soil reference material (IAEA-375), a certified sediment reference material (BCR- 320R) and a phosphogypsum reference material (MatControl CSN-CIEMAT 2008). Besides, environmental samples were analyzed, showing a similar behavior, i.e. the content of radionuclides decreases with the successive extractions. In all cases, the accumulative leached fraction of U and Th for different solid matrices studied (soil, sediment and phosphogypsum) were extremely low, up to 0.05% and 0.005% of U and Th, respectively. However, a great variability was observed in terms of mass concentration released, e.g. between 44 and 13,967ngUkg -1 . Copyright © 2017 Elsevier B.V. All rights reserved.

  2. 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

  3. 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)

  4. 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)

  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. 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)

  7. 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.

  8. 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)

  9. 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)

  10. 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

  11. 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

  12. 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.

  13. 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...

  14. 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

  15. 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.

  16. 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.

  17. Detrital zircon U-Pb and (U-Th)/He double-dating of Upper Cretaceous-Cenozoic Zagros foreland basin strata in the Kurdistan Region of northern Iraq

    Science.gov (United States)

    Barber, D. E.; Stockli, D. F.; Koshnaw, R. I.; Horton, B. K.; Tamar-Agha, M. Y.; Kendall, J. J.

    2014-12-01

    The NW Zagros orogen is the result of the multistage collisional history associated with Late Cretaceous-Cenozoic convergence of the Arabian and Eurasian continents and final closure of Neotethys. Siliciclastic strata preserved within a ~400 km segment of the NW Zagros fold-thrust belt and foreland basin in the Iraqi Kurdistan Region (IKR) provide a widespread record of exhumation and sedimentation. As a means of assessing NW Zagros foreland basin evolution and chronostratigraphy, we present coupled detrital zircon (DZ) U-Pb and (U-Th)/He geo-thermochronometric data of Upper Cretaceous to Pliocene siliciclastic strata from the Duhok, Erbil, and Suleimaniyah provinces of IKR. LA-ICP-MS U-Pb age analyses reveal that the foreland basin fill in IKR in general was dominantly derived from Pan-African/Arabian-Nubian, Peri-Gondwandan, Eurasian, and Cretaceous volcanic arc terrenes. However, the provenance of these strata varies systematically along strike and through time, with an overall increase in complexity upsection. DZ age distribution of Paleocene-Eocene strata is dominated by a ~95 Ma grain age population, likely sourced from the Late Cretaceous Hassanbag-Bitlis volcanic arc complex along the northern margin of Arabia. In contrast, DZ U-Pb age distributions of Neogene strata show a major contribution derived from various Eurasian (e.g., Iranian, Tauride, Pontide; ~45, 150, 300 Ma) and Pan-African (~550, 950 Ma) sources. The introduction of Eurasian DZ ages at the Paleogene-Neogene transition likely records the onset of Arabian-Eurasian collision. Along strike to the southeast, the DZ U-Pb spectra of Neogene strata show a decreased percentage of Pan-African, Peri-Gondwandan, Tauride, and Ordovician ages, coupled with a dramatic increase in 40-50 Ma DZ ages that correspond to Urumieh-Dokhtar magmatic rocks in Iran. Combined with paleocurrent data, this suggests that Neogene sediments were transported longitudinally southeastward through an unbroken foreland basin

  18. 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

  19. 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

  20. High temperature (>350 °C) thermal histories of the long lived (>500 Ma) active margin of Ecuador and Colombia: Apatite, titanite and rutile U-Pb thermochronology

    Science.gov (United States)

    Paul, Andre N.; Spikings, Richard A.; Ulianov, Alexey; Ovtcharova, Maria

    2018-05-01

    Quantitative reconstruction of thermal histories can be a powerful tool to study numerous natural processes such as tectonic plate interaction, cratonic stability and extra-terrestrial phenomena such as asteroid ejection. A majority of thermochronological studies have focused on temperatures lower than 300 °C. Few previous studies have demonstrated that U-Pb data from apatite and other accessory phases can be used to recover thermal history information at T > 350 °C. We present U-Pb data from apatite, to constrain the thermal histories of Triassic peralluminous anatectites from the Northern Andes between the temperatures of ∼350-550 °C. The accuracy of the thermal history models is assessed by comparisons with previous geological models, and comparisons with pre-existing and newly acquired U/Pb (titanite and rutile), 40Ar/39Ar (muscovite) and low temperature thermochronological data. This study also examines the feasibility of using a large, regionally dispersed apatite U-Pb data set to obtain continuous thermal history paths along a long-lived (>500 Ma) active margin. A second aim of this study is to further test the hypothesis that the dominant mechanism for Pb displacement through apatite is volume diffusion, as opposed to aqueous fluid interaction. The thermal history models derived from the Triassic anatectites exposed in the Andes of Colombia and Ecuador are entirely consistent with lower temperature thermochronological constraints, and previously established geochronological and geochemical constraints. They reveal and quantify trench parallel changes in the amount of Jurassic - Early Cretaceous extension, significantly bolstering and adding to previous tectonic interpretations. Confirmation of the utility of U-Pb thermochronology provides geologists with a powerful tool for investigating the high-temperature thermal evolution of accessory minerals.

  1. 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.

  2. 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)

  3. U, Th, and Pb isotopes in hot springs on the Juan de Fuca Ridge

    International Nuclear Information System (INIS)

    Chen, J.H.

    1987-01-01

    The concentrations and isotopic compositions of U, Th, and Pb in three hydrothermal fluids from the Juan de Fuca Ridge were determined. The samples consisted of 10.2--57.6% of the pure hydrothermal end-members based on Mg contents. The Pb contents of the samples ranged from 34 to 87 ng/g, U from 1.3 to 3.0 ng/g, and Th from 0.2 to 7.7 pg/g. These samples showed large enrichments of Pb and Th relative to deep-sea water and some depletion of U. They did not show coherent relationships with Mg, however, indicating nonideal mixings between the hot hydrothermal fluids and cold ambient seawater. Particles filtered from these hydrothermal fluids contained significant amounts of Th and Pb which may effectively increase the concentration of these elements in the fluids when acidified. The /sup 234/U//sup 238/U values in all samples show a /sup 234/U enrichment relative to the equilibrium value and have a seawater signature. The Pb isotopic composition of the Juan de Fuca hydrothermal fluids resembles that of 21 0 N East Pacific Rise and has a uniform mid-ocean ridge basalt signature. The hydrothermal systems at oceanic spreading ridges have circulated through a large volume of basalts. Therefore Pb in these fluids may represent the best average value of the local oceanic crust. From the effects of U deposition from seawater to the crust and Pb extraction from rock to the ocean, the U/Pb ratio in the hydrothermally altered oceanic crust may be increased significantly. copyright American Geophysical Union 1987

  4. 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.)

  5. Geologic evolution of the Paraiba do Sul complex, in the central part of the Ribeira belt, based on the geochemistry and U-Pb geochronology studies; Evolucao geologica do complexo Paraiba do Sul, no segmento central da faixa Ribeira, com base em estudos de geoquimica e geocronologia U-Pb

    Energy Technology Data Exchange (ETDEWEB)

    Valladares, Claudia Sayao

    1996-12-31

    Aiming the definition of the Complexo Paraiba do Sul evolution, the work presents a geochronological approach by the U-Pb method, considered appropriate to study polideformed terrains. The minerals used to the U-Pb dating (zircon, titanite and monazite) provides information about the ages of rock generation and the successive geological events the rocks were submitted. The U-Pb geochronological approach is pioneer in the investigated area and two questions referent to the Complexo Paraiba do Sul evolution in the central part of the Ribeira belt, were the aim of this approach. The first of them refers to the crystallization epoch and the gneisses metamorphism, interpreted here like orthogneisses, called Unidade Quirino of the Complexo Paraiba do Sul. The second refers to the metamorphism ages and meta sedimentary unit deformation. Looking for the contribution to the Complexo Paraiba do Sul evolution understanding, this work presents the data based on the geologic map of this area, comprising part of the Folha Volta Redonda (1:50.000), including petrographic, structural and microtectonic studies. It also presents and discusses the results of: 17 U-Pb analysis in zircon and titanite of the Complexo Paraiba do Sul orthogneisses collection; 24 geochemical analysis of major, minor, trace elements and ETR of the same collection; an U-Pb analysis in titanite of the Unidade Sao Joao, 5 U-Pb analysis in titanites and/or monazites of granites and granitoids; 12 geochemical analysis including major, minor and trace elements and ETR, in granites and sills of leucogranites. Finally, the data achieved were integrated with the objective to elaborate an evolutive view of the Complexo Paraiba do Sul 157 refs., 54 figs., 17 tabs.

  6. Geologic evolution of the Paraiba do Sul complex, in the central part of the Ribeira belt, based on the geochemistry and U-Pb geochronology studies; Evolucao geologica do complexo Paraiba do Sul, no segmento central da faixa Ribeira, com base em estudos de geoquimica e geocronologia U-Pb

    Energy Technology Data Exchange (ETDEWEB)

    Valladares, Claudia Sayao

    1997-12-31

    Aiming the definition of the Complexo Paraiba do Sul evolution, the work presents a geochronological approach by the U-Pb method, considered appropriate to study polideformed terrains. The minerals used to the U-Pb dating (zircon, titanite and monazite) provides information about the ages of rock generation and the successive geological events the rocks were submitted. The U-Pb geochronological approach is pioneer in the investigated area and two questions referent to the Complexo Paraiba do Sul evolution in the central part of the Ribeira belt, were the aim of this approach. The first of them refers to the crystallization epoch and the gneisses metamorphism, interpreted here like orthogneisses, called Unidade Quirino of the Complexo Paraiba do Sul. The second refers to the metamorphism ages and meta sedimentary unit deformation. Looking for the contribution to the Complexo Paraiba do Sul evolution understanding, this work presents the data based on the geologic map of this area, comprising part of the Folha Volta Redonda (1:50.000), including petrographic, structural and microtectonic studies. It also presents and discusses the results of: 17 U-Pb analysis in zircon and titanite of the Complexo Paraiba do Sul orthogneisses collection; 24 geochemical analysis of major, minor, trace elements and ETR of the same collection; an U-Pb analysis in titanite of the Unidade Sao Joao, 5 U-Pb analysis in titanites and/or monazites of granites and granitoids; 12 geochemical analysis including major, minor and trace elements and ETR, in granites and sills of leucogranites. Finally, the data achieved were integrated with the objective to elaborate an evolutive view of the Complexo Paraiba do Sul 157 refs., 54 figs., 17 tabs.

  7. 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.

  8. Leaching behavior of U, Mn, Sr, and Pb from different particle-size fractions of uranium mill tailings.

    Science.gov (United States)

    Liu, Bo; Peng, Tongjiang; Sun, Hongjuan

    2017-06-01

    Pollution by the release of heavy metals from tailings constitutes a potential threat to the environment. To characterize the processes governing the release of Mn, Sr, Pb, and U from the uranium mill tailings, a dynamic leaching test was applied for different size of uranium mill tailings samples. Inductively coupled plasma atomic emission spectroscopy (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) were performed to determine the content of Mn, Sr, Pb, and U in the leachates. The release of mobile Mn, Sr, Pb, and U fraction was slow, being faster in the initial stage and then attained a near steady-state condition. The experimental results demonstrate that the release of Mn, Sr, Pb, and U from uranium mill tailings with different size fractions is controlled by a variety of mechanisms. Surface wash-off is the release mechanism for Mn. The main release mechanism of Sr and Pb is the dissolution in the initial leaching stage. For U, a mixed process of wash-off and diffusion is the controlling mechanism.

  9. Timing of metamorphism and exhumation in the Nordøyane ultra-high-pressure domain, Western Gneiss Region, Norway: New constraints from complementary CA-ID-TIMS and LA-MC-ICP-MS geochronology

    Science.gov (United States)

    Butler, J. P.; Jamieson, R. A.; Dunning, G. R.; Pecha, M. E.; Robinson, P.; Steenkamp, H. M.

    2018-06-01

    We present the results of a combined CA-ID-TIMS and LA-MC-ICP-MS U-Pb geochronology study of zircon and associated rutile and titanite from the Nordøyane ultra-high-pressure (UHP) domain in the Western Gneiss Region (WGR) of Norway. The dated samples include 4 eclogite bodies, 2 host-rock migmatites, and 2 cross-cutting pegmatites and leucosomes, all from the island of Harøya. Zircon from a coesite eclogite yielded an age of ca. 413 Ma, interpreted as the time of UHP metamorphism in this sample. Zircon data from the other eclogite bodies yielded metamorphic ages of ca. 413 Ma, 407 Ma, and 406 Ma; zircon trace-element data associated with 413 Ma and 407 Ma ages are consistent with eclogite-facies crystallization. In all of the eclogites, U-Pb dates from zircon cores, interpreted as the times of protolith crystallization, range from ca. 1680-1586 Ma, consistent with Gothian ages from orthogneisses in Nordøyane and elsewhere in the WGR. A zircon core age of ca. 943 Ma from one sample agrees with Sveconorwegian ages of felsic gneisses and pegmatites in the western part of the area. Migmatites hosting the eclogite bodies yielded zircon core ages of ca. 1657-1591 Ma and rim ages of ca. 395-392 Ma, interpreted as the times of Gothian protolith formation and Scandian partial melt crystallization, respectively. Pegmatite in an eclogite boudin neck yielded a crystallization age of ca. 388 Ma, interpreted as the time of melt crystallization. Rutile and titanite from 3 samples (an eclogite and two migmatites) yielded concordant ID-TIMS ages of 378-376 Ma. The results are similar to existing U-Pb data from other Nordøyane eclogites (415-405 Ma). In combination with previous pressure-temperature data from the coesite eclogite, these ages indicate that peak metamorphic conditions of 3 GPa/760 °C were reached ca. 413 Ma, followed by decompression to 1 GPa/810 °C by ca. 397 Ma and cooling below ca. 600 °C by ca. 375 Ma. The results are compatible with protracted UHP

  10. 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.)

  11. U-Th Burial Dates on Ostrich Eggshell

    Science.gov (United States)

    Sharp, W. D.; Fylstra, N. D.; Tryon, C. A.; Faith, J. T.; Peppe, D. J.

    2015-12-01

    Obtaining precise and accurate dates at archaeological sites beyond the range of radiocarbon dating is challenging but essential for understanding human origins. Eggshells of ratites (large flightless birds including ostrich, emu and others) are common in many archaeological sequences in Africa, Australia and elsewhere. Ancient eggshells are geochemically suitable for the U-Th technique (1), which has about ten times the range of radiocarbon dating (>500 rather than 50 ka), making eggshells attractive dating targets. Moreover, C and N isotopic studies of eggshell provide insights into paleovegetation and paleoprecipitation central to assessing past human-environment interactions (2,3). But until now, U-Th dates on ratite eggshell have not accounted for the secondary origin of essentially all of their U. We report a novel approach to U-Th dating of eggshell that explicitly accounts for secondary U uptake that begins with burial. Using ostrich eggshell (OES) from Pleistocene-Holocene east African sites, we have measured U and 232Th concentration profiles across OES by laser ablation ICP-MS. U commonly peaks at 10s to 100s of ppb and varies 10-fold or more across the ~2 mm thickness of OES, with gradients modulated by the layered structure of the eggshell. Common Th is high near the shell surfaces, but low in the middle "pallisade" layer of OES, making it optimal for U-Th dating. We determine U-Th ages along the U concentration gradient by solution ICP-MS analyses of two or more fractions of the pallisade layer. We then estimate OES burial dates using a simple model for diffusive uptake of uranium. Comparing such "U-Th burial dates" with radiocarbon dates for OES calcite from the same shells, we find good agreement in 7 out of 9 cases, consistent with rapid burial and confirming the accuracy of the approach. The remaining 2 eggshells have anomalous patterns of apparent ages that reveal they are unsuitable for U-Th dating, thereby providing reliability criteria innate

  12. Community-based Approaches to Improving Accuracy, Precision, and Reproducibility in U-Pb and U-Th Geochronology

    Science.gov (United States)

    McLean, N. M.; Condon, D. J.; Bowring, S. A.; Schoene, B.; Dutton, A.; Rubin, K. H.

    2015-12-01

    The last two decades have seen a grassroots effort by the international geochronology community to "calibrate Earth history through teamwork and cooperation," both as part of the EARTHTIME initiative and though several daughter projects with similar goals. Its mission originally challenged laboratories "to produce temporal constraints with uncertainties approaching 0.1% of the radioisotopic ages," but EARTHTIME has since exceeded its charge in many ways. Both the U-Pb and Ar-Ar chronometers first considered for high-precision timescale calibration now regularly produce dates at the sub-per mil level thanks to instrumentation, laboratory, and software advances. At the same time new isotope systems, including U-Th dating of carbonates, have developed comparable precision. But the larger, inter-related scientific challenges envisioned at EARTHTIME's inception remain - for instance, precisely calibrating the global geologic timescale, estimating rates of change around major climatic perturbations, and understanding evolutionary rates through time - and increasingly require that data from multiple geochronometers be combined. To solve these problems, the next two decades of uranium-daughter geochronology will require further advances in accuracy, precision, and reproducibility. The U-Th system has much in common with U-Pb, in that both parent and daughter isotopes are solids that can easily be weighed and dissolved in acid, and have well-characterized reference materials certified for isotopic composition and/or purity. For U-Pb, improving lab-to-lab reproducibility has entailed dissolving precisely weighed U and Pb metals of known purity and isotopic composition together to make gravimetric solutions, then using these to calibrate widely distributed tracers composed of artificial U and Pb isotopes. To mimic laboratory measurements, naturally occurring U and Pb isotopes were also mixed in proportions to mimic samples of three different ages, to be run as internal

  13. Lead isotope ratios in lichen samples evaluated by ICP-ToF-MS to assess possible atmospheric pollution sources in Havana, Cuba.

    Science.gov (United States)

    Alvarez, Alfredo Montero; Estévez Alvarez, Juan R; do Nascimento, Clístenes Williams Araújo; González, Iván Pupo; Rizo, Oscar Díaz; Carzola, Lázaro Lima; Torres, Roberto Ayllón; Pascual, Jorge Gómez

    2017-01-01

    Epiphytic lichens, collected from 119 sampling sites grown over "Roistonea Royal Palm" trees, were used to assess the spatial distribution pattern of lead (Pb) and identify possible pollution sources in Havana (Cuba). Lead concentrations in lichens and topsoils were determined by flame atomic absorption spectrophotometry and inductively coupled plasma (ICP) atomic emission spectrometry, respectively, while Pb in crude oils and gasoline samples were measured by ICP-time of flight mass spectrometry (ICP-ToF-MS). Lead isotopic ratios measurements for lichens, soils, and crude oils were obtained by ICP-ToF-MS. We found that enrichment factors (EF) reflected a moderate contamination for 71% of the samples (EF > 10). The 206 Pb/ 207 Pb ratio values for lichens ranged from 1.17 to 1.20 and were a mixture of natural radiogenic and industrial activities (e.g., crude oils and fire plants). The low concentration of Pb found in gasoline (leaded gasoline is no longer used in Cuba.

  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. Geologic evolution of the Paraiba do Sul complex, in the central part of the Ribeira belt, based on the geochemistry and U-Pb geochronology studies

    International Nuclear Information System (INIS)

    Valladares, Claudia Sayao

    1996-01-01

    Aiming the definition of the Complexo Paraiba do Sul evolution, the work presents a geochronological approach by the U-Pb method, considered appropriate to study polideformed terrains. The minerals used to the U-Pb dating (zircon, titanite and monazite) provides information about the ages of rock generation and the successive geological events the rocks were submitted. The U-Pb geochronological approach is pioneer in the investigated area and two questions referent to the Complexo Paraiba do Sul evolution in the central part of the Ribeira belt, were the aim of this approach. The first of them refers to the crystallization epoch and the gneisses metamorphism, interpreted here like orthogneisses, called Unidade Quirino of the Complexo Paraiba do Sul. The second refers to the metamorphism ages and meta sedimentary unit deformation. Looking for the contribution to the Complexo Paraiba do Sul evolution understanding, this work presents the data based on the geologic map of this area, comprising part of the Folha Volta Redonda (1:50.000), including petrographic, structural and microtectonic studies. It also presents and discusses the results of: 17 U-Pb analysis in zircon and titanite of the Complexo Paraiba do Sul orthogneisses collection; 24 geochemical analysis of major, minor, trace elements and ETR of the same collection; an U-Pb analysis in titanite of the Unidade Sao Joao, 5 U-Pb analysis in titanites and/or monazites of granites and granitoids; 12 geochemical analysis including major, minor and trace elements and ETR, in granites and sills of leucogranites. Finally, the data achieved were integrated with the objective to elaborate an evolutive view of the Complexo Paraiba do Sul

  16. History of individuals of the 18th/19th centuries stored in bones, teeth, and hair analyzed by LA-ICP-MS--a step in attempts to confirm the authenticity of Mozart's skull.

    Science.gov (United States)

    Stadlbauer, Christina; Reiter, Christian; Patzak, Beatrix; Stingeder, Gerhard; Prohaska, Thomas

    2007-06-01

    A cranium stored in the Stiftung Mozarteum in Salzburg/Austria which is believed to be that of Mozart, and skeletal remains of suspected relatives which have been excavated from the Mozart family grave in the cemetery in Salzburg, have been subjected to scientific investigations to determine whether or not the skull is authentic. A film project by the Austrian television ORF in collaboration with Interspot Film on this issue was broadcast at the beginning of the "Mozart year 2006". DNA analysis could not clarify relationships among the remains and, therefore, assignment of the samples was not really possible. In our work this skull and excavated skeletal remains have been quantified for Pb, Cr, Hg, As, and Sb content by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) to obtain information about the living conditions of these individuals. A small splinter of enamel (less than 1 mm(3)) from a tooth of the "Mozart cranium" was also available for investigation. Quantification was performed by using spiked hydroxyapatite standards. Single hair samples which are recorded to originate from Mozart have also been investigated by LA-ICP-MS and compared with hair samples of contemporary citizens stored in the Federal Pathologic-Anatomical Museum, Vienna. In general, Pb concentrations up to approximately 16 mug g(-1) were found in the bone samples of 18th century individuals (a factor of 7 to 8 higher than in recent samples) reflecting elevated Pb levels in food or beverages. Elevated Pb levels were also found in hair samples. The amount of Sb in the enamel sample of the "Mozart cranium" (approx. 3 mug g(-1)) was significantly higher than in all the other tooth samples investigated, indicating possible Sb ingestion in early childhood. Elevated concentrations of elements in single hair samples gave additional information about possible exposure of the individuals to heavy metals at a particular point in their life.

  17. 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.

  18. New zircon (U-Th)/He and U/Pb eruption age for the Rockland tephra, western USA

    Science.gov (United States)

    Coble, Matthew A.; Burgess, Seth D.; Klemetti, Erik W.

    2017-09-01

    Eruption ages of a number of prominent Quaternary volcanic deposits remain inaccurately and/or imprecisely constrained, despite their importance as regional stratigraphic markers in paleo-environment reconstruction and as evidence of climate-altering eruptions. Accurately dating volcanic deposits presents challenging analytical considerations, including poor radiogenic yield, scarcity of datable minerals, and contamination of crystal populations by magma, eruption, and transport processes. One prominent example is the Rockland tephra, which erupted from the Lassen Volcanic Center in the southern Cascade arc. Despite a range in published eruption ages from 0.40 to 0.63 Ma, the Rockland tephra is extensively used as a marker bed across the western United States. To more accurately and precisely constrain the age of the Rockland tephra-producing eruption, we report U/Pb crystallization dates from the outermost ∼2 μm of zircon crystal faces (surfaces) using secondary ion mass spectrometry (SIMS). Our new weighted mean 238U/206Pb age for Rockland tephra zircon surfaces is 0.598 ± 0.013 Ma (2σ) and MSWD = 1.11 (mean square weighted deviation). As an independent test of the accuracy of this age, we obtained new (U-Th)/He dates from individual zircon grains from the Rockland tephra, which yielded a weighted mean age of 0.599 ± 0.012 Ma (2σ, MSWD = 5.13). We also obtained a (U-Th)/He age of 0.628 ± 0.014 Ma (MSWD = 1.19) for the Lava Creek Tuff member B, which was analyzed as a secondary standard to test the accuracy of the (U-Th)/He technique for Quaternary tephras, and to evaluate assumptions made in the model-age calculation. Concordance of new U/Pb and (U-Th)/He zircon ages reinforces the accuracy of our preferred Rockland tephra eruption age, and confirms that zircon surface dates sample zircon growth up to the time of eruption. We demonstrate the broad applicability of coupled U/Pb zircon-surface and single-grain zircon (U-Th)/He geochronology to accurate

  19. U-Pb geochronology by La-CIP-MS and petrography of Sao Carlos massif - stanniferous province of Rondonia

    International Nuclear Information System (INIS)

    Debowski, Beatriz P.; Geraldes, Mauro Cesar; Nogueira, Camila; Almeida, Bruna Saar de

    2015-01-01

    U-Pb dating by ICP-MS-LA were performed in four samples of the Massif Sao Carlos massif, representative of the younger Granites of Rondonia belonging to the stanniferous province of the same State. Dated samples are granites of pink in colour and coarse-grained to porphyry with main mineralogy consisting of feldspar pertitic to mesopertitic, quartz, plagioclase in lower proportion, biotite and amphibole in some cases. Ages obtained were 986 ± 14 Ma, 974 ± 10 Ma, ± 8 Ma 992.7 and 996 ± 8 Ma and represent the age of crystallization of the Massif. Such ages are concordant with others reported on the bibliography ratifying the inclusion of the massif in the younger Granites of Rondonia, which are directly associated with the most significant mineralization of cassiterite in the State

  20. 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.

  1. Preliminary Report on U-Th-Pb Isotope Systematics of the Olivine-Phyric Shergottite Tissint

    Science.gov (United States)

    Moriwaki, R.; Usui, T.; Yokoyama, T.; Simon, J. I.; Jones, J. H.

    2014-01-01

    Geochemical studies of shergottites suggest that their parental magmas reflect mixtures between at least two distinct geochemical source reservoirs, producing correlations between radiogenic isotope compositions, and trace element abundances.. These correlations have been interpreted as indicating the presence of a reduced, incompatible-element- depleted reservoir and an oxidized, incompatible-element-rich reservoir. The former is clearly a depleted mantle source, but there has been a long debate regarding the origin of the enriched reservoir. Two contrasting models have been proposed regarding the location and mixing process of the two geochemical source reservoirs: (1) assimilation of oxidized crust by mantle derived, reduced magmas, or (2) mixing of two distinct mantle reservoirs during melting. The former clearly requires the ancient martian crust to be the enriched source (crustal assimilation), whereas the latter requires a long-lived enriched mantle domain that probably originated from residual melts formed during solidification of a magma ocean (heterogeneous mantle model). This study conducts Pb isotope and U-Th-Pb concentration analyses of the olivine-phyric shergottite Tissint because U-Th-Pb isotope systematics have been intensively used as a powerful radiogenic tracer to characterize old crust/sediment components in mantle- derived, terrestrial oceanic island basalts. The U-Th-Pb analyses are applied to sequential acid leaching fractions obtained from Tissint whole-rock powder in order to search for Pb isotopic source components in Tissint magma. Here we report preliminary results of the U-Th-Pb analyses of acid leachates and a residue, and propose the possibility that Tissint would have experienced minor assimilation of old martian crust.

  2. 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)

  3. 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

  4. 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

  5. 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.

  6. 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.)

  7. Analysis of whole human blood for Pb, Cd, Hg, Se, and Mn by ICP-DRC-MS for biomonitoring and acute exposures.

    Science.gov (United States)

    Jones, Deanna R; Jarrett, Jeffery M; Tevis, Denise S; Franklin, Melanie; Mullinix, Neva J; Wallon, Kristen L; Derrick Quarles, C; Caldwell, Kathleen L; Jones, Robert L

    2017-01-01

    We improved our inductively coupled plasma mass spectrometry (ICP-MS) whole blood method [1] for determination of lead (Pb), cadmium (Cd), and mercury (Hg) by including manganese (Mn) and selenium (Se), and expanding the calibration range of all analytes. The method is validated on a PerkinElmer (PE) ELAN® DRC II ICP-MS (ICP-DRC-MS) and uses the Dynamic Reaction Cell (DRC) technology to attenuate interfering background ion signals via ion-molecule reactions. Methane gas (CH 4 ) eliminates background signal from 40 Ar 2 + to permit determination of 80 Se + , and oxygen gas (O 2 ) eliminates several polyatomic interferences (e.g. 40 Ar 15 N + , 54 Fe 1 H + ) on 55 Mn + . Hg sensitivity in DRC mode is a factor of two higher than vented mode when measured under the same DRC conditions as Mn due to collisional focusing of the ion beam. To compensate for the expanded method's longer analysis time (due to DRC mode pause delays), we implemented an SC4-FAST autosampler (ESI Scientific, Omaha, NE), which vacuum loads the sample onto a loop, to keep the sample-to-sample measurement time to less than 5min, allowing for preparation and analysis of 60 samples in an 8-h work shift. The longer analysis time also resulted in faster breakdown of the hydrocarbon oil in the interface roughing pump. The replacement of the standard roughing pump with a pump using a fluorinated lubricant, Fomblin®, extended the time between pump maintenance. We optimized the diluent and rinse solution components to reduce carryover from high concentration samples and prevent the formation of precipitates. We performed a robust calculation to determine the following limits of detection (LOD) in whole blood: 0.07µgdL -1 for Pb, 0.10µgL -1 for Cd, 0.28μgL -1 for Hg, 0.99µgL -1 for Mn, and 24.5µgL -1 for Se. Published by Elsevier B.V.

  8. Improved 206Pb/238U microprobe geochronology by the monitoring of a trace-element-related matrix effect; SHRIMP, ID-TIMS, ELA-ICP-MS and oxygen isotope documentation for a series of zircon standards

    Science.gov (United States)

    Black, L.P.; Kamo, S.L.; Allen, C.M.; Davis, D.W.; Aleinikoff, J.N.; Valley, J.W.; Mundil, R.; Campbell, I.H.; Korsch, R.J.; Williams, I.S.; Foudoulis, C.

    2004-01-01

    Precise isotope dilution-thermal ionisation mass spectrometry (ID-TIMS) documentation is given for two new Palaeozoic zircon standards (TEMORA 2 and R33). These data, in combination with results for previously documented standards (AS3, SL13, QGNG and TEMORA 1), provide the basis for a detailed investigation of inconsistencies in 206Pb/238U ages measured by microprobe. Although these ages are normally consistent between any two standards, their relative age offsets are often different from those established by ID-TIMS. This is true for both sensitive high-resolution ion-microprobe (SHRIMP) and excimer laser ablation-inductively coupled plasma-mass spectrometry (ELA-ICP-MS) dating, although the age offsets are in the opposite sense for the two techniques. Various factors have been investigated for possible correlations with age bias, in an attempt to resolve why the accuracy of the method is worse than the indicated precision. Crystallographic orientation, position on the grain-mount and oxygen isotopic composition are unrelated to the bias. There are, however, striking correlations between the 206Pb/238U age offsets and P, Sm and, most particularly, Nd abundances in the zircons. Although these are not believed to be the primary cause of this apparent matrix effect, they indicate that ionisation of 206Pb/238U is influenced, at least in part, by a combination of trace elements. Nd is sufficiently representative of the controlling trace elements that it provides a quantitative means of correcting for the microprobe age bias. This approach has the potential to reduce age biases associated with different techniques, different instrumentation and different standards within and between laboratories. Crown Copyright ?? 2004 Published by Elsevier B.V. All rights reserved.

  9. 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)

  10. 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)

  11. 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)

  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. 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

  14. Characterization of flux-grown Trace-element-doped titanite using the high-mass-resolution ion microprobe (SHRIMP-RG)

    Science.gov (United States)

    Mazdab, F.K.

    2009-01-01

    Crystals of titanite can be readily grown under ambient pressure from a mixture of CaO, TiO2 and SiO2 in the presence of molten sodium tetraborate. The crystals produced are euhedral and prismatic, lustrous and transparent, and up to 5 mm in length. Titanite obtained by this method contains approximately 4300 ppm Na and 220 ppm B contributed from the flux. In addition to dopant-free material, titanite containing trace alkali and alkaline earth metals (K, Sr, Ba), transition metals (Sc, Cr, Ni, Y, Zr, Nb, Hf and Ta), rare-earth elements (REE), actinides (Th, U) and p-block elements (F, S, Cl, Ge, Sn and Pb) have been prepared using the same procedure. Back-scattered electron (BSE) imaging accompanied by ion-microprobe (SHRIMP-RG) analysis confirms significant incorporation of selected trace-elements at structural sites. Regardless of some zonation, the large size of the crystals and broad regions of chemical homogeneity make these crystals useful as experimental starting material, and as matrix-matched trace-element standards for a variety of microbeam analytical techniques where amorphous titanite glass, heterogeneous natural titanite or a non-titanite standard may be less than satisfactory. Trace-element-doped synthetic crystals can also provide a convenient proxy for a better understanding of trace-element incorporation in natural titanite. Comparisons with igneous, authigenic and high-temperature metasomatic titanite are examined. The use of high-mass-resolution SIMS also demonstrates the analytical challenges inherent to any in situ mass-spectrometry-based analysis of titanite, owing to the production of difficult-to-resolve molecular interferences. These interferences are dominated by Ca-Ca, Ca-Ti and Ti-Ti dimers that are significant in the mass range of 80-100, affecting all isotopes of Sr and Zr, as well as 89Y and 93Nb. Methods do exist for the evaluation of interferences by these dimers and of polyatomic interferences on the LREE.

  15. Simultaneous determination of V, As, Se, Cd, Ba and Pb in coal by ICP-MS after high pressure oxygen combustion

    Energy Technology Data Exchange (ETDEWEB)

    Akiyama, K.; Arikawa, Y. [Japan Womens University, Tokyo (Japan). Graduate School of Science

    2007-04-15

    A simple decomposition procedure by a high pressure oxygen combustion method was employed for the determination of six elements (V, As, Se, Cd, Ba and Pb) in coal by inductively coupled plasma mass spectrometry (ICP-MS). Combustion under 3 MPa pressure of oxygen in a sealed bomb is a simple and effective method for the decomposition of carbonaceous materials. Organic components are burnt to form CO{sub 2} and H{sub 2}O. Other components also form oxides, which are absorbed in the absorbing solution of a 5 mL of 5% HNO{sub 3} - 1% H{sub 2}O1 Mixed solution put in a bomb. To completely decompose the sample, 600 mg of starch is added to 300 mg of a ground coal sample. Though ignition normally takes about s, 30 min is required before opening the bomb to keep to the oxides absorbed into the absorbing solution. The accuracy of the procedure was evaluated by comparing the determination value of each element with a certified value of a standard reference material. In this study, NIST SRM 1632c and 1632b, given by the National Institute for Standards and Technology in Washington DC, USA were used as standard reference materials. The results obtained by ICP-MS after high pressure oxygen combustion showed good agreements with the certified values of NIST 1632c for 6 elements (V, As, Se, Cd, Ba, Pb). This method was applied to the determination of 6 elements in coal real samples supplied by CCUJ (Center of Coal Utilization Japan).

  16. Determination of U, Th and Nb by ICP-MS in biological samples from a group non-occupationally exposed persons

    International Nuclear Information System (INIS)

    Santos, Maristela S.; Juliao, Ligia; Fernandes, Paulo Cesar; Melo, Dunstana; Godoy, Maria Luiza Duarte Pinto; Azeredo, Adelaide

    2001-01-01

    In order to have a good intake assessment for workers, by in vitro bioassay, appropriate methods to determine trace concentrations in urine and feces samples are required. Since the concentration of the radionuclides in the excretion samples of the workers shall be compared to the ones in the excretion samples of the members of the public. The adoption of this procedure is need to evaluate the contribution of the intake through diet ingestion or inhalation of particles in high background radiation areas, which can result in an increasing of the concentration of radionuclides in urine and feces samples due to environmental exposure independent of the occupational exposure. In Brazil, the radionuclides from the uranium and thorium series can be found associated to the ores. In order to carry out an evaluation of the internal contamination in workers from mine industry, specially niobium mine, the optimization of the methodology of the urine and feces sample preparation for determination of U, Th e Nb content using ICP-MS (Inductively Coupled Plasma - Mass Spectrometer) was need. For the feces sample preparation, the sample ash (400 deg C) was the first step, followed by the addition of the nitric, hydrofluoric and perchloric suprapur acids in PTFE recipient covered. The residue was dissolved with 2% nitric acid. For the urine samples, 1-ml aliquot was diluted in 2% nitric acid. A total of 23 feces samples and 25 urine samples from a group of inhabitants of Rio de Janeiro city, including children and adults, were analyzed. The results will be used as reference values in studies of evaluation of intake due to occupational exposure in Brazil. (author)

  17. 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)

  18. 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.)

  19. 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.

  20. 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

  1. 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.

  2. Trace elements (Rb, Cs, Sr, Pb, Th, U) bioavailability potential and speciation in the Piracicaba river bottom sediments, Sao Paulo, Brazil

    International Nuclear Information System (INIS)

    Fernandes, Alexandre Martins; Mortatti, Jefferson; Oliveira, Helder de; Bibian, Joao Paulo Rambelli; Moraes, Graziela Meneghel de; Probst, Jean-Luc

    2007-01-01

    It was studied the bioavailability potential of Rb, Cs, Sr, Pb, Th and U and their chemical speciation in Piracicaba river bottom sediments. This river system crosses important agricultural and urban areas of Sao Paulo state, which groups about 3 million people and receives a large load of agricultural, industrial and domestic wastes. The procedure used to estimate trace elements bioavailability potential was related to a 7-step sequential chemical extraction. This scheme was designed to dissolved and separate sample chemical phases, which can be affected by changes in physical-chemical conditions; in the following order: water soluble, exchangeable, bound to carbonates or acid fraction, bound to Mn-oxides, bound to Fe-oxides and bound to organic matter. Trace element concentrations were determined by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) after each extraction step. With the used extraction procedure, it was possible to identify the fraction where some trace elements could be found in order to evaluate their bioavailability potential. Rb and Cs were particularly involved with the organic fraction, while Sr revealed to be associated mainly to the exchangeable fraction (clay minerals). Pb, Th and U were mainly bound to the residual and Fe-oxide fractions. (author)

  3. Magma Mixing, Mingling and Its Accompanying Isotopic and Elemental Partitioning: Records from Titanites in Guojialing-type Granodiorites and Dioritic Enclaves, Jiaodong, North China

    Science.gov (United States)

    Jiang, P.; Yang, K. F.; Fan, H. R.; Liu, X.

    2016-12-01

    The grain-scale textural and in-situ compositional analyses on accessory minerals (such as titanite, rutile, apatite, monazite, etc.) have recently been a hot topic for geologists, through which a detailed information on magmatic, metamorphic or hydrothermal process can be extracted. As an attempt to unravel the petrogenesis of Early Cretaceous Guojialing-type granodiorites and their bearing dioritic enclaves, we accomplished an integrated geochronological and geochemical study on titanites within these rocks. Three types of titanites, with distinguishable textural and geochemical features, are identified. G-type titanites (from granodiorites) and E-type-I titanites (from plagioclase-rich dioritic enclaves) yield identical U-Pb age of 130 Ma, but reveal distinct back-scattered electron (BSE) zonings. G-type titanites are characterized by oscillatory zonings whereas E-type-I titanites are marked by core-mantle-rim zonings, exhibiting drastic but contrary variation trends for several key elements (such as LREEs, Zr, Hf and F) among their transition BSE zones. These two types of titanites are interpreted to crystallize coevally, and record a notable temperature and compositional change of two corresponding melts, as a response to magma mixing. E-type-II titanites (from plagioclase-poor dioritic enclaves) yield a relatively younger U-Pb age at 128 Ma, and show typical interstitial growth with narrower and lower range of Zr, total REEs contents, but higher F content and Nb/Ta ratios. Such titanites are perceived to record late-stage mingling, during which F-rich and REE-poor hybrid granodioritic magma squeezed into the incompletely consolidated dioritic enclaves with accompanying fluid-rock interaction. Unlike the dramatic elemental changes in these differentiated titanites, in-situ Nd isotopic compositions are relatively homogeneous, which in our view is a good sign of showing that isotopic equilibrium among two magma systems was more easily reached compared to

  4. 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.)

  5. A study on the determination of phosphorus in Th-U matrix by a high resolution spectroanalyser (ICP-AES)

    International Nuclear Information System (INIS)

    Save, Neeta; Kumar, Neeraj; Jaiswal, Rajesh; Ghosh, Seema; Malav, R.K.; Das, D.K.; Prakash, Amrit; Behere, P.G.; Afzal, Mohd

    2013-01-01

    Phosphorus is present as an impurity in Thoria and constitutes an important chemical specification of the Thoria based fuel. The present paper depicts the importance of determination of phosphorus, which forms an important quality control step during the fabrication of mixed oxide (Th-U)O 2 pellet. A high resolution spectroanalyser using ICP-AES has been used for the determination of Phosphorus in (ThO 2 -3.25%UO 2 ). (author)

  6. Analysis of plutonium isotope ratios including 238Pu/239Pu in individual U-Pu mixed oxide particles by means of a combination of alpha spectrometry and ICP-MS.

    Science.gov (United States)

    Esaka, Fumitaka; Yasuda, Kenichiro; Suzuki, Daisuke; Miyamoto, Yutaka; Magara, Masaaki

    2017-04-01

    Isotope ratio analysis of individual uranium-plutonium (U-Pu) mixed oxide particles contained within environmental samples taken from nuclear facilities is proving to be increasingly important in the field of nuclear safeguards. However, isobaric interferences, such as 238 U with 238 Pu and 241 Am with 241 Pu, make it difficult to determine plutonium isotope ratios in mass spectrometric measurements. In the present study, the isotope ratios of 238 Pu/ 239 Pu, 240 Pu/ 239 Pu, 241 Pu/ 239 Pu, and 242 Pu/ 239 Pu were measured for individual Pu and U-Pu mixed oxide particles by a combination of alpha spectrometry and inductively coupled plasma mass spectrometry (ICP-MS). As a consequence, we were able to determine the 240 Pu/ 239 Pu, 241 Pu/ 239 Pu, and 242 Pu/ 239 Pu isotope ratios with ICP-MS after particle dissolution and chemical separation of plutonium with UTEVA resins. Furthermore, 238 Pu/ 239 Pu isotope ratios were able to be calculated by using both the 238 Pu/( 239 Pu+ 240 Pu) activity ratios that had been measured through alpha spectrometry and the 240 Pu/ 239 Pu isotope ratios determined through ICP-MS. Therefore, the combined use of alpha spectrometry and ICP-MS is useful in determining plutonium isotope ratios, including 238 Pu/ 239 Pu, in individual U-Pu mixed oxide particles. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. 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.)

  8. 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.

  9. 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.)

  10. 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.

  11. Determination of Cd, Hg, Pb and Se in sediments slurries by isotopic dilution calibration ICP-MS after chemical vapor generation using an on-line system or retention in an electrothermal vaporizer treated with iridium

    International Nuclear Information System (INIS)

    Vieira, Mariana Antunes; Ribeiro, Anderson Schwingel; Dias, Lucia Felicidade; Curtius, Adilson Jose

    2005-01-01

    A method for the determination of Cd, Hg, Pb and Se in sediments reference materials by slurry sampling chemical vapor generation (CVG) using isotopic dilution (ID) calibration and detection by inductively coupled plasma mass spectrometry (ICP-MS) is proposed. Two different systems were used for the investigation: an on-line flow injection system (FI-CVG-ICP-MS) and an off-line system with in situ trapping electrothermal vaporization (CVG-ETV-ICP-MS). About 100 mg of the reference material, ground to a particle size ≤50 μm, was mixed with acid solutions (aqua regia, HF and HCl) in an ultrasonic bath. The enriched isotopes 111 Cd, 198 Hg, 206 Pb and 77 Se were then added to the slurry in an adequate amount in order to produce an altered isotopic ratio close to 1. For the on-line system, a standing time for the slurry of 12 h before measurement was required, while for the batch system, no standing time is needed to obtain accurate results. The conditions for the formation of the analyte vapor were optimized for the evaluated systems. The following altered isotope ratios were measured: 111 Cd/ 114 Cd, 198 Hg/ 199 Hg, 206 Pb/ 208 Pb e 77 Se/ 82 Se. The obtained detection limits in the on-line system, in μg g -1 , were: Cd: 0.15; Hg: 0.09; Pb: 6.0 and Se: 0.03. Similar detection limits were obtained with the system that uses the ETV: 0.21 for Hg, 6.0 for Pb and 0.06 μg g -1 for Se. No signal for Cd was obtained in this system. One estuarine, two marine and two river certified sediments were analyzed to check the accuracy. The obtained values by both systems were generally in agreement with the certified concentrations, according to the t-test for a confidence level of 95%, demonstrating that isotope equilibration was attained in the slurries submitted to a chemical vapor generation procedure and detection by ICP-MS. The relative standard deviations were lower than 10%, adequate for slurry analysis. The almost quantitative analytes extractions to the aqueous phase

  12. 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.

  13. 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.)

  14. 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)

  15. Trace metals analysis in estuarine and seawater by ICP-MS using on line preconcentration and matrix elimination with chelating resin.

    Science.gov (United States)

    Nicolaı, M; Rosin, C; Tousset, N; Nicolai, Y

    1999-09-13

    The main difficulties of trace metals analysis in estuarine and seawater stem from their very low concentration (mug/l to sub-mug/l), and, by contrast, the high salt content (up to 38 g/l in the Mediterranean Sea). ICP-MS allows multi-elemental analysis and offers great sensitivity, but may be strongly affected by matrix effects induced by high salt contents (> 1 g/l). To perform trace metals analysis both in riverine, estuarine and seawater, we have developed a hyphenated method: ion chelation chromatography coupled on-line with ICP-MS. Iminodiacetate resin, Metpac CC-1 (Dionex), was used to concentrate most of the trace metals, and to separate them from alkaline and alkaline-earth metals. Behaviour of 17 elements (Pb, Cu, Cd, Ni, U, Cr, Mn, Al, Co, Ga, In, Zn, V, Tl, Bi, Ag and Sn) towards the resin was qualitatively investigated. A method validation, partly derived from AFNOR standard XPT 90-210, was carried out on 12 elements (Pb, Cu, Cd, Ni, U, Cr, Mn, Al, Co, Ga, Bi and In). Replicate measurements of multi-elemental standard solutions were used to check linearity, and to determine repeatability and detection limits. Method accuracy was then assessed by analysing two certified materials: a synthetic freshwater (SRM 1643d), and a natural filtered coastal seawater (NRCC CASS-3). An application assay of natural samples from the Rhône river (France) was eventually carried out, and the analytical results were found to be consistent with previous works.

  16. 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.

  17. 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...

  18. 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.)

  19. 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.

  20. Determination of uranium isotopes (235U, 238U) and trace elements (Cd, Pb, Cu and As) in bottled drinking water by Icp-SFMS

    International Nuclear Information System (INIS)

    Lara A, N.; Hernandez M, H.; Romero G, E. T.; Kuri de la C, A.; Perez B, M. A.

    2016-09-01

    In the present work we propose an optimized method for the quantification of uranium isotopes ( 235 U, 2 38 U) and the elements Cd, Pb, Cu and As in bottled water for drinking at trace levels of concentration. Based on the multi-element detection capability, the high sensitivity and resolution that the Mass Spectrometry with Magnetic Sector with Inductively Coupled Plasma Source (Icp-SFMS) technique offers; the high, medium and low resolution analysis conditions for the elements under study were established and optimized using and Element 2/Xr equipment and the 23 multi-elemental Certified Reference Material (CRM). The analysis method was validated using the standard reference material Nist 1643d and CRM mono-elemental s as external standards for the quantification of the analytes. Samples, targets and CRM were acidified with 2% of HNO 3 and analyzed without pretreatment under the established analysis conditions. The results obtained show concentrations of 235 U, 238 U, 111 Cd, 208 Pb, 63 Cu and 75 As in the range of μg L -1 , the linearity obtained from the calibration curves for each element has correlation coefficients < 0.99 in all cases, the accuracy of the method in terms of percent relative standard deviation (RSD %) was less than 5%, the mean recovery rate of Nist 1643d ranged from 96.46% to 101.12%. The optimization of the method guarantees the stability and calibration of the equipment throughout the analysis, as well as the ability to resolve interferences. In conclusion, the method proposed using Icp-SFMS offers the advantages of being fast and simple for the multi-elemental analysis in water at trace levels, with low limits of quantification and detection, with good linearity, accuracy, precision and reproducibility to a degree of reliability of 95%. (Author)

  1. The Wall-Rock Record of Incremental Emplacement in the Little Cottonwood-Alta Magmatic and Hydrothermal System, Wasatch Mountains, Utah, U.S.A.

    Science.gov (United States)

    Stearns, M.; Callis, S.; Beno, C.; Bowman, J. R.; Bartley, J. M.

    2017-12-01

    Contact aureoles record the cumulative effects on wall rocks of magma emplacement. Like the plutons they surround, contact aureoles have long been regarded to form geologically instantaneously. Protracted incremental emplacement of plutons must be reconciled with the wall-rock record of heat and mass transfer. Fundamental questions include how heat and material move from intrusions into their aureoles and how long that process takes. The Little Cottonwood stock is surrounded by a 2 km-wide contact aureole that contains prograde AFM mineral assemblages in the pelitic layers of the Proterozoic Big Cottonwood Formation. The Alta stock is surrounded by a well characterized 1 km-wide contact aureole containing both prograde AFM and CMS mineral assemblages in Ophir Shale and Mississippian dolostones, respectively. Understanding the petrogenesis of these aureoles requires the timing of magmatism and wall-rock metamorphism to be independently determined. Preliminary petrochronology (U/Th-Pb dates and trace element concentrations collected by LASS-ICP-MS) from the inner aureoles of both intrusions establishes a protracted history of monazite (re)crystallization from 35-25 Ma in the Little Cottonwood aureole and 35 Ma in the Alta aureole. Little Cottonwood aureole monazites are characterized by a positive age correlation with heavy rare earth elements (HREE) and a negative correlation with Eu/Eu*. Alta aureole monazites have a similar range of the HREE concentrations and Eu/Eu* variation. Zircon growth interpreted to record emplacement-level magmatic crystallization of the western Little Cottonwood stock ranges from 33-28 Ma near the contact. Multi-grain U-Pb zircon TIMS dates from the Alta stock range from 35-33 Ma and are interpreted to suggest the full range of emplacement-level magmatism in the Alta stock. Additionally, in situ U-Pb titanite dates from the Alta stock record intermittent high temperature hydrothermal activity in the stock margin from 35-24 Ma. These new

  2. Determination of uranium isotopes ({sup 235}U, {sup 238}U) and trace elements (Cd, Pb, Cu and As) in bottled drinking water by Icp-SFMS; Determinacion de isotopos de uranio ({sup 235}U, {sup 238}U) y elementos traza (Cd, Pb, Cu y As) en agua embotellada para beber por ICP-SFMS

    Energy Technology Data Exchange (ETDEWEB)

    Lara A, N.; Hernandez M, H.; Romero G, E. T.; Kuri de la C, A.; Perez B, M. A., E-mail: nancy.lara@inin.gob.mx [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico)

    2016-09-15

    In the present work we propose an optimized method for the quantification of uranium isotopes ({sup 235}U, 2{sup 38}U) and the elements Cd, Pb, Cu and As in bottled water for drinking at trace levels of concentration. Based on the multi-element detection capability, the high sensitivity and resolution that the Mass Spectrometry with Magnetic Sector with Inductively Coupled Plasma Source (Icp-SFMS) technique offers; the high, medium and low resolution analysis conditions for the elements under study were established and optimized using and Element 2/Xr equipment and the 23 multi-elemental Certified Reference Material (CRM). The analysis method was validated using the standard reference material Nist 1643d and CRM mono-elemental s as external standards for the quantification of the analytes. Samples, targets and CRM were acidified with 2% of HNO{sub 3} and analyzed without pretreatment under the established analysis conditions. The results obtained show concentrations of {sup 235}U, {sup 238}U, {sup 111}Cd, {sup 208}Pb, {sup 63}Cu and {sup 75}As in the range of μg L{sup -1}, the linearity obtained from the calibration curves for each element has correlation coefficients < 0.99 in all cases, the accuracy of the method in terms of percent relative standard deviation (RSD %) was less than 5%, the mean recovery rate of Nist 1643d ranged from 96.46% to 101.12%. The optimization of the method guarantees the stability and calibration of the equipment throughout the analysis, as well as the ability to resolve interferences. In conclusion, the method proposed using Icp-SFMS offers the advantages of being fast and simple for the multi-elemental analysis in water at trace levels, with low limits of quantification and detection, with good linearity, accuracy, precision and reproducibility to a degree of reliability of 95%. (Author)

  3. 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

  4. 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)

  5. 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)

  6. 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.

  7. 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

  8. 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)

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. Crustal melting and recycling: geochronology and sources of Variscan syn-kinematic anatectic granitoids of the Tormes Dome (Central Iberian Zone). A U-Pb LA-ICP-MS study

    Science.gov (United States)

    López-Moro, F. J.; López-Plaza, M.; Gutiérrez-Alonso, G.; Fernández-Suárez, J.; López-Carmona, A.; Hofmann, M.; Romer, R. L.

    2018-04-01

    In this study, we report U-Pb Laser Ablation ICP-MS zircon and ID-TIMS monazite ages for peraluminous granitoid plutons (biotite ± muscovite ± cordierite ± sillimanite) in the Tormes Dome, one of the gneiss-cored domes located in the Central Iberian Zone of the Variscan belt of northern Spain. Textural domains in zircon, interpreted to represent the magmatic crystallization of the granitoids (and one monazite fraction in the Ledesma pluton) yielded ages around 320 Ma, in agreement with other geochronological studies in the region. This age is interpreted to date the timing of decompression crustal melting driven by the extensional collapse of the orogenic belt in this domain of the Variscan chain of western Europe. In addition, there are several populations of inherited (xenocrystic) zircon: (1) Carboniferous zircon crystals (ca. 345 Ma) as well as one of the monazite fractions in the coarse-grained facies of the Ledesma pluton that also yielded an age of ca. 343 Ma. (2) Devonian-Silurian zircon xenocrysts with scattered ages between ca. 390 and 432 Ma. (3) Middle Cambrian-Ordovician (ca. 450-511 Ma). (4) Ediacaran-Cryogenian zircon ages (ca. 540-840 Ma). (5) Mesoproterozoic to Archaean zircon (900-2700 Ma). The abundance of Carboniferous-inherited zircon shows that crustal recycling/cannibalization may often happen at a fast pace in orogenic scenarios with only short lapses of quiescence. In our case study, it seems plausible that a "crustal layer" of ca. 340 Ma granitoids/migmatites was recycled, partially or totally, only 15-20 My after its emplacement.

  14. 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)

  15. Evaluation of potential of adsorption of U, Th, Pb, Zn and Ni by coconut fibers; Avaliacao do potencial de adsorcao de U, Th, Pb, Zn e Ni pelas fibras de coco

    Energy Technology Data Exchange (ETDEWEB)

    Monteiro, Raquel Almeida

    2009-07-01

    The residual biomass from agricultural activities has been evaluated as biosorbent for metals and organic composts from aqueous solutions, because of its adsorptive properties, low cost, abundance and to be a renewable resource. In this work, the efficiency of coir pith as biosorbent for the removal of U, Th, Pb, Zn e Ni ions from the aqueous solutions is presented. The coir pith is a by-product of the harvest of the coconut, a renewable natural source. The study was conducted by batch method. The influence of pH from 1 to 8, the dosage of the coir pith and the equilibrium time were studied. The adsorption of metal ions increased with the increase of pH and the dose. The Langmuir and Freundlich models were applied to describe the adsorption equilibrium isotherm. The kinetic process was studied using the pseudo-first order and pseudo-second order models. The Gibbs free energy was calculated. In the concentration range of 100 mg.L{sup -1} - 500 mg.L{sup -1}, the adsorption process was described better by the Langmuir equation for Pb{sup 2+} and Zn{sup 2+} ions and the Freundlich equation for UO{sub 2} 2{sup +}, Th{sup 4+} and Ni{sup 2+} ions, and represented by the pseudo-second order model. The biosorption process for removal of metal ions from the solutions was considered spontaneous. The results were promising, showing perspectives of application of coir pith as biosorbent of U, Th, Pb, Zn and Ni ions in wastewater treatment processes. (author)

  16. 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

  17. 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

  18. 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)

  19. U-Th-Pb dating of the Brossasco ultrahigh-pressure metagranite, Dora-Maira massif, western Alps

    Energy Technology Data Exchange (ETDEWEB)

    Paquette, J.L.; Montel, J.M. [Centre National de la Recherche Scientifique, 63 - Clermont-Ferrand (France); Chopin, C. [Ecole Normale Superieure, 75 - Paris (France). Lab. de Geologie

    1999-01-01

    The Brossasco metagranite is part of the coherent ultrahigh-pressure metamorphic terrane in the Dora-Maira massif and, although it has reached Alpine peak metamorphic conditions of about 725 C/30 kbar, still locally preserves an undeformed magmatic texture. In order to obtain new chronological constraints on this key area of the western Alps, we studied the behaviour of the U-Th-Pb system in zircons and monazites from such an undeformed facies. Only zircon fractions containing very small needle-shaped inclusions are concordant at 304{+-}3 Ma. This result is interpreted as the emplacement age of the granite. All other zircons show an old inherited memory and the more U-rich of these crystals were affected by an episodic Pb loss with a poorly defined lower intercept at 60{+-}45 Ma. Both TIMS (thermo-ionisation mass spectrometry) and electron-microprobe analysis of monazites show that this last event has also disturbed their U-Pb and Th-Pb isotopic systems, without resetting them completely. Comparison with cofacial rock-types which have been completely reworked under these extreme P-T conditions shows that deformation and mass transfer as well as the nature of the protoliths and the characteristics of their zircons have a much more pronounced influence on the behaviour of isotopic systems than the temperature and/or pressure parameters. This evidence is an obvious limitation to the use of the blocking-temperature concept. (orig.)

  20. U-Th-Pb dating of the Brossasco ultrahigh-pressure metagranite, Dora-Maira massif, western Alps

    International Nuclear Information System (INIS)

    Paquette, J.L.; Montel, J.M.; Chopin, C.

    1999-01-01

    The Brossasco metagranite is part of the coherent ultrahigh-pressure metamorphic terrane in the Dora-Maira massif and, although it has reached Alpine peak metamorphic conditions of about 725 C/30 kbar, still locally preserves an undeformed magmatic texture. In order to obtain new chronological constraints on this key area of the western Alps, we studied the behaviour of the U-Th-Pb system in zircons and monazites from such an undeformed facies. Only zircon fractions containing very small needle-shaped inclusions are concordant at 304±3 Ma. This result is interpreted as the emplacement age of the granite. All other zircons show an old inherited memory and the more U-rich of these crystals were affected by an episodic Pb loss with a poorly defined lower intercept at 60±45 Ma. Both TIMS (thermo-ionisation mass spectrometry) and electron-microprobe analysis of monazites show that this last event has also disturbed their U-Pb and Th-Pb isotopic systems, without resetting them completely. Comparison with cofacial rock-types which have been completely reworked under these extreme P-T conditions shows that deformation and mass transfer as well as the nature of the protoliths and the characteristics of their zircons have a much more pronounced influence on the behaviour of isotopic systems than the temperature and/or pressure parameters. This evidence is an obvious limitation to the use of the blocking-temperature concept. (orig.)

  1. 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

  2. Measurement of L sub(III) subshell fluorescence yields in Pb, Th and U

    Energy Technology Data Exchange (ETDEWEB)

    Arora, S K; Allawadhi, K L; Sood, B S [Punjabi Univ., Patiala (India). Nuclear Science Labs.

    1981-01-01

    L sub(III) subshell fluorescence yields in Pb, Th and U have been measured using photoionization for creating vacancies. The results have been compared with the available data and are found to agree with the recent measurements of Price made using K-L coincidence technique but higher than those of Stephenson made using fluorescent excitation of L sub(III) subshell.

  3. Investigating Pu and U isotopic compositions in sediments: a case study in Lake Obuchi, Rokkasho Village, Japan using sector-field ICP-MS and ICP-QMS.

    Science.gov (United States)

    Zheng, Jian; Yamada, Masatoshi

    2005-08-01

    The objectives of the present work were to study isotope ratios and the inventory of plutonium and uranium isotope compositions in sediments from Lake Obuchi, which is in the vicinity of several nuclear fuel facilities in Rokkasho, Japan. Pu and its isotopes were determined using sector-field ICP-MS and U and its isotopes were determined with ICP-QMS after separation and purification with a combination of ion-exchange and extraction chromatography. The observed (240)Pu/(239)Pu atom ratio (0.186 +/- 0.016) was similar to that of global fallout, indicating that the possible early tropospheric fallout Pu did not deliver Pu from the Pacific Proving Ground to areas above 40 degrees N. The previously reported higher Pu inventory in the deep water area of Lake Obuchi could be attributed to the lateral transportation of Pu deposited in the shallow area which resulted from the migration of deposited global fallout Pu from the land into the lake by river runoff and from the Pacific Ocean by tide movement and sea water scavenging, as well as from direct soil input by winds. The (235)U/(238)U atom ratios ranged from 0.00723 to 0.00732, indicating the natural origin of U in the sediments. The average (234)U/(238)U activity ratio of 1.11 in a sediment core indicated a significant sea water U contribution. No evidence was found for the release of U containing wastes from the nearby nuclear facilities. These results will serve as a reference baseline on the levels of Pu and U in the studied site so that any further contamination from the spent nuclear fuel reprocessing plants, the radioactive waste disposal and storage facilities, and the uranium enrichment plant can be identified, and the impact of future release can be rapidly assessed.

  4. 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

  5. Enhanced provenance interpretation using combined U-Pb and (U-Th)/He double dating of detrital zircon grains from lower Miocene strata, proximal Gulf of Mexico Basin, North America

    Science.gov (United States)

    Xu, Jie; Stockli, Daniel F.; Snedden, John W.

    2017-10-01

    Detrital zircon U-Pb analysis is an effective approach for investigating sediment provenance by relating crystallization age to potential crystalline source terranes. Studies of large passive margin basins, such as the Gulf of Mexico Basin, that have received sediment from multiple terranes with non-unique crystallization ages or sedimentary strata, benefit from additional constraints to better elucidate provenance interpretation. In this study, U-Pb and (U-Th)/He double dating analyses on single zircons from the lower Miocene sandstones in the northern Gulf of Mexico Basin reveal a detailed history of sediment source evolution. U-Pb age data indicate that most zircon originated from five major crystalline provinces, including the Western Cordillera Arc (1800 Ma) terranes. Zircon (U-Th)/He ages record tectonic cooling and exhumation in the U.S. since the Mesoproterozoic related to the Grenville to Laramide Orogenies. The combined crystallization and cooling information from single zircon double dating can differentiate volcanic and plutonic zircons. Importantly, the U-Pb-He double dating approach allows for the differentiation between multiple possible crystallization-age sources on the basis of their subsequent tectonic evolution. In particular, for Grenville zircons that are present in all of lower Miocene samples, four distinct zircon U-Pb-He age combinations are recognizable that can be traced back to four different possible sources. The integrated U-Pb and (U-Th)/He data eliminate some ambiguities and improves the provenance interpretation for the lower Miocene strata in the northern Gulf of Mexico Basin and illustrate the applicability of this approach for other large-scale basins to reconstruct sediment provenance and dispersal patterns.

  6. Determination {sup 230}Th by ICP-MS for the control of activities of restoration of an area of land contaminated with uranium mining sterile; Determinacion de {sup 230}Th mediante ICP-MS durante el control de las actividades de restauracion de un area de terreno contaminada con esteriles de mineria de uranio

    Energy Technology Data Exchange (ETDEWEB)

    Yague, L.; Conde, E.; Navarro, N.; Fernandez, M.; Ortiz, M. I.; Noguerales, C.; Gasco, C.

    2013-07-01

    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 {sup 230}Th by ICP-MS. (Author)

  7. 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.).

  8. 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.

  9. Provenance analysis of the Late Triassic Yichuan Basin: constraints from zircon U-Pb geochronology

    Directory of Open Access Journals (Sweden)

    Meng Xianghong

    2018-03-01

    Full Text Available Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS U-Pb dating has been performed on detrital zircons from the Chunshuyao Formation sandstone of Yichuan Basin. The ages of 85 detrital zircon grains are divided into three groups: 252-290 Ma, 1740-2000 Ma, and 2400-2600 Ma. The lack of Early Paleozoic and Neoproterozoic U-Pb ages indicates that there is no input from the Qinling Orogen, because the Qinling Orogen is characterized by Paleozoic and Neoproterozoic material. In combination with previous research, we suggest that the source of the Chunshuyao Formation is most likely recycled from previous sedimentary rocks from the North China Craton. In the Late Triassic, the Funiu ancient land was uplifted which prevented source material from the Qinling Orogen. Owing to the Indosinian orogeny, the strata to the east of the North China Craton were uplifted and eroded. The Yichuan Basin received detrital material from the North China Craton.

  10. 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...

  11. 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)

  12. 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.

  13. Migration of 226 Ra, 228 Ra, 210 Pb, U and Th from phosphogypsum

    International Nuclear Information System (INIS)

    Silva, Nivaldo Carlos da; Cipriani, Moacir; Taddei, Maria Helena T.

    2002-01-01

    The physico-chemical availability of radioactive elements ( 210 Pb, 226 Ra, 228 Ra, Th and U) in Brazilian phosphogypsum was investigated in a large scale leaching experiment carried out in lysimeters, using phosphogypsum samples (approximately 1.2 tons) from two phosphoric acid industries. Lysimeters were built using cylindrical concrete containers with 0.9 m inner diameter and 2 m depth. The bottom of the lysimeter was filled with a 10 cm layer of gravel covered with geomembrane sheet. Under this layer a pipe was designed to drain the percolated water. Three lysimeters were filled with phosphogypsum from each industry and a mixture of both. As percolated water comes exclusively from the rain, sample was collected daily when available. Samples were then pooled weekly, carefully prepared and submitted to radiochemical analysis. Radiochemical characterization of phosphogypsum and percolated water was performed by radiochemical separation followed by gross alpha and beta counting ( 226 Ra, 228 Ra and 210 Pb) and UV-Vis spectrophotometry with Arsenazo III (U and Th). This experiment was carried out from 12/01/1999 to 01/22/2001, with a precipitation of 2,732 mm. It was observed that approximately 40% (534 L) of the rain fall percolated through the lysimeter 1. The analysis of 22 samples of percolated water from lysimeter 1 showed mean radionuclides activities of 70±30 mBqL -1 , 70±50 mBqL -1 , 100±60 mBqL -1 and 110±55 mBqL -1 for U, 226 Ra, 228 Ra and 210 Pb, respectively. Thorium activities were below detection limit. (author)

  14. 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

  15. 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

  16. 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.

  17. 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.

  18. Petrochronology in constraining early Archean Earth processes and environments: Barberton greenstone belt, South Africa

    Science.gov (United States)

    Grosch, Eugene

    2017-04-01

    Analytical and petrological software developments over the past decade have seen rapid innovation in high-spatial resolution petrological techniques, for example, laser-ablation ICP-MS, secondary ion microprobe (SIMS, nano-SIMS), thermodynamic modelling and electron microprobe microscale mapping techniques (e.g. XMapTools). This presentation will focus on the application of petrochronology to ca. 3.55 to 3.33 billion-year-old metavolcanic and sedimentary rocks of the Onverwacht Group, shedding light on the earliest geologic evolution of the Paleoarchean Barberton greenstone belt (BGB) of South Africa. The field, scientific drilling and petrological research conducted over the past 8 years, aims to illustrate how: (a) LA-ICP-MS and SIMS U-Pb detrital zircon geochronology has helped identify the earliest tectono-sedimentary basin and sediment sources in the BGB, as well as reconstructing geodynamic processes as early as ca. 3.432 billion-years ago; (b) in-situ SIMS multiple sulphur isotope analysis of sulphides across various early Archean rock units help to reconstruct atmospheric, surface and subsurface environments on early Archean Earth and (c) the earliest candidate textural traces for subsurface microbial life can be investigated by in-situ LA-ICP-MS U-Pb dating of titanite, micro-XANES Fe-speciation analysis and metamorphic microscale mapping. Collectively, petrochronology combined with high-resolution field mapping studies, is a powerful multi-disciplinary approach towards deciphering petrogenetic and geodynamic processes preserved in the Paleoarchean Barberton greenstone belt of South Africa, with implications for early Archean Earth evolution.

  19. Elemental and Isotopic Analysis of Uranium Oxide an NIST Glass Standards by FEMTOSECOND-LA-ICP-MIC-MS

    International Nuclear Information System (INIS)

    Ebert, Chris; Zamzow, Daniel S.; McBay, Eddie H.; Bostick, Debra A.; Bajic, Stanley J.; Baldwin, David P.; Houk, R.S.

    2009-01-01

    The objective of this work was to test and demonstrate the analytical figures of merit of a femtosecond-laser ablation (fs-LA) system coupled with an inductively coupled plasma-multi-ion collector-mass spectrometer (ICP-MIC-MS). The mobile fs-LA sampling system was designed and assembled at Ames Laboratory and shipped to Oak Ridge National Laboratory (ORNL), where it was integrated with an ICP-MIC-MS. The test period of the integrated systems was February 2-6, 2009. Spatially-resolved analysis of particulate samples is accomplished by 100-shot laser ablation using a fs-pulsewidth laser and monitoring selected isotopes in the resulting ICP-MS transient signal. The capability of performing high sensitivity, spatially resolved, isotopic analyses with high accuracy and precision and with virtually no sample preparation makes fs-LA-ICP-MIC-MS valuable for the measurement of actinide isotopes at low concentrations in very small samples for nonproliferation purposes. Femtosecond-LA has been shown to generate particles from the sample that are more representative of the bulk composition, thereby minimizing weaknesses encountered in previous work using nanosecond-LA (ns-LA). The improvement of fs- over ns-LA sampling arises from the different mechanisms for transfer of energy into the sample in these two laser pulse-length regimes. The shorter duration fs-LA pulses induce less heating and cause less damage to the sample than the longer ns pulses. This results in better stoichiometric sampling (i.e., a closer correlation between the composition of the ablated particles and that of the original solid sample), which improves accuracy for both intra- and inter-elemental analysis. The primary samples analyzed in this work are (a) solid uranium oxide powdered samples having different 235 U to 238 U concentration ratios, and (b) glass reference materials (NIST 610, 612, 614, and 616). Solid uranium oxide samples containing 235 U in depleted, natural, and enriched abundances were

  20. 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.

  1. 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)

  2. 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

  3. Using titanite petrochronology to monitor CO2-degassing episodes from the Himalayas

    Science.gov (United States)

    Rapa, Giulia; Groppo, Chiara; Rolfo, Franco; Petrelli, Maurizio; Mosca, Pietro

    2017-04-01

    Metamorphic degassing from active collisional orogens supplies a significant fraction of CO2 to the atmosphere, playing a fundamental role in the long-term (> 1 Ma) global carbon cycle (Gaillardet & Galy, 2008). The petro-chronologic study of the CO2-source rocks (e.g. calc-silicate rocks) in collisional settings is therefore fundamental to understand the nature, timing, duration and magnitude of the orogenic carbon cycle. So far, the incomplete knowledge of these systems hindered a reliable quantitative modelling of metamorphic CO2 fluxes. A detailed petrological modelling of a clinopyroxene + scapolite + K-feldspar + plagioclase + biotite + zoisite ± calcite calc-silicate rock from central Nepal Himalaya allowed us to identify and fully characterize - for the first time - different metamorphic reactions that led to the simultaneous growth of titanite and production of CO2. These reactions involve biotite (rather than rutile) as the Ti-bearing reactant counterpart of titanite. The results of petrological modelling combined with Zr-in-Ttn thermometry and U-Pb geochronology suggest that in the studied sample, most titanite grains grew during two nearly continuous episodes of titanite formation: a near-peak event at 730-740°C, 10 kbar, 25.5±1.5 Ma, and a peak event at 740-765°C, 10.5 kbar, 22±3 Ma. Both episodes of titanite growth are correlated to specific CO2-producing reactions, thus allowing to constrain the timing, duration and P-T conditions of the main CO2-producing events, as well as the amounts of CO2 produced. Assuming that fluids released at a depth of ca. 30 km are able to reach the Earth's surface 10 Ma after their production, it is therefore possible to speculate on the role exerted by the Himalayan orogenesis on the climate in the past. Gaillardet J. & Galy A. (2008): Himalaya-carbon sink or source? Science, 320, 1727-1728.

  4. 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.

  5. Physical and chemical properties of fluid and melt inclusions of the Lagoa Real uraniferous albitites (Brazil)

    International Nuclear Information System (INIS)

    Chaves, Alexandre de Oliveira

    2010-01-01

    Data of melt and fluid inclusions obtained by LA-ICP-MS and microthermometry techniques represent an important investigation complement to understand geological processes which took place in Lagoa Real uraniferous albitites (Brazil). Melt inclusions found in augite structure, which reveals the previous presence of U in the syenitic magma. Primary fluid inclusions in magmatic augite of the albitites contain Na, denoting once more its presence in original magma. The formation of andradite from augite during shear events that generated the metamorphosed syenite (uraniferous albitite) was certified by the ICP-MS signals and uranium released by magmatic titanite (U source mineral)during the 1.9 Ga metamorphism was recorded in the fluid inclusions found in andradite, mineral that was formed in this same metamorphic event which recrystallized titanite crystals. Such uranium was responsible by precipitation of the disseminated uraninite found inside andradite. (author)

  6. Evaluation of potential of adsorption of U, Th, Pb, Zn and Ni by coconut fibers

    International Nuclear Information System (INIS)

    Monteiro, Raquel Almeida

    2009-01-01

    The residual biomass from agricultural activities has been evaluated as biosorbent for metals and organic composts from aqueous solutions, because of its adsorptive properties, low cost, abundance and to be a renewable resource. In this work, the efficiency of coir pith as biosorbent for the removal of U, Th, Pb, Zn e Ni ions from the aqueous solutions is presented. The coir pith is a by-product of the harvest of the coconut, a renewable natural source. The study was conducted by batch method. The influence of pH from 1 to 8, the dosage of the coir pith and the equilibrium time were studied. The adsorption of metal ions increased with the increase of pH and the dose. The Langmuir and Freundlich models were applied to describe the adsorption equilibrium isotherm. The kinetic process was studied using the pseudo-first order and pseudo-second order models. The Gibbs free energy was calculated. In the concentration range of 100 mg.L -1 - 500 mg.L -1 , the adsorption process was described better by the Langmuir equation for Pb 2+ and Zn 2+ ions and the Freundlich equation for UO 2 2 + , Th 4+ and Ni 2+ ions, and represented by the pseudo-second order model. The biosorption process for removal of metal ions from the solutions was considered spontaneous. The results were promising, showing perspectives of application of coir pith as biosorbent of U, Th, Pb, Zn and Ni ions in wastewater treatment processes. (author)

  7. 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

  8. 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

  9. 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...

  10. Cooling rates and the depth of detachment faulting at oceanic core complexes: Evidence from zircon Pb/U and (U-Th)/He ages

    Science.gov (United States)

    Grimes, Craig B.; Cheadle, Michael J.; John, Barbara E.; Reiners, P.W.; Wooden, J.L.

    2011-01-01

    Oceanic detachment faulting represents a distinct mode of seafloor spreading at slow spreading mid-ocean ridges, but many questions persist about the thermal evolution and depth of faulting. We present new Pb/U and (U-Th)/He zircon ages and combine them with magnetic anomaly ages to define the cooling histories of gabbroic crust exposed by oceanic detachment faults at three sites along the Mid-Atlantic Ridge (Ocean Drilling Program (ODP) holes 1270D and 1275D near the 15??20???N Transform, and Atlantis Massif at 30??N). Closure temperatures for the Pb/U (???800??C-850??C) and (U-Th)/He (???210??C) isotopic systems in zircon bracket acquisition of magnetic remanence, collectively providing a temperature-time history during faulting. Results indicate cooling to ???200??C in 0.3-0.5 Myr after zircon crystallization, recording time-averaged cooling rates of ???1000??C- 2000??C/Myr. Assuming the footwalls were denuded along single continuous faults, differences in Pb/U and (U-Th)/He zircon ages together with independently determined slip rates allow the distance between the ???850??C and ???200??C isotherms along the fault plane to be estimated. Calculated distances are 8.4 ?? 4.2 km and 5.0 2.1 km from holes 1275D and 1270D and 8.4 ?? 1.4 km at Atlantis Massif. Estimating an initial subsurface fault dip of 50 and a depth of 1.5 km to the 200??C isotherm leads to the prediction that the ???850??C isotherm lies ???5-7 km below seafloor at the time of faulting. These depth estimates for active fault systems are consistent with depths of microseismicity observed beneath the hypothesized detachment fault at the TAG hydrothermal field and high-temperature fault rocks recovered from many oceanic detachment faults. Copyright 2011 by the American Geophysical Union.

  11. Extrapolation of tectonic boundaries across the Labrador shelf: U-Pb geochronology of well samples

    International Nuclear Information System (INIS)

    Wasteneys, H.A.; Krogh, T.E.

    1996-01-01

    Near Saglek Fiord, a northerly trending boundary between the early Archean Saglek block and the middle Archean Hopedale block extends between drill sites which, respectively, sampled Uivak amphibolite gneiss with U-Pb zircon intercept ages of 3742 ± 12 and 2752 ± 42 Ma, and migmatitic Lister gneiss with concordant ages of 3213 -4 +21 Ma for restite and 2552 -21 +4 Ma for leucosome. Titanite ages of ca. 2508 Ma are common to both rocks. A nearby metapsammitic gneiss has detrital zircon and monazite ages of 2681 ± 5, 2700 ± 4, ca. 2730, and 2750 ± 2 Ma representing high-grade metamorphism related to the Hopedale-Saglek collision and metamorphic monazite of ca. 2560 Ma age representing metamorphism of the sediment during reactivation of the Saglek-Hopedale suture. Two hundred kilometres southeast, a gneissic granite records a protolith age of 3170 Ma and Late Proterozoic Pb loss. Near the Nain-Makkovik boundary, 1269 ± 4 Ma zircons indicate a significant extension of the Nain Plutonic Suite. South of the Makkovik boundary, a foliated granite yielded an upper intercept age defining intrusion at 1895 ± 8 Ma and concordant 1872 ± 5 Ma titanite ages that date subsequent metamorphism. Discordant U-Pb ages from an alkali-feldspar granite also constrain crystallization to ca. 1890 Ma and together with the gneiss represent the previously defined Iggiuk event in the Kaipokok domain. Wells near the southerly end of the transect record 1801 ± 5, 1813 ± 3, and 1806 ± 8 Ma ages, respectively, that are typical of the synorogenic granitoid suite representing the Cape Harrison domain of southern Makkovik Province. (author). 46 refs., 1 tab., 5 figs

  12. {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.

  13. Determination of the concentration of 238U, 234U, 232Th, 228Th, 228Ra, 226Ra and 210Pb in the feces of workers from a mining company of niobium and their families

    International Nuclear Information System (INIS)

    Oliveira, Roges de; Lopes, Ricardo T.; Melo, Dunstana R.; Juliao, Ligia M.Q.C.

    2005-01-01

    The object of this study consists of an open mine from which Niobium ore (pyrochlore) is extracted and a metallurgy company, where Fe-Nb alloys are produced for export. For geological reasons, the main ore is associated to natural radionuclides U and Th, and its decay products. The concentration of 234 U, 238 U, 232 Th, 226 Ra and 228 Ra, 228 Th, including 210 Pb in fecal excretion of 12:0 am, 29 workers and 13 family members were determined. The technique employed for the determination of the elements was the sequential method of radiochemical separation, followed by alpha spectrometry and counting α and β in proportional detector. Statistically significant difference was observed in the concentration of 234 U and 238 U, in feces samples, among the group of mining workers and family members; as well as for 232 Th in the feces of workers of crushing and metallurgy groups when compared with the Family Group. No statistically significant difference was detected at a concentration of 226 Ra, 228 Ra and 210 Pb, in feces of any group of workers of the installation in relation to the family group

  14. Determination of Leacheability of U, Th and Heavy Metals of Water Leached Purification (WLP) Residue and Soil from Bauxite Mining Area using Toxicity Characteristic Leaching Technique

    International Nuclear Information System (INIS)

    Siti Aminah Omar; Suhaimi Hamzah; Shamsiah Abdul Rahman

    2016-01-01

    The study was conducted to analyse the leachability of U, Th and heavy metals Cu, Cd, As, Pb, Mn, Zn, Ba, Se, Cr and Fe of water leached purification (WLP) residue gathered from Lynas Malaysia Sdn Bhd and soil from bauxite mining area, Kuantan. Their toxicity was assessed using the toxicity characteristic leaching procedure (TCLP) developed by the United States Environmental Protection Agency. The concentration of the elements studied was analysed using inductively coupled plasma mass spectrometry (ICP-MS). Results from the analysis indicated that the concentrations for all the elements studied in this project are well below than the TCLP regulatory limit. The concentrations of U and Th in leached solution were between 0.01 - 0.20 Bq/ kg. The concentrations of the multi elements were mostly between 0.02 - 1471 μg/ l, but certain elements such as Fe had concentration as high as 4707 μg/ l. Hence, it can be concluded that the WLP residue from Lynas and soil from bauxite mining area are very stable in the environment and does not pose any environmental problem. (author)

  15. Two high resolution terrestrial records of atmospheric Pb deposition from New Brunswick, Canada, and Loch Laxford, Scotland

    International Nuclear Information System (INIS)

    Kylander, Malin E.; Weiss, Domink J.; Kober, Bernd

    2009-01-01

    Environmental archives like peat deposits allow for the reconstruction of both naturally and anthropogenically forced changes in the biogeochemical cycle of Pb as well as the quantification of past and present atmospheric Pb pollution. However, records of atmospheric Pb deposition from pre-industrial times are lacking. In a publication by Weiss et al. [Weiss, D., Shotyk, W., Boyle, E.A., Kramers, J.D., Appleby, P.G., Cheburkin, A.K., Comparative study of the temporal evolution of atmospheric lead deposition in Scotland and eastern Canada using blanket peat bogs. Sci Total Environ 2002;292:7-18]. Pb isotopes data measured by Q-ICP-MS and TIMS, concentration and enrichment data was presented for sites in eastern Canada (PeW1) and northwestern Scotland (LL7c), dating to 1586 A.D and 715 A.D., respectively. Here these same cores are re-analysed for Pb isotopes by MC-ICP-MS thereby acquiring 204 Pb data and improving on the original data in terms of resolution and temporal coverage. Significant differences were found between the Q-ICP-MS/TIMS and MC-ICP-MS measurements, particularly at PeW1. These discrepancies are attributed to the problematic presence of organic matter during sample preparation and analysis complicated by the heterogeneity of the organic compounds that survived sample preparation steps. The precision and accuracy of Pb isotopes in complex matrices like peat is not always well estimated by industrial standards like NIST-SRM 981 Pb. Lead pollution histories at each site were constructed using the MC-ICP-MS data. The entire LL7c record is likely subject to anthropogenic additions. Contributions from local mining were detected in Medieval times. Later, coal use and mining in Scotland, Wales and England became important. After industrialization (ca. 1885 A.D.) contributions from Broken Hill type ores and hence, leaded petrol, dominate atmospheric Pb signatures right up to modern times. At PeW1 anthropogenic impacts are first distinguishable in the late 17

  16. 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

  17. 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.

  18. Study of in vivo generators Pb-212/Bi--212 and U-230/Th-226 for alpha radioimmunotherapy

    International Nuclear Information System (INIS)

    Le Du, A.

    2011-01-01

    Alpha-radioimmunotherapy is a promising cancer therapy that uses a-particles vectorized by monoclonal antibody to break down cancerous tumors. The notion of in vivo generator was introduced in 1989 by Leonard Mausner. The concept involves labeling of various molecular carriers (antibodies, peptides, etc) with intermediate half-life generator parents, which after accumulation in the desired tissue generate much shorter half-life daughter radionuclide. This thesis focuses on the study of two in vivo generators potentially interesting for alpha-radioimmunotherapy: Pb-212 / Bi-212 generator and U-230 / Th-226 generator. The first part of this work presents the Pb-212 / Bi-212 generator, two approaches allowing the vectorization. Chelation approach on a protein and an approach by encapsulation in liposomes have been proposed. This last approach appears to be the most interesting. In vitro stability studies have been performed on these labeling. The second part of this work presents the U-230 / Th-226 generator. Studies have first been made to achieve a theoretical model to describe the speciation of Th(IV) in human serum. The efficacy of DTPA as chelating agent for complexation of Th(IV) in human serum could thus be estimated. (author)

  19. Studies on 232Th and 238U levels in marine algae collected from the coast of Niigata Prefecture

    International Nuclear Information System (INIS)

    Kato, Kenji; Tonouchi, Shigemasa; Maruta, Fumiyuki; Ebata, Hidekazu

    2001-01-01

    To evaluate the properties of algae to concentrate radioactive elements, 14 species of algae like Sargassum were collected in the Prefecture and analyzed for their 232 Th and 238 U levels with Yokogawa HP4500 ICP-MS apparatus. The places of collection included those near the water discharge of an atomic power station. Mean 232 Th and 238 U levels were found to be 120 and 260 ng/g dry wt, respectively, and Phaeophyta showed more than several times higher 238 U level than Chlorophyta and Rhodophyta. There was no clear difference in 232 Th levels. No difference between places of collection was observed in Sargassum 232 Th or 238 U level. Adsorption of 232 Th particle to and incorporation of soluble 238 U into algae body were suggested. Mean 232 Th and 238 U radioactivities were found 73 and 510 μBq/g wet wt, respectively, and the respective annual committed effective doses, 0.2 and 0.3 μSv, calculated from those values were confirmed to be enough lower than the annual public dose limit, 1 mSv. (K.H.)

  20. High resolution analysis of uranium and thorium concentration as well as U-series isotope distributions in a Neanderthal tooth from Payre (Ardèche, France) using laser ablation ICP-MS

    Science.gov (United States)

    Grün, Rainer; Aubert, Maxime; Joannes-Boyau, Renaud; Moncel, Marie-Hélène

    2008-11-01

    We have mapped U ( 238U) and Th ( 232Th) elemental concentrations as well as U-series isotope distributions in a Neanderthal tooth from the Middle Palaeolithic site of Payre using laser ablation ICP-MS. The U-concentrations in an enamel section varied between 1 and 1500 ppb. The U-concentration maps show that U-migration through the external enamel surface is minute, the bulk of the uranium having migrated internally via the dentine into the enamel. The uranium migration and uptake is critically dependent on the mineralogical structure of the enamel. Increased U-concentrations are observed along lineaments, some of which are associated with cracks, and others may be related to intra-prismatic zones or structural weaknesses reaching from the dentine into the enamel. The uranium concentrations in the dentine vary between about 25,000 and 45,000 ppb. Our systematic mapping of U-concentration and U-series isotopes provides insight into the time domain of U-accumulation. Most of the uranium was accumulated in an early stage of burial, with some much later overprints. None of the uranium concentration and U-series profiles across the root of the tooth complied with a single stage diffusion-adsorption (D-A) model that is used for quality control in U-series dating of bones and teeth. Nevertheless, in the domains that yielded the oldest apparent U-series age estimates, U-leaching could be excluded. This means that the oldest apparent U-series ages of around 200 ka represent a minimum age for this Neanderthal specimen. This is in good agreement with independent age assessments (200-230 ka) for the archaeological layer, in which it was found. The Th elemental concentrations in the dental tissues were generally low (between about 1 and 20 ppb), and show little relationship with the nature of the tissue.

  1. Uranium isotopic ratio measurements ({sup 235}U/{sup 238}U) by laser ablation high resolution inductively coupled plasma mass spectrometry for environmental radioactivity monitoring - {sup 235}U/{sup 238}U isotope ratio analysis by LA-ICP-MS-HR for environmental radioactivity monitoring

    Energy Technology Data Exchange (ETDEWEB)

    David, K.; Mokili, M.B.; Rousseau, G.; Deniau, I.; Landesman, C. [SUBATECH, Ecole des Mines de Nantes, Universite de Nantes, CNRS/IN2P3, 4 rue Alfred Kastler, 44307 Nantes cedex 3 (France)

    2014-07-01

    The protection of the aquatic and terrestrial environments from a broad range of contaminants spread by nuclear activities (nuclear plants, weapon tests or mining) require continuous monitoring of long-lives radionuclides that were released into the environment. The precise determination of uranium isotope ratios in both natural and potential contaminated samples is of primary concern for the nuclear safeguards and the control of environmental contamination. As an example, analysis of environmental samples around nuclear plants are carried out to detect the traces in the environment originating from nuclear technology activities. This study deals with the direct analysis of {sup 235}U/{sup 238}U isotope ratios in real environmental solid samples performed with laser ablation (LA)-HR-ICP-MS. A similar technique has already been reported for the analysis of biological samples or uranium oxide particles [1,2] but to our knowledge, this was never applied on real environmental samples. The high sensitivity, rapid acquisition time and low detection limits are the main advantages of high resolution ICP-MS for accurate and precise isotope ratio measurements of uranium at trace and ultra-trace levels. In addition, the use of laser ablation allows the analysis of solid samples with minimal preparation. A a consequence, this technique is very attractive for conducting rapid direct {sup 235}U/{sup 238}U isotope ratio analysis on a large set of various matrix samples likely to be encountered in environmental monitoring such as corals, soils, sands, sediments, terrestrial and marine bio-indicators. For the present study, LA-ICP-MS-HR analyses are performed using a New Wave UP213 nano-second Nd:YAG laser coupled to a Thermo Element-XR high resolution mass spectrometer. Powdered samples are compacted with an hydraulic press (5 tons) in order to obtain disk-shaped pellet (10-13 mm in diameter and 2 mm in thickness). The NIST612 reference glass is used for LA-ICP-MS-HR tuning and as

  2. 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.

  3. Determination of Heavy Metals in Almonds and Mistletoe as a Parasite Growing on the Almond Tree Using ICP-OES or ICP-MS.

    Science.gov (United States)

    Kamar, Veysi; Dağalp, Rukiye; Taştekin, Mustafa

    2017-12-28

    In this study, the elements of Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Mo, Ni, Sr, Pb, Ti, and Zn were determined in the leaves, fruits, and branches of mistletoe, (Viscum albüm L.), used as a medicinal plant, and in the leaves, branches and barks of almond tree which mistletoe grows on. The aim of the study is to investigate whether the mistletoe are more absorbent than the almond tree in terms of the heavy metal contents and the determination of the amount of the elements penetrated into the mistletoe from the almond tree. ICP-MS (inductively coupled plasma-mass spectrometry) was used for the analysis of As, Cd, Mo, and Pb, whereas ICP-OES (inductively coupled plasma optical emission spectrometry) was used for the other elements. The results obtained were statistically evaluated at 95% confidence level. Within the results obtained in this study, it was determined whether there is a significant difference between metal elements in almond tree and mistletoe, or not. As a result, it was observed that there were higher contents of B, Ba, K, Mg, and Zn in the mistletoe than in the almond tree. K was found much higher than other elements in the mistletoe. On the other hand, Al, As, Ca, Cd, Cr, Cu, Fe, Mo, Ni, Sr, Pb, and Ti contents were determined to be more in almond tree than mistletoe.

  4. U/Th dating by SHRIMP RG ion-microprobe mass spectrometry using single ion-exchange beads

    Science.gov (United States)

    Bischoff, J.L.; Wooden, J.; Murphy, F.; Williams, Ross W.

    2005-01-01

    We present a new analytical method for U-series isotopes using the SHRIMP RG (Sensitive High mass Resolution Ion MicroProbe) mass spectrometer that utilizes the preconcentration of the U-series isotopes from a sample onto a single ion-exchange bead. Ion-microprobe mass spectrometry is capable of producing Th ionization efficiencies in excess of 2%. Analytical precision is typically better than alpha spectroscopy, but not as good as thermal ionization mass spectroscopy (TIMS) and inductively coupled plasma multicollector mass spectrometry (ICP-MS). Like TIMS and ICP-MS the method allows analysis of small samples sizes, but also adds the advantage of rapidity of analysis. A major advantage of ion-microprobe analysis is that U and Th isotopes are analyzed in the same bead, simplifying the process of chemical separation. Analytical time on the instrument is ???60 min per sample, and a single instrument-loading can accommodate 15-20 samples to be analyzed in a 24-h day. An additional advantage is that the method allows multiple reanalyses of the same bead and that samples can be archived for reanalysis at a later time. Because the ion beam excavates a pit only a few ??m deep, the mount can later be repolished and reanalyzed numerous times. The method described of preconcentrating a low concentration sample onto a small conductive substrate to allow ion-microprobe mass spectrometry is potentially applicable to many other systems. Copyright ?? 2005 Elsevier Ltd.

  5. 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

  6. 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)

  7. 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...

  8. [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.

  9. 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

  10. 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

  11. Finding the "true" age: ways to read high-precision U-Pb zircon dates

    Science.gov (United States)

    Schaltegger, U.; Schoene, B.; Ovtcharova, M.; Sell, B. K.; Broderick, C. A.; Wotzlaw, J.

    2011-12-01

    Refined U-Pb dating techniques, applying an empirical chemical abrasion treatment prior to analysis [1], and using a precisely calibrated double isotope Pb, U EARTHTIME tracer solution, have led to an unprecedented two problems: (A) Post-crystallization Pb loss from decay damaged areas is considered to be mitigated by applying chemical abrasion techniques. The success of such treatment can, however, not be assumed a priori. The following examples demonstrate that youngest zircons are not biased by lead loss but represent close-to-youngest zircon growth: (i) coincidence of youngest zircon dates with co-magmatic titanite in tonalite; (ii) coincidence with statistically equivalent clusters of 206Pb/238U dates from zircon in residual melts of cogenetic mafic magmas; (iii) youngest zircons in ash beds of sedimentary sequences do not violate the stratigraphic superposition, whereas conventional statistical interpretation (mean or median values) does; (iv) results of published inter-laboratory cross-calibration tests using chemical abrasion on natural zircon crystals of the same sample arrive at the same 206Pb/238U result within case of single, significantly younger dates (>3 sigma), and are common in many pre-Triassic and hydrothermally altered rocks. (B) Pre-eruptive/pre-intrusive growth is found to be the main reason for scattered zircon ages in igneous rocks. Zircons crystallizing from the final magma batch are called autocrystic [3]. Autocrystic growth will happen in a moving or stagnant magma shortly before or after the rheological lockup by the crystals. Last crystallizing zircons in the interstitial melt may therefore postdate emplacement of the magma. The range of 206Pb/238U ages may yield a time frame for the cooling of a given magma batch, which could be added to quantitative thermal models of magma emplacement and cooling. Hf isotopes and trace elements of the dated zircon are used to trace the nature of the dated grains [4], specifically for identification of

  12. 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

  13. [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.

  14. A rapid and reliable method for Pb isotopic analysis of peat and lichens by laser ablation-quadrupole-inductively coupled plasma-mass spectrometry for biomonitoring and sample screening

    International Nuclear Information System (INIS)

    Kylander, M.E.; Weiss, D.J.; Jeffries, T.E.; Kober, B.; Dolgopolova, A.; Garcia-Sanchez, R.; Coles, B.J.

    2007-01-01

    An analytical protocol for rapid and reliable laser ablation-quadrupole (LA-Q)- and multi-collector (MC-) inductively coupled plasma-mass spectrometry (ICP-MS) analysis of Pb isotope ratios ( 207 Pb/ 206 Pb and 208 Pb/ 206 Pb) in peats and lichens is developed. This technique is applicable to source tracing atmospheric Pb deposition in biomonitoring studies and sample screening. Reference materials and environmental samples were dry ashed and pressed into pellets for introduction by laser ablation. No binder was used to reduce contamination. LA-MC-ICP-MS internal and external precisions were 207 Pb/ 206 Pb and 208 Pb/ 206 Pb ratios. LA-Q-ICP-MS internal precisions on 207 Pb/ 206 Pb and 208 Pb/ 206 Pb ratios were lower with values for the different sample sets 208 Pb by Q-ICP-MS are identified as sources of reduced analytical performance

  15. 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)

  16. 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)

  17. 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.

  18. 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.

  19. 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)

  20. Contribution of some food categories on intakes of U, Th and other nuclides

    International Nuclear Information System (INIS)

    Shiraishi, Kunio

    1999-01-01

    The assessment of radiation dose in human from radioactive 232 Th, 238 U, 137 Cs, and 90 Sr are important because those nuclides are the largest contributors to committed internal doses. A market basket study was conducted to clarify the food pathways of the nuclides in Japanese subjects. Foodstuffs of 336 were purchased from markets in the vicinity of Mito-City during 1994-1995. Statistical consumption data were used for collection of the food samples. Thorium-232, 238 U, and stable isotope ( 133 Cs) in eighteen food groups were determined by inductively coupled mass spectrometry (ICP-MS). Radioisotopes ( 137 Cs) was analyzed by γ-spectrometry. Stable strontium ( 88 Sr) was also analyzed by inductively coupled atomic emission spectrometry (ICP-AES). Big contributors to the nuclide intakes in Japanese were as follows: 232 Th fishes and shellfishes (44%) and green vegetables (11%); 238 U seaweeds (50%) and fishes and shellfishes (26%); 88 Sr seaweeds (53%) and fishes and shellfishes (14%); 137 Cs mushrooms (17%), fishes and shell fishes (15%), milk products (11%), meats (9%), and potatoes (7%). The food categories of oil and fats, eggs and cooked meals were minor contributors in those nuclides. Dietary intake studies by using eighteen or more food categories should be effective procedure to resolve critical food and critical pathway for Japanese. Furthermore, critical pathways of radionuclides could be estimated by the analyses of stable isotopes. (author)

  1. Dietary 232Th and 238U intakes for Japanese as obtained in a market basket study and contributions of imported foods to internal doses

    International Nuclear Information System (INIS)

    Shiraishi, K.

    1995-01-01

    Thorium-232 and 238 U contents in four food groups were measured by inductively coupled plasma mass spectrometry (ICP-MS). Daily intakes of 232 Th and 238 U for Japanese were estimated to 2.22 mBq and 15.5 mBq per person, respectively. Furthermore, preliminary estimations were made for the effects of imported foods on internal exposures for Japanese. (author). 16 refs., 1 fig., 3 tabs

  2. Trace level determination of precious metals in aqueous medium, U, Th and Zr based nuclear materials by ICP-AES and EDXRF - a comparative study

    International Nuclear Information System (INIS)

    Sengupta, Arijit; Thulasidas, S.K.; Natarajan, V.

    2015-01-01

    A comparative study was carried out to determine Ag, Au and Pt in aqueous samples, uranium, zirconium, and thorium based nuclear fuels and associated materials by CCD based ICP-AES and EDXRF. In ICP-AES, the spectral interference of U, Th, Zr matrices on trace level determination of Ag, Au and Pt were studied for different analytical lines of these analytes. The analytical performance of different lines including detection limits, sensitivity, linear dynamic range etc were studied both by ICP-AES and EDXRF. Though EDXRF technique was known its non destructive nature, the overall analytical performance of ICP-AES technique was found to be superior to EDXRF. Based on the spectral contribution from emission rich matrix elements and the analytical performance of different analytical lines of these analytes, a method was developed for direct determination of these analytes by ICP-AES without chemical separation. The method was validated with synthetic samples and compared with EDXRF technique and conventional ICP-AES technique where the major matrix was chemically separated using suitable organic phase containing selective ligands. The ICP-AES method for direct determination of analytes without chemical separation was found to be simple, less time consuming, without generation of organic waste with acceptable analytical performance

  3. 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

  4. 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)

  5. Quantifying K, U and Th contents of marine sediments using shipboard natural gamma radiation spectra measured on DV JOIDES Resolution

    Science.gov (United States)

    De Vleeschouwer, David; Dunlea, Ann G.; Auer, Gerald; Anderson, Chloe H.; Brumsack, Hans; de Loach, Aaron; Gurnis, Michael C.; Huh, Youngsook; Ishiwa, Takeshige; Jang, Kwangchul; Kominz, Michelle A.; März, Christian; Schnetger, Bernhard; Murray, Richard W.; Pälike, Heiko; Expedition 356 shipboard scientists, IODP

    2017-04-01

    During International Ocean Discovery Program (IODP) expeditions, shipboard-generated data provide the first insights into the cored sequences. The natural gamma radiation (NGR) of the recovered material, for example, is routinely measured on the ocean drilling research vessel DV JOIDES Resolution. At present, only total NGR counts are readily available as shipboard data, although full NGR spectra (counts as a function of gamma-ray energy level) are produced and archived. These spectra contain unexploited information, as one can estimate the sedimentary contents of potassium (K), thorium (Th), and uranium (U) from the characteristic gamma-ray energies of isotopes in the 40K, 232Th, and 238U radioactive decay series. Dunlea et al. [2013] quantified K, Th and U contents in sediment from the South Pacific Gyre by integrating counts over specific energy levels of the NGR spectrum. However, the algorithm used in their study is unavailable to the wider scientific community due to commercial proprietary reasons. Here, we present a new MATLAB algorithm for the quantification of NGR spectra that is transparent and accessible to future NGR users. We demonstrate the algorithm's performance by comparing its results to shore-based inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-emission spectrometry (ICP-ES), and quantitative wavelength-dispersive X-ray fluorescence (XRF) analyses. Samples for these comparisons come from eleven sites (U1341, U1343, U1366-U1369, U1414, U1428-U1430, U1463) cored in two oceans during five expeditions. In short, our algorithm rapidly produces detailed high-quality information on sediment properties during IODP expeditions at no extra cost. Dunlea, A. G., R. W. Murray, R. N. Harris, M. A. Vasiliev, H. Evans, A. J. Spivack, and S. D'Hondt (2013), Assessment and use of NGR instrumentation on the JOIDES Resolution to quantify U, Th, and K concentrations in marine sediment, Scientific Drilling, 15, 57-63.

  6. Th-U-PbT dating by Electron Probe Microanalysis, Part I. Monazite: analytical procedures and data treatment;Datacao Th-U-Pb{sub T} com microssonda eletronica, Parte I. Monazita: procedimentos analiticos e tratamento de dados

    Energy Technology Data Exchange (ETDEWEB)

    Vlach, Silvio Roberto Farias, E-mail: srfvlach@usp.b [Universidade de Sao Paulo (IG/USP), SP (Brazil). Inst. de Geociencias. Dept. de Mineralogia e Geotectonica

    2010-03-15

    Dating methodology by the electron probe microanalyser (EPMA) of (Th, U)-bearing minerals, highlighting monazite, acquired greater than ever importance in literature, particularly due to its superior spatial resolution, as well as versatility, which allow correlating petrological processes at times registered only in micro-scales in minerals and rocks with absolute ages. Although the accuracy is inferior to the one achieved with conventional isotopic methods in up to an order of magnitude, EPMA is the instrument that allows the best spatial resolution, reaching a few {mu}m{sup 3} in some conditions. Quantification of minor and trace elements with suitable precision and accuracy involves the own instrumental and analytical set-ups and data treatment strategies, significantly more rigorous when compared with those applied in conventional analyses. Th-U-Pb{sub T} dating is an example of these cases. Each EPMA is a unique machine as for its instrumental characteristics and respective automation system. In such a way, analytical procedures ought to be adjusted for laboratory specificities. The analytical strategies and data treatment adopted in the Electronic Microprobe Laboratory from Instituto de Geociencias of Universidade de Sao Paulo, Brazil, with a JEOL JXA8600S EPMA, and a ThermoNoran-Voyager 4.3 automation system, are presented and compared with the ones used in other laboratories. The influence of instrumental factors and spectral overlaps on Th, U, and Pb quantification is discussed. Applied procedures to interference correction, error propagation, data treatment, and fi nal chemical age presentation as well as to sampling and analyses are emphasized. Some typical applications are discussed, drawing attention to the most relevant aspects of electron microprobe dating. (author)

  7. New zircon U-Pb LA-ICP-MS ages and Hf isotope data from the Central Pontides (Turkey): Geological and geodynamic constraints

    Science.gov (United States)

    Çimen, Okay; Göncüoğlu, M. Cemal; Simonetti, Antonio; Sayit, Kaan

    2018-05-01

    The Central Pontides in northern Anatolia is located on the accretionary complex formed by the closure of Neotethyan Intra-Pontide Ocean between the southern Eurasian margin (Istanbul-Zonguldak Terrane) and the Cimmerian Sakarya Composite Terrane. Among other components of the oceanic lithosphere, it comprises not yet well-dated felsic igneous rocks formed in arc-basin as well as continent margin settings. In-situ U-Pb age results for zircons from the arc-basin system (öangaldağ Metamorphic Complex) and the continental arc (Devrekani Metadiorite and Granitoid) yield ages of 176 ± 6 Ma, 163 ± 9 Ma and 165 ± 3 Ma, respectively. Corresponding in-situ average (initial) 176Hf/177Hf initial ratios are 0.28261 ± 0.00003, 0.28267 ± 0.00002 and 0.28290 ± 0.00004 for these units and indicative of a subduction-modified mantle source. The new U-Pb ages and Hf isotope data from these oceanic and continental arc units together with regional geological constraints support the presence of a multiple subduction system within the Intra-Pontide Ocean during the Middle Jurassic.

  8. 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.

  9. Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples

    International Nuclear Information System (INIS)

    Boulyga, Sergei F.; Heilmann, Jens; Heumann, Klaus G.; Prohaska, Thomas

    2007-01-01

    A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for 35 Cl + to more than 6 x 10 5 cps for 238 U + for 1 μg of trace element per gram of coal sample. Detection limits vary from 450 ng g -1 for chlorine and 18 ng g -1 for sulfur to 9.5 pg g -1 for mercury and 0.3 pg g -1 for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis. (orig.)

  10. Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples.

    Science.gov (United States)

    Boulyga, Sergei F; Heilmann, Jens; Prohaska, Thomas; Heumann, Klaus G

    2007-10-01

    A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for (35)Cl+ to more than 6 x 10(5) cps for (238)U+ for 1 microg of trace element per gram of coal sample. Detection limits vary from 450 ng g(-1) for chlorine and 18 ng g(-1) for sulfur to 9.5 pg g(-1) for mercury and 0.3 pg g(-1) for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis.

  11. Genesis of the Bangbule Pb-Zn-Cu polymetallic deposit in Tibet, western China: Evidence from zircon U-Pb geochronology and S-Pb isotopes

    Science.gov (United States)

    Kan, Tian; Zheng, Youye; Gao, Shunbao

    2016-04-01

    The Banbule Pb-Zn-Cu skarn deposit is located in the Longger-Gongbujiangda volcanic magma arc in the Gangdese-Nyainqentanglha Plate. It is the only lead-zinc polymetallic deposit discovered in the westernmost Nyainqentanglha metallogenic belt. The measured and indicated resources include 0.9 Mt of Pb+Zn (4.77% Pb and 4.74% Zn, respectively), 6499 t of Cu, and 178 t of Ag (18.75g/t Ag). The orebodies mainly occur as lenses, veins and irregular shapes in the contact zone between the quartz-porphyry and limestone of the Upper Permian Xiala Formation, or in the boundaries between limestone and sandstone. Pb-Zn-Cu mineralization in the Banbule deposit is closely associated with skarns. The ore minerals are dominated by galena, sphalerite, chalcopyrite, bornite, and magnetite, with subordinate pyrite, malachite, and azurite. The gangue minerals are mainly garnet, actinolite, diopside, quartz, and calcite. The ore-related quartz-porphyry displays LA-ICP-MS zircon U-Pb age of 77.31±0.74 Ma. The δ34S values of sulfides define a narrow range of -0.8 to 4.7‰ indicating a magmatic source for the ore-forming materials. Lead isotopic systematics yield 206Pb/204Pb of 18.698 to 18.752, 207Pb/204Pb of 15.696 to 15.760, and 208Pb/204Pb of 39.097 to 39.320. The data points are constrained around the growth curves of upper crust and orogenic belt according to the tectonic discrimination diagrams. The calculated Δβ - Δγ values plot within the magmatic field according to the discrimination diagram of Zhu et al. (1995). The S-Pb isotopic data suggest that Bangbule is a typical skarn deposit, and the Pb-Zn-Cu mineralization is genetically related to the quartz-porphyry in the mining district. The discovery of the Bangbule deposit indicates that there is metallogenic potential in the westernmost Nyainqentanglha belt, which is of great importance for the exploration work in this area.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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)

  17. Age relationships from U-Th-Pb isotope studies of uranium mineralization in Wernecke breccias, Yukon Territory

    International Nuclear Information System (INIS)

    Archer, A.

    1986-01-01

    Pb-U ± Th isotope analyses for 17 specimens of uraniferous breccia from the northeastern Wernecke Mountains reveal several apparent ages for mineralization. The oldest date, 1194 Ma, reflects either initial emplacement of the breccias or their modification by effects of the Rackla of Rapitan (Windermere) thick clastic wedges and iron formation. The 510 Ma date reflects mid-Cambrian mineralization roughly coincident with regional uplift (and attendant karstification) and development of thick clastic wedges. This was also an important period for Pb-Zn mineralization. Younger dates resulted from continuing remobilization, and all isotopic ages for mineralized breccia reflect movements associated with the Richardson Fault array

  18. U-Pb thermochronology of the lower crust: producing a long-term record of craton thermal evolution

    Science.gov (United States)

    Blackburn, T.; Bowring, S. A.; Mahan, K. H.; Perron, T.; Schoene, B.; Dudas, F. O.

    2010-12-01

    The EarthScope initiative is focused on providing an enhanced view of the North American lithosphere and the present day stress field of the North American continent. Of key interest is the interaction between convecting asthenosphere and the conducting lithospheric mantle that underlie the continents, especially the cold ‘keels’ that underlie Archean domains. Cratonic regions are in general characterized by minimal erosion and or sediment accumulation. The Integration of seismic tomography, and mantle xenolith studies reveal a keel of seismically fast and relatively buoyant and viscous mantle; physical properties that are intimately linked with the long-term stability and topographic expression of the region. Missing from this model of the continental lithosphere is the 4th dimension--time--and along with it our understanding of the long-term evolution of these stable continental interiors. Here we present a thermal record from the North American craton using U-Pb thermochronology of lower crustal xenoliths. The use of temperature sensitive dates on lower crustal samples can produce a unique time-temperature record for a well-insulated and slowly cooling lithosphere. The base of the crust is insulated enough to remain unperturbed by any plausible changes to surface topography, yet unlike the subadjacent lithospheric mantle, contains accessory phases amenable to U-Pb dating (rutile, apatite, titanite). With near steady state temperatures in the lower crust between 400-600 °C, U-Pb thermochronometers with similar average closure temperatures for Pb are perfectly suited to record the long-term cooling of the lithosphere. Xenoliths from multiple depths, and across the craton yield time-temperature paths produced from U-Pb thermochronometers that record extremely slow cooling (<0.25 °C/Ma) over time scales of billions of years. Combining these data with numerical thermal modeling allow constraints to be placed on the dominant heat transfer mechanisms operating

  19. Studies on {sup 232}Th and {sup 238}U levels in marine algae collected from the coast of Niigata Prefecture

    Energy Technology Data Exchange (ETDEWEB)

    Kato, Kenji; Tonouchi, Shigemasa; Maruta, Fumiyuki; Ebata, Hidekazu [Niigata Prefectural Inst. of Public Health and Environmental Sciences (Japan)

    2001-12-01

    To evaluate the properties of algae to concentrate radioactive elements, 14 species of algae like Sargassum were collected in the Prefecture and analyzed for their {sup 232}Th and {sup 238}U levels with Yokogawa HP4500 ICP-MS apparatus. The places of collection included those near the water discharge of an atomic power station. Mean {sup 232}Th and {sup 238}U levels were found to be 120 and 260 ng/g dry wt, respectively, and Phaeophyta showed more than several times higher {sup 238}U level than Chlorophyta and Rhodophyta. There was no clear difference in {sup 232}Th levels. No difference between places of collection was observed in Sargassum {sup 232}Th or {sup 238}U level. Adsorption of {sup 232}Th particle to and incorporation of soluble {sup 238}U into algae body were suggested. Mean {sup 232}Th and {sup 238}U radioactivities were found 73 and 510 {mu}Bq/g wet wt, respectively, and the respective annual committed effective doses, 0.2 and 0.3 {mu}Sv, calculated from those values were confirmed to be enough lower than the annual public dose limit, 1 mSv. (K.H.)

  20. Properties and recrystallization of radiation damaged pyrochlore and titanite

    Energy Technology Data Exchange (ETDEWEB)

    Zietlow, Peter

    2016-11-02

    Radiation damage in minerals is caused by the alpha-decay of incorporated radionuclides, such as U and Th and their decay products. The effect of thermal annealing (400-1400 K) on radiation-damaged pyrochlores has been investigated by Raman scattering, X-ray powder diffraction (XRD), and combined differential scanning calorimetry/thermogravimetry (DSC/TG) (Zietlow et al., in print). The analysis of three natural radiation-damaged pyrochlore samples from Miass/Russia (6.4 wt% Th, 23.1.10{sup 18} a-decay events per gram (dpg)), Zlatoust/Russia (6.3 wt% Th, 23.1.10{sup 18} dpg), Panda Hill/Tanzania (1.6 wt% Th, 1.6.10{sup 18} dpg), and Blue River/Canada (10.5 wt% U, 115.4.10{sup 18} dpg), are compared with a crystalline reference pyrochlore from Schelingen (Germany). The type of structural recovery depends on the initial degree of radiation damage (Panda Hill 28 %, Blue River 85 %, Zlatoust and Miass 100 % according to XRD), as the recrystallization temperature increases with increasing degree of amorphization. Raman spectra indicate reordering on the local scale during annealing-induced recrystallization. As Raman modes around 800 cm{sup -1} are sensitive to radiation damage (Vandenborre and Husson 1983, Moll et al. 2011), the degree of local order was deduced from the ratio of the integrated intensities of the sum of the Raman bands between 605 and 680 cm{sup -1} devided by the sum of the integrated intensities of the bands between 810 and 860 cm{sup -1}. The most radiation damaged pyrochlores (Miass and Zlatoust) show an abrupt recovery of both, its short- (Raman) and long-range order (X-ray) between 800 and 850 K. The volume decrease upon recrystallization in Zlatoust pyrochlore was large enough to crack the sample repeatedly. In contrast, the weakly damaged pyrochlore (Panda Hill) begins to recover at considerably lower temperatures (near 500 K), extending over a temperature range of ca. 300 K, up to 800 K (Raman). The pyrochlore from Blue River shows in its

  1. 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.

  2. 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.)

  3. Rapid screening of natually occurring radioactive nuclides({sup 2}'3{sup 8}U, {sup 232}Th) in raw materials and by-products samples using XRF

    Energy Technology Data Exchange (ETDEWEB)

    Park, Ji Young; Lim, Chung Sup [Radiation Biotechnology and Applied Radioiostope Science, University of Science and Technology, Daejeon (Korea, Republic of); Lim, Jong Myoung; Ji, Young Yong; Chung, Kun Ho; Lee, Wan No; Kang, Mun Ja [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of); Jang, Byung Uck [Korea Institute of Nuclear Safety, Daejeon (Korea, Republic of)

    2016-12-15

    As new legislation has come into force implementing radiation safety management for the use of naturally occurring radioactive materials (NORM), it is necessary to establish a rapid and accurate measurement technique. Measurement of {sup 238}U and {sup 232}Th using conventional methods encounter the most significant difficulties for pretreatment (e.g., purification, speciation, and dilution/enrichment) or require time-consuming processes. Therefore, in this study, the applicability of ED-XRF as a non-destructive and rapid screening method was validated for raw materials and by-product samples. A series of experiments was conducted to test the applicability for rapid screening of XRF measurement to determine activity of {sup 238}U and {sup 23{sup 2}}Th based on certified reference materials (e.g., soil, rock, phosphorus rock, bauxite, zircon, and coal ash) and NORM samples commercially used in Korea. Statistical methods were used to compare the analytical results of ED-XRF to those of certified values of certified reference materials (CRM) and inductively coupled plasma mass spectrometry (ICP-MS). Results of the XRF measurement for {sup 238}U and {sup 232}Th showed under 20% relative error and standard deviation. The results of the U-test were statistically significant except for the case of U in coal fly ash samples. In addition, analytical results of {sup 238}U and {sup 232}Th in the raw material and by-product samples using XRF and the analytical results of those using ICP-MS (R{sup 2}≥0.95) were consistent with each other. Thus, the analytical results rapidly derived using ED-XRF were fairly reliable. Based on the validation results, it can be concluded that the ED-XRF analysis may be applied to rapid screening of radioactivities ({sup 238}U and {sup 232}Th) in NORM samples.

  4. Ion microprobe U-Pb dating of a dinosaur tooth

    International Nuclear Information System (INIS)

    Sano, Yuji; Terada, Kentaro; Ly, Chi V.; Park, Eun Ju

    2006-01-01

    Ion microprobe U-Pb dating of apatite is applied to a fossil tooth of a Allosaurid derived from the Hasandong Formation in the Gyeongsang basin, southeastern Korea. Twelve spots on a single fragment of the fossil dentine yield a Tera-Wasserburg concordia intercept age of 115±10 Ma (2σ, MSWD=0.59) on a 238 U/ 206 Pb- 207 Pb/ 206 Pb- 204 Pb/ 206 Pb diagram. The age provides a constraint on the depositional age of the fossil in its host Hassandong Formation as Early Aptian. The success of the ion microprobe dating depends on the heterogeneities of diagenetically incorporated U and Pb at the few hundred μm scale, the consequent variations in Pb isotopic compositions due to radioactive decay and the closed-system behavior of U and Pb. There are at least three end-members to explain the variations of minor chemical components such as FeO, SiO 2 and Al 2 O 3 , and trace elements as Th, U and rare earth elements (REE) in the sample by a simple mixing model. They are (1) very low minor and REE, very high common Pb with variable U abundances, (2) low common Pb, high minor, REE, and U abundances, and (3) low minor, common Pb, and U with intermediate REE abundances, even though groups (2) and (3) may consist of a larger group. Various contributions of the three (and/or two) end-members during diagenetic processes may cause the elemental fractionation of U and Pb in a fossil tooth. (author)

  5. U-Pb dating of deformed mafic dyke and host gneiss: implications for understanding reworking processes on the western margin of the Archaean U3o8 Block, NE Sao Francisco Craton, Brazil

    International Nuclear Information System (INIS)

    Oliveira, Elson Paiva

    2000-01-01

    U-Pb ages of deformed mafic dyke and host migmatitic grey gneiss from the transition zone between the Archaen Uaua Block and the Caldeirao Belt are presented. Titanites from the metamorphic dyke's margin and zircons from the gneiss were dated at 2,039 ± 2 Ma and 2,956 ± 39 Ma, respectively. The Sm-Nd data (T DM =2,965 Ma and ε Nd(t) =1.69) on the gneiss, coupled with the U-Pb data on both dyke and gneiss, suggest than an Archaen granodioritic batholith, probably originated at an andean-type continental margin, was intruded by mafic dykes, and subsequently was reworked during the Paleoproterozoic collisional event associated with the development of the Salvador-Curaca Orogen. (author)

  6. 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

  7. 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.

  8. 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.

  9. 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

  10. Lead Isotopic Composition in Biogenic Certified Reference Materials Determined by Different ICP-based Mass Spectrometric Techniques

    Czech Academy of Sciences Publication Activity Database

    Ďurišová, Jana; Ackerman, Lukáš; Strnad, L.; Chrastný, V.; Borovička, Jan

    2015-01-01

    Roč. 39, č. 2 (2015), s. 209-220 ISSN 1639-4488 Institutional support: RVO:67985831 Keywords : Pb isotopes * 206 Pb/ 207 Pb * 208 Pb/ 206 Pb * ICP-MS * certified reference materials * vegetation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.885, year: 2015

  11. U-Pb age constraints for the La Tuna Granite and Montevideo Formation (Paleoproterozoic, Uruguay): Unravelling the structure of the Río de la Plata Craton

    Science.gov (United States)

    Pamoukaghlián, Karina; Gaucher, Claudio; Frei, Robert; Poiré, Daniel G.; Chemale, Farid; Frei, Dirk; Will, Thomas M.

    2017-11-01

    The Río de la Plata Craton is a continental block that crops out in Uruguay, eastern Argentina, southernmost Brazil and Paraguay. It comprises in Uruguay the Piedra Alta, Tandilia and Nico Pérez terranes, separated by the Colonia and the Sarandí del Yí megashears. The La Tuna Granite, which intrudes the Araminda metasandstones in the Tandilia Terrane, was considered Cambrian in age and the intruded sandstones were assigned to the Neoproterozoic Piedras de Afilar Formation. We show that the granite is Paleoproterozoic in age and that the host metasandstones do not belong to the Piedras de Afilar Formation, but to the Paleoproterozoic Montevideo Formation. U-Pb LA ICP-MS of zircon ages for the La Tuna Granite yielded a concordant crystallization age of 2156 ± 26 Ma. Furthermore a metamorphic event at 2010 ± 9 Ma is revealed by Pb stepwise leaching dating of monazites. U-Pb detrital zircon ages of the host Araminda metasandstone yield an upper intercept discordia age of 2152 ± 29 Ma, which marks the intrusion of the La Tuna pluton, and which is in accordance with the zircon U-Pb LA ICP MS constraints. A concordant U-Pb detrital zircon age of 2465 ± 40 Ma provides a maximum depositional age constraint for the metapsammites. Comparing quartz arenites of the Ediacaran Piedras de Afilar Formation with the Araminda metaquartzites, we conclude that they are very similar regarding petrology but they differ in age and metamorphic overprint. Detrital zircons in quartz arenites of the Piedras de Afilar Formation show youngest ages of 1.0 Ga. On the other hand, detrital zircons recovered from the Araminda metasandstones and the age of the intruding granite allow interpreting a depositional age between 2465 and 2150 Ma. Nd model ages show crustal residence times in average more than 200 myr older for the Tandilia Terrane both in Uruguay and Argentina, with a significant Neoarchean component, which is lacking in the Piedra Alta Terrane. Whereas the Piedra Alta Terrane was

  12. 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.

  13. 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.

  14. 230Th-234U Model-Ages of Some Uranium Standard Reference Materials

    International Nuclear Information System (INIS)

    Williams, R.W.; Gaffney, A.M.; Kristo, M.J.; Hutcheon, I.D.

    2009-01-01

    The 'age' of a sample of uranium is an important aspect of a nuclear forensic investigation and of the attribution of the material to its source. To the extent that the sample obeys the standard rules of radiochronometry, then the production ages of even very recent material can be determined using the 230 Th- 234 U chronometer. These standard rules may be summarized as (a) the daughter/parent ratio at time=zero must be known, and (b) there has been no daughter/parent fractionation since production. For most samples of uranium, the 'ages' determined using this chronometer are semantically 'model-ages' because (a) some assumption of the initial 230 Th content in the sample is required and (b) closed-system behavior is assumed. The uranium standard reference materials originally prepared and distributed by the former US National Bureau of Standards and now distributed by New Brunswick Laboratory as certified reference materials (NBS SRM = NBL CRM) are good candidates for samples where both rules are met. The U isotopic standards have known purification and production dates, and closed-system behavior in the solid form (U 3 O 8 ) may be assumed with confidence. We present here 230 Th- 234 U model-ages for several of these standards, determined by isotope dilution mass spectrometry using a multicollector ICP-MS, and compare these ages with their known production history

  15. 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).

  16. 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...

  17. Quantification of {sup 232}Th, {sup 234}U, {sup 235}U and {sup 238}U in river mollusks by magnetic sector mass spectrometry with inductively coupled plasma source (Icp-SFMS); Cuantificacion de {sup 232}Th, {sup 234}U, {sup 235}U y {sup 238}U en moluscos de rios por espectrometria de masas de sector magnetico con fuente de plasma acoplado inductivamente (ICP-SFMS)

    Energy Technology Data Exchange (ETDEWEB)

    Arevalo R, D. L.; Hernandez M, H.; Romero G, E. T.; Lara A, N. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Alfaro de la T, M. C., E-mail: arevalo0591@hotmail.com [Universidad Autonoma de San Luis Potosi, Dr. Salvador Nava s/n, Zona Universitaria, 78290 San Luis Potosi, SLP (Mexico)

    2016-09-15

    The present work deals with the methodology established for the quantification of {sup 232}Th, {sup 234}U, {sup 238}U and {sup 235}U in the shell of gastropod mollusks collected in the rivers Valles, Coy and Axtla of San Luis Potosi, Mexico, which belong to the Panuco River basin; these rivers have as main source of pollution the discharge of municipal sewage, waste from small industries, agricultural and cattle residues and from natural sources. Conventional methods for measuring radio-nuclides are confronted with certain conditions related to the requirement in measurement, basically in the characterization that is related to the concepts of precision and accuracy. The analysis of the gastropod mollusk shell was performed by the Icp-SFMS technique; the main advantages of this technique lie in the isotope quantification capacity, the high precision and the low limits of detection, in this study are very important because these elements are in concentrations between ppb and ppt. This technique allowed the analysis of the samples having a complex matrix by the presence CaCO{sub 3} minimizing the interferences thanks to the ionization efficiency of the Ar plasma. For the species Pachychilus monachus were found concentrations of {sup 232}Th of 0.16-5.37 μg/g and of total U of 0.101-4.081 μg/g being this species where the highest values of total U were found. For Thiara (melanoids) tuberculata the lowest values were found among the different species ({sup 232}Th 0.61-3.61 μg/g and total U 0.006-0.042 μg/g), for Pachychilus suturalis, values of {sup 232}Th of 0.58-6.4 μg/g and for Pachychilus sp. were found between 0.26-7.62 μg/g and for total U values between 0.28-3.33 μg/g. The method offers several advantages: speed, good precision, low values of quantification limits and high sensitivity in the measurement of radio-nuclides and heavy metals. (Author)

  18. 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...

  19. High-precision timing of Nanhai coral by using MC-ICP-MS and TIMS techniques and its paleo-environmental significance

    International Nuclear Information System (INIS)

    Peng Zicheng; Nie Baofu; Chen Tegu

    2004-01-01

    The techniques of thermal ionization mass spectrometry (TIMS) and multicollector-inductively coupled plasma-mass spectrometry (MC-ICP-MS) were used for the high-precision timing of the domestic stalagmite standard (GBW04412), international coral standard (RKM-4) and the Nanhai corals. The results of uranium contents and the ratios of 234 U/ 238 U and 230 Th/ 234 U in the two standards measured by using two techniques were consistent within the error range. Most of the Nanhai corals have less than 3 μg/g of the uranium contents and 150 ± 5 of the δ 234 U(T) values, which means that the corals have not been subjected to the alternation since they were brought up 7000 years ago, therefore, they preserve the original environmental signals. The age sequence of the corals shows that three events of the high sea level happened in Nanhai area in the periods corresponding to 6799-6307 a B.P., 4472-4285 a B.P. and 1279-1012 a B.P. respectively. The above-mentioned three stages were relative to the Megathermal and Medieval Warm Periods in our country. (authors)

  20. Isotopic composition of Pb and Th in interplinian volcanics from Somma-Vesuvius volcano, Italy

    International Nuclear Information System (INIS)

    Cortini, M.; De Vivo, B.; Somma, R.; Ayuso, R.A.; Holden, P.

    2004-01-01

    We present a detailed isotopic study of volcanic rocks emitted from Somma-Vesuvius volcano during three periods of interplinian activity: 'Protohistoric' (3550 y B.P. to 79 A.D.), 'Ancient Historic' (79 to 472 A.D.) and 'Medieval' (472 to 1631 A.D.). Pb isotopic compositions of two acid leached fractions and whole rock residues of 37 whole rock samples (determined by Somma et al., 2001) show that each of the three interplinian periods is distinguished by small, systematic, and unique uranogenic and thorogenic Pb isotopic trends. This key and novel feature is compatible with the notion that the Pb isotopic data reflect small-scale source heterogeneity operating over relatively short periods of time. From this representative group of samples, a selected set of nine whole rocks were analyzed for Th isotopes. 232 Th/ 238 U ratios in the source can be obtained independently from Pb and from Th isotopes. Those obtained from Pb isotopes represent source ratios, time-integrated over the whole age of the earth; they range from 3.9 to 4.1. 232 Th/ 238 U obtained from Th isotopes are those of the present source. They are lower, and cluster around 3.5; this difference probably indicates recent U enrichment of the present source. The behavior of Pb, as inferred by its isotopic ratios, is quite distinct from that of Sr and Nd isotopes: Pb isotope variations are not correlated to Sr or Nd isotope variations. The isotopic contrast is compatible with the idea that the isotopes were decoupled during magmatic production, evolution, and ascent through the crust. Thus, the Pb isotopes do not reflect the effects of the same processes as in the case of the Sr and Nd isotopes, or, as we also favor, they do not necessarily reflect the same source contributions into the magmas. Moreover, the Pb isotopic evolution of the interplinian rocks chiefly reflects mixing, driven by processes that are superimposed on, and independent of, other source contributions that determine the isotopic

  1. 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.

  2. 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.

  3. Th-U-PbT dating by Electron Probe Microanalysis, Part I. Monazite: analytical procedures and data treatment

    International Nuclear Information System (INIS)

    Vlach, Silvio Roberto Farias

    2010-01-01

    Dating methodology by the electron probe microanalyser (EPMA) of (Th, U)-bearing minerals, highlighting monazite, acquired greater than ever importance in literature, particularly due to its superior spatial resolution, as well as versatility, which allow correlating petrological processes at times registered only in micro-scales in minerals and rocks with absolute ages. Although the accuracy is inferior to the one achieved with conventional isotopic methods in up to an order of magnitude, EPMA is the instrument that allows the best spatial resolution, reaching a few μm 3 in some conditions. Quantification of minor and trace elements with suitable precision and accuracy involves the own instrumental and analytical set-ups and data treatment strategies, significantly more rigorous when compared with those applied in conventional analyses. Th-U-Pb T dating is an example of these cases. Each EPMA is a unique machine as for its instrumental characteristics and respective automation system. In such a way, analytical procedures ought to be adjusted for laboratory specificities. The analytical strategies and data treatment adopted in the Electronic Microprobe Laboratory from Instituto de Geociencias of Universidade de Sao Paulo, Brazil, with a JEOL JXA8600S EPMA, and a ThermoNoran-Voyager 4.3 automation system, are presented and compared with the ones used in other laboratories. The influence of instrumental factors and spectral overlaps on Th, U, and Pb quantification is discussed. Applied procedures to interference correction, error propagation, data treatment, and fi nal chemical age presentation as well as to sampling and analyses are emphasized. Some typical applications are discussed, drawing attention to the most relevant aspects of electron microprobe dating. (author)

  4. 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)

  5. 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....

  6. Triethylamine-assisted Mg(OH)2 coprecipitation/preconcentration for determination of trace metals and rare earth elements in seawater by inductively coupled plasma mass spectrometry (ICP-MS).

    Science.gov (United States)

    Arslan, Zikri; Oymak, Tulay; White, Jeremy

    2018-05-30

    In this paper, we report an improved magnesium hydroxide, Mg(OH) 2 , coprecipitation method for the determination of 16 trace elements (Al, V, Cr, Mn, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Sb, Sn and Pb) and 18 rare earth elements (REEs), including Sc, Y, U and Th in seawater and estuarine water samples. The procedure involves coprecipitation of the trace elements and REEs on Mg(OH) 2 upon addition of a small volume of triethylamine (TEA) followed by analysis of the dissolved pellet solutions by inductively coupled plasma mass spectrometry (ICP-MS). Three-step sequential coprecipitation was carried out on 10 mL aliquots of seawater to eliminate the matrix ions and to preconcentrate the analytes of interest into a 1 mL final volume. Spike recoveries varied from 85% (Th) to 105% (Y). Calcium (Ca), sodium (Na) and potassium (K) matrices were virtually eliminated from the analysis solutions. Collision reaction interface (CRI) technology utilizing H 2 and He gases was employed to determine its effectiveness in removing the spectral interferences originating from the residual Mg matrix, TEA and plasma gases. H 2 was more effective than He in reducing spectral interferences from TEA and plasma gases. Limits of detection (LODs) ranged from 0.01 ng L -1 (Ho) to 72 ng L -1  (Al). The method was validated by using certified seawater (CASS-4) and estuarine water (SLEW-3) reference materials. Precision for five (n = 5) replicate measurements were between 1.2% (Pr) and 18% (Lu). Fe, Pb, Sn, and Zn impurities in TEA were significant in comparison to the levels in CASS-4 and SLEW-3, while relatively high background signals impacted determinations of low levels of Sc and Th. The effects of these hurdles on precision and accuracy were alleviated by measuring these elements in spiked CASS-4 and SLEW-3. Copyright © 2018 Elsevier B.V. All rights reserved.

  7. Correcting for long-alpha stopping distances in (U-Th)/He dating

    Science.gov (United States)

    Glotzbach, Christoph; Lang, Karl; Avdievitch, Nikita; Flowers, Rebecca; Metcalf, James; Ehlers, Todd

    2017-04-01

    factors from photomicrographs taken at multiple perspectives that include images where the crystallographic c-axis of grains perpendicular to the field of view. This approach works on grains of any shape, as the 3D grain shape is numerically approximated directly from photomicrographs. A Monte Carlo simulation is then used to calculate the Ft correction factor. Preliminary applications of this new approach suggest that it is best applied to calculate Ft correction factors of broken grains and for those grains with abnormal shapes not well described by typical shapes used in the prior derivation of analytical solutions. In the latter case Ft values can be >10% different, largely exceeding the analytical error. Future MicroCT analyses may allow for quantitative evaluation of the accuracy of the numerical and traditional measurement approaches. References Dobson, K.J., Stuart, F.M., Dempster, T.J. 2008. U and Th zonation in Fish Canyon Tuff zircons: implications for a zircon (U-Th)/He standard. Geochim. Cosmochim. Acta 72, 4745-4755. Farley, K.A., Wolf, R.A., Silver, L.T. 1996.The effects of long alpha-stopping distances on (U-Th)/He ages. Geochim. Cosmochim. Acta 60, 4223-4229. Horne, A.M., van Soest, M.C., Hodges, K.V., Tripathy-Lang, A., Hourigan, J.K. 2016. Integrated single crystal laser ablation U/Pb and (U-Th)/He dating of detrital accessory minerals - Proof-of-concept studies of titanites and zircons from the Fish Canyon tuff. Geochim. Cosmochim. Acta 178, 106-123. Ketcham, R.A., Gautheron, C., Tassan-Got, L. 2011. Accounting for long alpha-particle stopping distances in (U-Th-Sm)/He geochronology: refinement of the baseline case. Geochim. Cosmochim. Acta 75, 7779-7791.

  8. 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.

  9. Development of an accurate, sensitive, and robust isotope dilution laser ablation ICP-MS method for simultaneous multi-element analysis (chlorine, sulfur, and heavy metals) in coal samples

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, Sergei F. [University of Natural Resources and Applied Life Sciences, Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, Vienna (Austria); Johannes Gutenberg-University, Institute of Inorganic Chemistry and Analytical Chemistry, Mainz (Germany); Heilmann, Jens; Heumann, Klaus G. [Johannes Gutenberg-University, Institute of Inorganic Chemistry and Analytical Chemistry, Mainz (Germany); Prohaska, Thomas [University of Natural Resources and Applied Life Sciences, Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, Vienna (Austria)

    2007-10-15

    A method for the direct multi-element determination of Cl, S, Hg, Pb, Cd, U, Br, Cr, Cu, Fe, and Zn in powdered coal samples has been developed by applying inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with laser-assisted introduction into the plasma. A sector-field ICP-MS with a mass resolution of 4,000 and a high-ablation rate laser ablation system provided significantly better sensitivity, detection limits, and accuracy compared to a conventional laser ablation system coupled with a quadrupole ICP-MS. The sensitivity ranges from about 590 cps for {sup 35}Cl{sup +} to more than 6 x 10{sup 5} cps for {sup 238}U{sup +} for 1 {mu}g of trace element per gram of coal sample. Detection limits vary from 450 ng g{sup -1} for chlorine and 18 ng g{sup -1} for sulfur to 9.5 pg g{sup -1} for mercury and 0.3 pg g{sup -1} for uranium. Analyses of minor and trace elements in four certified reference materials (BCR-180 Gas Coal, BCR-331 Steam Coal, SRM 1632c Trace Elements in Coal, SRM 1635 Trace Elements in Coal) yielded good agreement of usually not more than 5% deviation from the certified values and precisions of less than 10% relative standard deviation for most elements. Higher relative standard deviations were found for particular elements such as Hg and Cd caused by inhomogeneities due to associations of these elements within micro-inclusions in coal which was demonstrated for Hg in SRM 1635, SRM 1632c, and another standard reference material (SRM 2682b, Sulfur and Mercury in Coal). The developed LA-ICP-IDMS method with its simple sample pretreatment opens the possibility for accurate, fast, and highly sensitive determinations of environmentally critical contaminants in coal as well as of trace impurities in similar sample materials like graphite powder and activated charcoal on a routine basis. (orig.)

  10. U-Pb detrital zircon geochronology from the basement of the Central Qilian Terrane: implications for tectonic evolution of northeastern Tibetan Plateau

    Science.gov (United States)

    Liu, Changfeng; Wu, Chen; Zhou, Zhiguang; Yan, Zhu; Jiang, Tian; Song, Zhijie; Liu, Wencan; Yang, Xin; Zhang, Hongyuan

    2018-03-01

    The Tuolai Group dominates the Central Qilian Terrane, and there are different opinions on the age and tectonic attribute of the Tuolai Group. Based on large-scale geologic mapping and zircon dating, the Tuolai Group is divided into four parts: metamorphic supracrustal rocks, Neoproterozoic acid intrusive rocks, early-middle Ordovician acid intrusive rocks and middle Ordovician basic intrusive rocks. The metamorphic supracrustal rocks are the redefined Tuolai complex-group and include gneiss and schist assemblage by faulting contact. Zircon U-Pb LA-MC-ICP-MS dating was conducted on these samples of gneiss and migmatite from the gneiss assemblage, quartzite, two-mica schist and slate from the schist assemblage. The five detrital samples possess similar age spectra; have detrital zircon U-Pb main peak ages of 1.7 Ga with youngest U-Pb ages of 1150 Ma. They are intruded by Neoproterozoic acid intrusive rocks. Therefore, the Tuolai Group belonging to late Mesoproterozoic and early Neoproterozoic. With this caveat in mind, we believe that U-Pb detrital zircon dating, together with the geologic constraints obtained from this study and early work in the neighboring regions. We suggest that the formation age of the entire crystalline basement rocks of metasedimentary sequence from the Central Qilian Terrane should be constrained between the Late Mesoproterozoic and the Late Neoproterozoic, but not the previous Paleoproterozoic. The basement of the Central Qilian Terrane contains the typical Grenville ages, which indicates the Centre Qilian Terrane have been experienced the Grenville orogeny event.

  11. Geology, geochemistry, and geochronology (U-Pb) of the Rio Fortuna Gneiss - Serra do Bau intrusive Suite - Paragua Terrane SW Amazonian Craton

    Energy Technology Data Exchange (ETDEWEB)

    Faria, Debora Almeida; Ruiz, Amarildo Salina; Matos, Joao Batista; Sousa, Maria Zelia Aguiar de; Lima, Gabrielle Aparecida de [Research Group on Crustal and Tectonic Evolution, Guapore, RS (Brazil); Universidade Federal de Mato Grosso (ICET/UFMT), Cuiaba, MT (Brazil). Instituto de Ciencias Exatas e da Terra; Inst. Nacional de Ciencia e Tecnologia de Geociencias da Amazonia (GEOCIAM), Belem, PA (Brazil); Moacir Jose Buenano Macambira, E-mail: defaal.debora@gmail.com, E-mail: gabilimagel@gmail.com, E-mail: asruiz@gmail.com, E-mail: jmatos@ufmt.br, E-mail: prof.mzaguiar@gmail.com, E-mail: moamac@ufpa.br [Research Group on Crustal and Tectonic Evolution, Guapore, RS (Brazil); Universidade Federal do Para (UFPA), Belem, PA (Brazil)

    2014-07-01

    The Rio Fortuna Gneiss crops out in the Serra Santa Barbara, near the Fortuna military headquarters, on the Brazil-Bolivia border. These orthogneisses are located in a portion of the Paragua terrain affected by the Sunsas Orogeny (1.0-0.9 Ga.). They are classified as monzo to granodiorite orthogneisses and underwent at least three episodes of deformation. The U-Pb zircon age of 1,711 ± 13 Ma obtained by laser ablation MC-ICP-MS is interpreted as the crystallization age of this orthogneiss. Geochemically, these rocks form a sequence comprising acidic subalkaline magmatism, calc-alkalic-type high-K, and metaluminous to peraluminous. (author)

  12. 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

  13. 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.

  14. 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.

  15. A convenient approach to 10-12 g/ g ICP-MS limits for Th and U in aurubis electrolytic NA-ESN brand copper

    Science.gov (United States)

    Leonard, Douglas S.

    2014-06-01

    Inductively-coupled-plasma mass spectroscopy is a powerful technique for measuring trace levels of radioactive contaminants, specifically Th and U, in materials for use in construction of low-background rare-event detectors such as double beta decay and dark matter detectors. I describe here a technique for measuring Th and U contamination in copper by using direct acid digestion and dilution without further chemical processing, achieving results comparable to those achieved in previous work [1, 2] which utilized more complex chemical pre-concentration techniques. A convenient research-oriented analysis environment is described as well. Results are presented for measurements of three samples from the production line of electrolytically-purified, LME (London Metal Exchange) grade A, NA-ESN Aurubis copper. Purified samples showed levels consistent with zero contamination for both elements, while weak, but inconclusive, indications of contamination were present for the unpurified anode copper. The best limits achieved are near 1•10-12 g/ g (95% CL) for both Th and U measured for copper from the cathode of the purification process.

  16. 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.)

  17. 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)

  18. 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.)

  19. 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.

  20. 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

  1. Determination of trace levels of uranium and thorium in high purity gadolinium sulfate using the ICP-MS with solid-phase chromatographic extraction resin

    Science.gov (United States)

    Ito, S.; Takaku, Y.; Ikeda, M.; Kishimoto, Y.

    2017-11-01

    The new Super-Kamiokande-Gadolinium (SK-Gd) project is an upgrade of the Super-Kamiokande (SK) detector. In the SK-Gd project, 0.2% Gd_2(SO_4)_3 is loaded into the 50 kton water tank of the SK. One of the main purposes of the project is to discover supernova relic neutrinos. Neutrino measurements and proton decay searches will also be performed in the SK-Gd. In order to measure solar neutrinos with a low energy threshold of ˜3.5 MeV in the SK-Gd, the main radioactive contaminations, ^{238}U and ^{232}Th, in Gd_2(SO_4)_3{\\cdot}8H_2O, should be minimized before loading. Our maximum levels for U and Th are 5 mBq (U)/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) and 0.05 mBq (Th)/kg (Gd_2(SO_4)_3{\\cdot}8H_2O). In order to measure such low concentrations of U and Th in Gd_2(SO_4)_3{\\cdot}8H_2O, we developed the solid-phase extraction technique. Using this method, about 90% or more U and Th could be efficiently extracted while Gd was reduced by a factor of about 104. This allowed these radioactivity contaminations to be measured precisely as 0.04 mBq/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) for U and 0.01 mBq/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) for Th. We measured three pure Gd_2(SO_4)_3{\\cdot}8H_2O samples using this method and estimated that the purest one contained <0.04 mBq (U)/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) and 0.06 ± 0.01 mBq (Th)/kg (Gd_2(SO_4)_3{\\cdot}8H_2O) by the ICP-MS.

  2. 230Th-234U Model-Ages of Some Uranium Standard Reference Materials

    Energy Technology Data Exchange (ETDEWEB)

    Williams, R W; Gaffney, A M; Kristo, M J; Hutcheon, I D

    2009-05-28

    The 'age' of a sample of uranium is an important aspect of a nuclear forensic investigation and of the attribution of the material to its source. To the extent that the sample obeys the standard rules of radiochronometry, then the production ages of even very recent material can be determined using the {sup 230}Th-{sup 234}U chronometer. These standard rules may be summarized as (a) the daughter/parent ratio at time=zero must be known, and (b) there has been no daughter/parent fractionation since production. For most samples of uranium, the 'ages' determined using this chronometer are semantically 'model-ages' because (a) some assumption of the initial {sup 230}Th content in the sample is required and (b) closed-system behavior is assumed. The uranium standard reference materials originally prepared and distributed by the former US National Bureau of Standards and now distributed by New Brunswick Laboratory as certified reference materials (NBS SRM = NBL CRM) are good candidates for samples where both rules are met. The U isotopic standards have known purification and production dates, and closed-system behavior in the solid form (U{sub 3}O{sub 8}) may be assumed with confidence. We present here {sup 230}Th-{sup 234}U model-ages for several of these standards, determined by isotope dilution mass spectrometry using a multicollector ICP-MS, and compare these ages with their known production history.

  3. 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

  4. Determination of 11 trace elements in U3O8 CRMs by ICP-AES

    International Nuclear Information System (INIS)

    Liu Husheng

    1994-01-01

    The TBP extractant-containing resin and extraction chromatography technique were used to separate 11 trace elements in U 3 O 8 CRMs. The sample was separated at a flow rate of 0.5 mL/min with 3 mol/L HNO 3 as medium. A model 975 ICP direct reading spectrometer was used to determine the trace elements of Ca, Cd, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb and Sn in U 3 O 8 CRMs. The lowest quantitatively determinable concentration of impurities in U 3 O 8 CRMs are 0.02-1.6 μg/g. The RSD is less than 10%. The proposed method provides excellent and accurate analytical data for the U 3 O 8 samples prepared as certified reference materials (CRMs)

  5. Inductively coupled plasma – Tandem mass spectrometry (ICP-MS/MS): A powerful and universal tool for the interference-free determination of (ultra)trace elements – A tutorial review

    Energy Technology Data Exchange (ETDEWEB)

    Balcaen, Lieve; Bolea-Fernandez, Eduardo [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium); Resano, Martín [University of Zaragoza, Department of Analytical Chemistry, Pedro Cerbuna 12, E-50009 Zaragoza (Spain); Vanhaecke, Frank, E-mail: Frank.Vanhaecke@UGent.be [Ghent University, Department of Analytical Chemistry, Krijgslaan 281-S12, B-9000 Ghent (Belgium)

    2015-09-24

    This paper is intended as a tutorial review on the use of inductively coupled plasma – tandem mass spectrometry (ICP-MS/MS) for the interference-free quantitative determination and isotope ratio analysis of metals and metalloids in different sample types. Attention is devoted both to the instrumentation and to some specific tools and procedures available for advanced method development. Next to the more typical reaction gases, e.g., H{sub 2}, O{sub 2} and NH{sub 3}, also the use of promising alternative gases, such as CH{sub 3}F, is covered, and the possible reaction pathways with those reactive gases are discussed. A variety of published applications relying on the use of ICP-MS/MS are described, to illustrate the added value of tandem mass spectrometry in (ultra)trace analysis. - Highlights: • First review on tandem ICP-mass spectrometry (ICP-MS/MS). • Clear description of operating principles of ICP-MS/MS. • Description on how to make use of product ion scans, precursor ion scans and neutral gain scans in method development. • Overview of applications published so far.

  6. Inductively coupled plasma – Tandem mass spectrometry (ICP-MS/MS): A powerful and universal tool for the interference-free determination of (ultra)trace elements – A tutorial review

    International Nuclear Information System (INIS)

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

    2015-01-01

    This paper is intended as a tutorial review on the use of inductively coupled plasma – tandem mass spectrometry (ICP-MS/MS) for the interference-free quantitative determination and isotope ratio analysis of metals and metalloids in different sample types. Attention is devoted both to the instrumentation and to some specific tools and procedures available for advanced method development. Next to the more typical reaction gases, e.g., H_2, O_2 and NH_3, also the use of promising alternative gases, such as CH_3F, is covered, and the possible reaction pathways with those reactive gases are discussed. A variety of published applications relying on the use of ICP-MS/MS are described, to illustrate the added value of tandem mass spectrometry in (ultra)trace analysis. - Highlights: • First review on tandem ICP-mass spectrometry (ICP-MS/MS). • Clear description of operating principles of ICP-MS/MS. • Description on how to make use of product ion scans, precursor ion scans and neutral gain scans in method development. • Overview of applications published so far.

  7. 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)

  8. Th-U-Pb{sub T} dating by electron probe microanalysis, Part I. Monazite: analytical procedures and data treatment

    Energy Technology Data Exchange (ETDEWEB)

    Vlach, Silvio Roberto Farias [Universidade de Sao Paulo (USP), Sao Carlos, SP (Brazil). Inst. de Geociencias. Dept. de Mineralogia e Geotectonica], e-mail: srfvlach@usp.br

    2010-03-15

    Dating methodology by the electron probe microanalyser (EPMA) of (Th, U)-bearing minerals, highlighting monazite, acquired greater than ever importance in literature, particularly due to its superior spatial resolution, as well as versatility, which allow correlating petrological processes at times registered only in micro-scales in minerals and rocks with absolute ages. Although the accuracy is inferior to the one achieved with conventional isotopic methods in up to an order of magnitude, EPMA is the instrument that allows the best spatial resolution, reaching a few {mu}m{sup 3} in some conditions. Quantification of minor and trace elements with suitable precision and accuracy involves the own instrumental and analytical set-ups and data treatment strategies, significantly more rigorous when compared with those applied in conventional analyses. Th-U-Pb{sub T} dating is an example of these cases. Each EPMA is a unique machine as for its instrumental characteristics and respective automation system. In such a way, analytical procedures ought to be adjusted for laboratory specific cities. The analytical strategies and data treatment adopted in the Electronic Microprobe Laboratory from Instituto de Geociencias of Universidade de Sao Paulo, Brazil, with a JEOL JXA8600S EPMA, and a ThermoNoran-Voyager 4.3 automation system, are presented and compared with the ones used in other laboratories. The influence of instrumental factors and spectral overlaps on Th, U, and Pb quantification is discussed. Applied procedures to interference correction, error propagation, data treatment, and final chemical age presentation as well as to sampling and analyses are emphasized. Some typical applications are discussed, drawing attention to the most relevant aspects of electron microprobe dating. (author)

  9. Columbite-Group Minerals from New York Pegmatites: Insights from Isotopic and Geochemical Analyses

    Directory of Open Access Journals (Sweden)

    Marian V. Lupulescu

    2018-05-01

    Full Text Available Columbite crystals from niobium-yttrium-fluorine (NYF pegmatites lacking zircon or containing metamict cyrtolite were analyzed for major and minor elements (Electron Microprobe (EMP, trace elements (Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS, and U-Pb geochronology (Laser AblationMulti-Collector-Inductively Coupled Plasma-Mass Spectrometry (LA-MC-ICP-MS. All four pegmatite localities sampled are hosted by the Proterozoic Fordham gneiss and/or Paleozoic Bedford gneiss (Columbite-(Fe; Kinkel and Baylis localities and the Manhattan Schist of Lower Paleozoic age (Columbite-(Mn; Fort George and Harlem River Drive localities and yield Neoacadian ages. The weighted average U-Pb ages are 372.2 ± 8.2 Ma (Baylis Quarry, 371.3 ± 7.3 and 383.4 ± 8.9 Ma (Kinkel Quarry; 383 ± 15 Ma (185th St. and Harlem River Drive; and 372 ± 10 Ma (Fort George. A partial metamict zircon (“cyrtolite” from the Kinkel Quarry yielded a weighted average U-Pb age of 376.9 ± 4.3 Ma. The Neoacadian ages obtained agree with those determined by thermal ionization mass spectrometry (TIMS for zircon from Lithium-Cesium-Tantalum (LCT pegmatites from Connecticut and Maine. No pegmatites temporally associated with the Taconic orogeny were found. The size, lack of common Pb, uniform U concentrations across crystal cross-sections, sufficient but moderate uranium concentrations, lack of metamictization, and consistency in U-Pb isotopic ratios for columbite samples BCB-COL, NYSM #25232, and NYSM #525.8 suggests they show promise as potential standards for oxide mineral LA-MC-ICP-MS geochronological analyses, however, additional characterization using ID-TIMS would be necessary to develop as such.

  10. Lead Isotopic Composition in Biogenic Certified Reference Materials Determined by Different ICP-based Mass Spectrometric Techniques

    Czech Academy of Sciences Publication Activity Database

    Ďurišová, J.; Ackerman, L.; Strnad, L.; Chrastný, V.; Borovička, Jan

    2015-01-01

    Roč. 39, č. 2 (2015), s. 209-220 ISSN 1639-4488 R&D Projects: GA ČR(CZ) GAP504/11/0484 Institutional support: RVO:61389005 Keywords : Pb isotopes * Pb-206 * Pb-207 * Pb-208 * ICP-MS * certified reference materials * vegetation Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.885, year: 2015

  11. 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

  12. 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)

  13. Influence of metal loading and humic acid functional groups on the complexation behavior of trivalent lanthanides analyzed by CE-ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Kautenburger, Ralf, E-mail: r.kautenburger@mx.uni-saarland.de [Institute of Inorganic Solid State Chemistry, Saarland University, Campus Dudweiler, Am Markt Zeile 3-5, D-66125 Saarbrücken (Germany); Hein, Christina; Sander, Jonas M. [Institute of Inorganic Solid State Chemistry, Saarland University, Campus Dudweiler, Am Markt Zeile 3-5, D-66125 Saarbrücken (Germany); Beck, Horst P. [Institute of Inorganic and Analytical Chemistry and Radiochemistry, Saarland University, Campus Dudweiler, Am Markt Zeile 5, D-66125 Saarbrücken (Germany)

    2014-03-01

    Highlights: • Free and complexed HA-Ln species are separated by CE-ICP-MS. • Weaker and stronger HA-binding sites for Ln-complexation can be detected. • Complexation by original and modified humic acid (HA) with blocked phenolic hydroxyl- and carboxyl-groups is compared. • Stronger HA-binding sites for Ln³⁺ can be assumed as chelating complexes. • Chelates consist of trivalent Ln and a combination of both OH- and COOH-groups. Abstract: The complexation behavior of Aldrich humic acid (AHA) and a modified humic acid (AHA-PB) with blocked phenolic hydroxyl groups for trivalent lanthanides (Ln) is compared, and their influence on the mobility of Ln(III) in an aquifer is analyzed. As speciation technique, capillary electrophoresis (CE) was hyphenated with inductively coupled plasma mass spectrometry (ICP-MS). For metal loading experiments 25 mg L⁻¹ of AHA and different concentrations (c Ln(Eu+Gd)} = 100–6000 μg L⁻¹) of Eu(III) and Gd(III) in 10 mM NaClO₄ at pH 5 were applied. By CE-ICP-MS, three Ln-fractions, assumed to be uncomplexed, weakly and strongly AHA-complexed metal can be detected. For the used Ln/AHA-ratios conservative complex stability constants log βLnAHA decrease from 6.33 (100 μg L⁻¹ Ln³⁺) to 4.31 (6000 μg L⁻¹ Ln³⁺) with growing Ln-content. In order to verify the postulated weaker and stronger humic acid binding sites for trivalent Eu and Gd, a modified AHA with blocked functional groups was used. For these experiments 500 μg L⁻¹ Eu and 25 mg L⁻¹ AHA and AHA-PB in 10 mM NaClO₄ at pH-values ranging from 3 to 10 have been applied. With AHA-PB, where 84% of the phenolic OH-groups and 40% of the COOH-groups were blocked, Eu complexation was significantly lower, especially at the strong binding sites. The log β-values decrease from 6.11 (pH 10) to 5.61 at pH 3 (AHA) and for AHA-PB from 6.01 (pH 7) to 3.94 at pH 3. As a potential consequence, particularly humic acids with a high amount of

  14. U-Th isotopic systematics at 13deg N east Pacific Ridge segment

    International Nuclear Information System (INIS)

    Ben Othman, D.; Allegre, C.J.

    1990-01-01

    Fresh basaltic glasses have been analyzed for U-Th disequilibrium systematics as part of an extensive study on the East Pacific Rise (EPR) at 12deg 45'N. These samples are well described in terms of major and trace elements as well as in Nd, Pb and Sr isotopes. Our results show significant heterogeneities in the mantle source at a small scale, and show heterogeneities at larger scales also when compared to other EPR data. U and Th concentration and isotopic data rule out fractional crystallization as a main process and support a mixing model in agreement with the marble cake model developed by Allegre and Turcotte and constrained by trace elements and Nd, Sr and Pb isotopes on the same samples by Prinzhofer et al. Based on the high ( 230 Th/ 232 Th) isotopic ratios on recent tholeiites especially the Th/U values inferred for their sources clearly show that the upper mantle Th/U has decreased with time. (orig.)

  15. 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.

  16. 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.

  17. 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....

  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. 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.

  20. 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

  1. 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

  2. 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

  3. 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

  4. 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,

  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. 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)

  7. 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.

  8. 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.)

  9. 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.

  10. 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.)

  11. [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).

  12. Two age populations of zircons from the Timber Creek kimberlites, Northern Territory, as determined by laser-ablation ICP-MS analysis

    International Nuclear Information System (INIS)

    Belousova, E.A.; Jackson, S.E.; O'Reilly, S.Y.; Griffin, W.L.

    2001-01-01

    Two populations of kimberlitic zircon are present in the Timber Creek kimberlites, Northern Territory. Laser-ablation ICP-MS U-Pb dating yields an age of 1483 ± 15 (2σ) Ma for the main group and an age of 179 ± 2 Ma for the other group. This distinction of two age groups is strongly supported by Hf isotope data on the same zircons. Although the trace-element patterns of both populations are typical of mantle-derived zircons, the 'young' population has slightly higher concentrations of most trace elements, but has lower Hf, Nb, Ta and Pb contents. The distinct differences in trace-element contents and Hf isotopic composition of the two zircon populations indicate that they were derived from different magma sources. The dating results indicate that the emplacement age of the Timber Creek kimberlites cannot be older than the age of the 'young' zircon population (i.e. 179 ± 2 Ma). This clarifies the inconsistency between the previously reported SHRIMP age of the Timber Creek zircons (1462 ± 53 Ma) and the much younger age (1200Ma) of the sediments of the Victoria River Basin into which these kimberlites have intruded. The Timber Creek kimberlites are a newly recognised extension of the widespread Jurassic kimberlite activity known in Western Australia and South Australia. Copyright (2001) Geological Society of Australia

  13. 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)

  14. 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)

  15. 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

  16. Temporal evolution of the giant Salobo IOCG deposit, Carajás Province (Brazil): constraints from paragenesis of hydrothermal alteration and U-Pb geochronology

    Science.gov (United States)

    deMelo, Gustavo H. C.; Monteiro, Lena V. S.; Xavier, Roberto P.; Moreto, Carolina P. N.; Santiago, Erika S. B.; Dufrane, S. Andrew; Aires, Benevides; Santos, Antonio F. F.

    2017-06-01

    The giant Salobo copper-gold deposit is located in the Carajás Province, Amazon Craton. Detailed drill core description, petrographical studies, and U-Pb SHRIMP IIe and LA-ICP-MS geochronology unravel its evolution regarding the host rocks, hydrothermal alteration and mineralization. Within the Cinzento Shear Zone, the deposit is hosted by orthogneisses of the Mesoarchean Xingu Complex (2950 ± 25 and 2857 ± 6.7 Ma) and of the Neoarchean Igarapé Gelado suite (2763 ± 4.4 Ma), which are crosscut by the Old Salobo granite. Remnants of the Igarapé Salobo metavolcanic-sedimentary sequence are represented by a quartz mylonite with detrital zircon populations (ca. 3.1-3.0, 2.95, 2.86, and 2.74 Ga). High-temperature calcic-sodic hydrothermal alteration (hastingsite-actinolite) was followed by silicification, iron-enrichment (almandine-grunerite-magnetite), tourmaline formation, potassic alteration with biotite, copper-gold ore formation, and later Fe-rich hydrated silicate alteration. Myrmekitic bornite-chalcocite and magnetite comprise the bulk of copper-gold ore. All these alteration assemblages have been overprinted by post-ore hematite-bearing potassic and propylitic alteration, which is also recognized in the Old Salobo granite. In the central zone of the deposit the mylonitized Igarapé Gelado suite rocks yield an age of 2701 ± 30 Ma. Zircon ages of 2547 ± 5.3 and 2535 ± 8.4 Ma were obtained for the Old Salobo granite and for the high-grade copper ore, respectively. A U-Pb LA-ICP-MS monazite age (2452 ± 14 Ma) from the copper-gold ore indicates hydrothermal activity and overprinting in the Siderian. Therefore, a protracted tectono-thermal event due to the reactivation of the Cinzento Shear Zone is proposed for the evolution of the Salobo deposit.

  17. 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.

  18. Quantification of "2"3"2Th, "2"3"4U, "2"3"5U and "2"3"8U in river mollusks by magnetic sector mass spectrometry with inductively coupled plasma source (Icp-SFMS)

    International Nuclear Information System (INIS)

    Arevalo R, D. L.; Hernandez M, H.; Romero G, E. T.; Lara A, N.; Alfaro de la T, M. C.

    2016-09-01

    The present work deals with the methodology established for the quantification of "2"3"2Th, "2"3"4U, "2"3"8U and "2"3"5U in the shell of gastropod mollusks collected in the rivers Valles, Coy and Axtla of San Luis Potosi, Mexico, which belong to the Panuco River basin; these rivers have as main source of pollution the discharge of municipal sewage, waste from small industries, agricultural and cattle residues and from natural sources. Conventional methods for measuring radio-nuclides are confronted with certain conditions related to the requirement in measurement, basically in the characterization that is related to the concepts of precision and accuracy. The analysis of the gastropod mollusk shell was performed by the Icp-SFMS technique; the main advantages of this technique lie in the isotope quantification capacity, the high precision and the low limits of detection, in this study are very important because these elements are in concentrations between ppb and ppt. This technique allowed the analysis of the samples having a complex matrix by the presence CaCO_3 minimizing the interferences thanks to the ionization efficiency of the Ar plasma. For the species Pachychilus monachus were found concentrations of "2"3"2Th of 0.16-5.37 μg/g and of total U of 0.101-4.081 μg/g being this species where the highest values of total U were found. For Thiara (melanoids) tuberculata the lowest values were found among the different species ("2"3"2Th 0.61-3.61 μg/g and total U 0.006-0.042 μg/g), for Pachychilus suturalis, values of "2"3"2Th of 0.58-6.4 μg/g and for Pachychilus sp. were found between 0.26-7.62 μg/g and for total U values between 0.28-3.33 μg/g. The method offers several advantages: speed, good precision, low values of quantification limits and high sensitivity in the measurement of radio-nuclides and heavy metals. (Author)

  19. Determination of (90)Sr in soil samples using inductively coupled plasma mass spectrometry equipped with dynamic reaction cell (ICP-DRC-MS).

    Science.gov (United States)

    Feuerstein, J; Boulyga, S F; Galler, P; Stingeder, G; Prohaska, T

    2008-11-01

    A rapid method is reported for the determination of (90)Sr in contaminated soil samples in the vicinity of the Chernobyl Nuclear Power Plant by ICP-DRC-MS. Sample preparation and measurement procedures focus on overcoming the isobaric interference of (90)Zr, which is present in soils at concentrations higher by more than six orders of magnitude than (90)Sr. Zirconium was separated from strontium in two steps to reduce the interference by (90)Zr(+) ions by a factor of more than 10(7): (i) by ion exchange using a Sr-specific resin and (ii) by reaction with oxygen as reaction gas in a dynamic reaction cell (DRC) of a quadrupole ICP-MS. The relative abundance sensitivity of the ICP-MS was studied systematically and the peak tailing originating from (88)Sr on mass 90 u was found to be about 3 x 10(-9). Detection limits of 4 fg g(-1) (0.02 Bq g(-1)) were achieved when measuring Sr solutions containing no Zr. In digested uncontaminated soil samples after matrix separation as well as in a solution of 5 microg g(-1) Sr and 50 ng g(-1) Zr a detection limit of 0.2 pg g(-1) soil (1 Bq g(-1) soil) was determined. (90)Sr concentrations in three soil samples collected in the vicinity of the Chernobyl Nuclear Power Plant were 4.66+/-0.27, 13.48+/-0.68 and 12.9+/-1.5 pg g(-1) corresponding to specific activities of 23.7+/-1.3, 68.6+/-3.5 and 65.6+/-7.8 Bq g(-1), respectively. The ICP-DRC-MS results were compared to the activities measured earlier by radiometry. Although the ICP-DRC-MS is inferior to commonly used radiometric methods with respect to the achievable minimum detectable activity it represents a time- and cost-effective alternative technique for fast monitoring of high-level (90)Sr contamination in environmental or nuclear industrial samples down to activities of about 1 Bq g(-1).

  20. Determination of 90Sr in soil samples using inductively coupled plasma mass spectrometry equipped with dynamic reaction cell (ICP-DRC-MS)

    International Nuclear Information System (INIS)

    Feuerstein, J.; Boulyga, S.F.; Galler, P.; Stingeder, G.; Prohaska, T.

    2008-01-01

    A rapid method is reported for the determination of 90 Sr in contaminated soil samples in the vicinity of the Chernobyl Nuclear Power Plant by ICP-DRC-MS. Sample preparation and measurement procedures focus on overcoming the isobaric interference of 90 Zr, which is present in soils at concentrations higher by more than six orders of magnitude than 90 Sr. Zirconium was separated from strontium in two steps to reduce the interference by 90 Zr + ions by a factor of more than 10 7 : (i) by ion exchange using a Sr-specific resin and (ii) by reaction with oxygen as reaction gas in a dynamic reaction cell (DRC) of a quadrupole ICP-MS. The relative abundance sensitivity of the ICP-MS was studied systematically and the peak tailing originating from 88 Sr on mass 90 u was found to be about 3 x 10 -9 . Detection limits of 4 fg g -1 (0.02 Bq g -1 ) were achieved when measuring Sr solutions containing no Zr. In digested uncontaminated soil samples after matrix separation as well as in a solution of 5 μg g -1 Sr and 50 ng g -1 Zr a detection limit of 0.2 pg g -1 soil (1 Bq g -1 soil) was determined. 90 Sr concentrations in three soil samples collected in the vicinity of the Chernobyl Nuclear Power Plant were 4.66 ± 0.27, 13.48 ± 0.68 and 12.9 ± 1.5 pg g -1 corresponding to specific activities of 23.7 ± 1.3, 68.6 ± 3.5 and 65.6 ± 7.8 Bq g -1 , respectively. The ICP-DRC-MS results were compared to the activities measured earlier by radiometry. Although the ICP-DRC-MS is inferior to commonly used radiometric methods with respect to the achievable minimum detectable activity it represents a time- and cost-effective alternative technique for fast monitoring of high-level 90 Sr contamination in environmental or nuclear industrial samples down to activities of about 1 Bq g -1

  1. Determination of Th and REE in columbite - tantalite samples by ICP-OES

    International Nuclear Information System (INIS)

    Hanuman, V.V.; Khorge, C.R.; Radhamai, R.; Nair, Sajitha; Srivastava, P.K.

    2007-01-01

    A simple method of decomposition and separation of Th and REE in columbite- tantalite is developed for determination by ICP- OES. The sample is decomposed with hydrofluoric and hydrochloric acid in presence of little sulphuric acid to avoid drying on water bath. Th and rare earths are separated as fluoride together with undecomposed sample. The residue is fused with a 1: 1 mixture of sodium di hydrogen orthophosphate and sodium pyrophosphate. The melt is dissolved in water for measurement. Nitric acid is found unsuitable due to loss in Ce in some of the samples. Matrix elements (more than 97.5) are removed in single step by both the treatments. The free cassiterite present in samples is not attacked during acid digestion. However, the same is easily decomposed in fusion. U (IV) is also precipitated along with Th and REE when hydrochloric acid is used. As expected uranium is lost when nitric acid is used. The results are compared with existing well-established procedure involving peroxide fusion for decomposition; hydroxide and fluoride precipitation separation. Both the methods yielded comparable result. The method is simple, comparatively rapid and suitable for routine application for determination of REE , Th and U(IV) content. The RSD of the method was found to be in the range of 1- 1.5% for various elements. (author)

  2. The 230Th correction is the 1st priority for accurate dates of young zircons: U/Th partitioning experiments and measurements

    Science.gov (United States)

    Krawczynski, M.; McLean, N.

    2017-12-01

    One of the most accurate and useful ways of determining the age of rocks that formed more than about 500,000 years ago is uranium-lead (U-Pb) geochronology. Earth scientists use U-Pb geochronology to put together the geologic history of entire regions and of specific events, like the mass extinction of all non-avian dinosaurs about 66 million years ago or the catastrophic eruptions of supervolcanoes like the one currently centered at Yellowstone. The mineral zircon is often utilized because it is abundant, durable, and readily incorporates uranium into its crystal structure. But it excludes thorium, whose isotope 230Th is part of the naturally occurring isotopic decay chain from 238U to 206Pb. Calculating a date from the relative abundances of 206Pb and 238U therefore requires a correction for the missing 230Th. Existing experimental and observational constraints on the way U and Th behave when zircon crystallizes from a melt are not known precisely enough, and thus currently the uncertainty in dates introduced by they `Th correction' is one of the largest sources of systematic error in determining dates. Here we present preliminary results on our study of actinide partitioning between zircon and melt. Experiments have been conducted to grow zircon from melts doped with U and Th that mimic natural magmas at a range of temperatures, and compositions. Synthetic zircons are separated from their coexisting glass and using high precision and high-spatial-resolution techniques, the abundance and distribution of U and Th in each phase is determined. These preliminary experiments are the beginning of a study that will result in precise determination of the zircon/melt uranium and thorium partition coefficients under a wide variety of naturally occurring conditions. This data will be fit to a multidimensional surface using maximum likelihood regression techniques, so that the ratio of partition coefficients can be calculated for any set of known parameters. The results of

  3. Cenozoic foreland basins of Central Andes: a preliminary provenance U-Pb zircon analysis of sedimentary sequences of Calchaqui Valley

    International Nuclear Information System (INIS)

    Oliveira, Alisson Lopes; Hauser, Natalia; Pimentel, Marcio Martins; Matteini, Massimo; Coira, Beatriz; Alonso, Ricardo; Barrientos, Andrea

    2015-01-01

    The Eocene of northwestern Argentina records complex basin and structural evolution, including continental sedimentation of the post-rift Salta Basin and the beginning of the Andean uplift and foreland system evolution. This illuminates a significant period of evolutionary history of this and surrounding basins in northwestern Argentina. U-Pb zircon analyses by LA-ICP-MS for three formations representing post-rift to foreland stages allowed interpretation about provenance terrains. The Lumbrera Formation, representing the post-rift stage, shows bimodal sources with a main zircon population around 462 Ma, and a second population around 1023 Ma. The Los Colorados and Angastaco Formations representing the sedimentation in a foreland basin, show a unimodal source around 490 Ma, and 517 Ma respectively. Zircons younger than 50 Ma were not identified during this study. (author)

  4. Cenozoic foreland basins of Central Andes: a preliminary provenance U-Pb zircon analysis of sedimentary sequences of Calchaqui Valley

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Alisson Lopes; Hauser, Natalia; Pimentel, Marcio Martins; Matteini, Massimo, E-mail: alisson_oliveira@hotmail.com [Universidade de Brasilia (UnB), DF (Brazil). Laboratorio de Geocronologia; Galli, Claudia Ines [Faculdad de Ingenieria, Universidad Nacional de Jujuy (Argentina); Coira, Beatriz [CIT Jujuy, CONICET. Instituto de Geologia y Mineria (Argentina); Alonso, Ricardo; Barrientos, Andrea [Instituto CEGA, CONICET. Universidad Nacional de Salta (Argentina)

    2015-07-01

    The Eocene of northwestern Argentina records complex basin and structural evolution, including continental sedimentation of the post-rift Salta Basin and the beginning of the Andean uplift and foreland system evolution. This illuminates a significant period of evolutionary history of this and surrounding basins in northwestern Argentina. U-Pb zircon analyses by LA-ICP-MS for three formations representing post-rift to foreland stages allowed interpretation about provenance terrains. The Lumbrera Formation, representing the post-rift stage, shows bimodal sources with a main zircon population around 462 Ma, and a second population around 1023 Ma. The Los Colorados and Angastaco Formations representing the sedimentation in a foreland basin, show a unimodal source around 490 Ma, and 517 Ma respectively. Zircons younger than 50 Ma were not identified during this study. (author)

  5. 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)

  6. 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

  7. 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)

  8. Elemental fractionation in 785 nm picosecond and femtosecond laser ablation inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Shaheen, M.E.; Gagnon, J.E.; Fryer, B.J.

    2015-01-01

    Elemental fractionation and ICP-MS signal response were investigated for two different pulse width laser beams originating from the same laser system. Femtosecond and picosecond laser beams at pulse widths of 130 fs and 110 ps, respectively, and wavelength of 785 nm were used to ablate NIST 610 synthetic glass and SRM 1107 Naval Brass B at the same spot for 800 to 1000 laser pulses at different repetition rates (5 to 50 Hz). Elemental fractionation was found to depend on repetition rate and showed a trend with femtosecond laser ablation that is opposite to that observed in picosecond laser ablation for most measured isotopes. ICP-MS signal intensity was higher in femtosecond than picosecond LA-ICP-MS in both NIST 610 and naval brass when ablation was conducted under the same fluence and repetition rate. The differences in signal intensity were partly related to differences in particle size distribution between particles generated by femtosecond and picosecond laser pulses and the consequent differences in transport and ionization efficiencies. The main reason for the higher signal intensity resulting from femtosecond laser pulses was related to the larger crater sizes compared to those created during picosecond laser ablation. Elemental ratios measured using 66 Zn/ 63 Cu, 208 Pb/ 238 U, 232 Th/ 238 U, 66 Zn/ 232 Th and 66 Zn/ 208 Pb were found to change with the number of laser pulses with data points being more scattered in picosecond than femtosecond laser pulses. Reproducibility of replicate measurements of signal intensities, fractionation and elemental ratios was better for fs-LA-ICP-MS (RSD ~ 3 to 6%) than ps-LA-ICP-MS (RSD ~ 7 to 11%). - Highlights: • Fractionation and ICP-MS signal response were investigated for two different pulse widths using NIST 610 and Naval Brass. • Dependence of fractionation indices on repetition rate and pulse width. • Higher ablation rate was observed in picosecond compared to femtosecond laser ablation of NIST 610 and Brass

  9. 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...

  10. 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.

  11. 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.

  12. U-Pb (LA-ICPMS) zircon ages and Nd isotopes for granitoids of the Tamboril-Santa Quiteria Complex, Ceara Central Domain: implication for neoproterozoic syncollisional magmatism in north Borborema Province, Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Costa, Felipe Grandjean da; Araujo, Carlos Eduardo Ganade de; Vasconcelos, Antonio Maurilio, E-mail: felipe.costa@cprm.gov.br, E-mail: caegeo@gmail.com, E-mail: maurilio.vasconcelos@cprm.gov.br [Servico Geologico do Brasil (CPRM), Fortaleza, CE (Brazil); Amaral, Wagner da Silva, E-mail: wamaral@ufc.br [Universidade Federal do Ceara (UFC), Fortaleza, CE (Brazil). Departamento de Geologia; Rodrigues, Joseneusa Brilhante, E-mail: joseneusa.rodrigues@cprm.gov.br [Servico Geologico do Brasil (CPRM), Brasilia, DF (Brazil)

    2013-06-15

    The Tamboril-Santa Quiteria Complex (TSQC) is one of the largest Neoproterozoic plutonic manifestations in the north Borborema Province (NE Brazil). It represents an anatectic/igneous association characterized by a number of magmatic pulses that occurred in the 650-610 Ma interval. In this paper, we present U-Pb (LA-MC-ICP-MS) zircon ages and Nd isotopes for quartz monzonite and quartz diorites of the southern part of TSQC. The quartz monzonite belong to a hybrid granitoid association, including monzonite, syenites and quartz syenites, all with abundant mafic magmatic enclaves. A quartz monzonite sample yielded a U-Pb zircon age of 634 {+-} 10 Ma and a TDM age of 2.69 Ga. The quartz diorites are much more homogeneous in composition and yielded a U-Pb zircon age of 618 {+-} 23 Ma and a TDM age of 2.19 Ga. The presence of coeval mantle-derived magmatism and diatexites (crustal anatexis) post-dating high-pressure metamorphism (ca. 650 Ma), and together with high-temperature metamorphism (ca. 630-610 Ma), suggests that this large magmatic manifestation evolved in a collisional setting, probably related to slab break off during the Western Gondwana amalgamation. (author)

  13. 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.

  14. 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

  15. 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

  16. 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.

  17. Characterization of nuclear materials by laser ablation ICP(SF)MS for nuclear forensic purposes

    International Nuclear Information System (INIS)

    Stefanka, Z.; Katona, R.; Varga, Z.

    2009-01-01

    Full text: The task of the categorization and characterization of nuclear materials of unknown origin has been delegated to the Institute of Isotopes of the Hungarian Academy of Sciences in 1996 by a governmental decree. Since the investigated materials are forensic evidences special attention was paid for minimizing the required sample amount. Therefore LA-ICP(SF)MS has been developed and also applied for the determination of isotopic composition, production date and the concentration of trace impurities. The LA-ICP(SF)MS methods were validated by inter-laboratory comparisons and were applied for analysis of uranium oxide pellets seized in Hungary. (author)

  18. 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.

  19. 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....

  20. 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

  1. Determination of natural radionuclides, U, Th-232, Ra-226, Ra-228, Pb-210 and K-40 in sediments from CananÉIa-Iguape System, Brazil

    International Nuclear Information System (INIS)

    Jesus, Gleyka J.D.; Chiozzini, Vitor G.; Saueia, Cátia H.R.; Nisti, Marcelo B.; Braga, Elisabete S.; Fávaro, Deborah I.T.; Universidade de São Paulo

    2017-01-01

    The Cananéia-Iguape estuarine-lagoon complex, located in the south of São Paulo State, Brazil, is a protected area recognized by UNESCO as part of the Biosphere Reserve, due to its importance as a natural ecosystem. However, along the years, the mining activities in the region affected the river basin, to such an extent that contamination was observed for As, Cu, Pb and Zn. Since the mining activities can also enhance the levels of natural radioactivity in the sediments, this study aimed to determine the activity concentration of the natural radionuclides (K-40, U, Ra-226, Pb-210, Th-232 and Ra-228) in 34 bottom sediments samples collected in the Cananéia-Iguape system. The samples were measured by gamma spectrometry, using a HPGe for the determination of K-40, Ra-226, Pb-210 and Ra-228. The concentration of U and Th-232 was determined by instrumental neutron activation analysis. The activity concentration of K-40 varied from 119 ± 17 to 522 ± 74 Bq kg"-"1; U-238 varied from 0.31 ± 0.05 to 5.8 ± 0.3 mg kg"-"1; Ra-226 varied from 3.7 ± 0.3 to 43.3 ± 1.5 Bq kg"-"1; Pb-210 varied from 5.8 ± 2.6 to 118 ± 12 Bq kg"-"1; Th-232 varied from 0.67 ± 0.02 to 16.6 ± 0.4 mg kg"-"1 and Ra-228 varied from 3.5 ± 0.6 to 64.9 ± 2.4 Bq kg"-"1. These results were compared with literature values for the region, indicating that they are the background of the region and no contamination was observed from NORM (Naturally Occurring Radioactive Material) industries. (author)

  2. Determination of natural radionuclides, U, Th-232, Ra-226, Ra-228, Pb-210 and K-40 in sediments from CananÉIa-Iguape System, Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Jesus, Gleyka J.D.; Chiozzini, Vitor G.; Saueia, Cátia H.R.; Nisti, Marcelo B.; Braga, Elisabete S.; Fávaro, Deborah I.T., E-mail: gjdjesus@ipen.br, E-mail: chsaueia@ipen.br, E-mail: mbnisti@ipen.br, E-mail: defavaro@ipen.br, E-mail: vitor.chio@usp.br, E-mail: edsbraga@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Universidade de São Paulo (USP), SP (Brazil). Instituto Oceanográfico

    2017-07-01

    The Cananéia-Iguape estuarine-lagoon complex, located in the south of São Paulo State, Brazil, is a protected area recognized by UNESCO as part of the Biosphere Reserve, due to its importance as a natural ecosystem. However, along the years, the mining activities in the region affected the river basin, to such an extent that contamination was observed for As, Cu, Pb and Zn. Since the mining activities can also enhance the levels of natural radioactivity in the sediments, this study aimed to determine the activity concentration of the natural radionuclides (K-40, U, Ra-226, Pb-210, Th-232 and Ra-228) in 34 bottom sediments samples collected in the Cananéia-Iguape system. The samples were measured by gamma spectrometry, using a HPGe for the determination of K-40, Ra-226, Pb-210 and Ra-228. The concentration of U and Th-232 was determined by instrumental neutron activation analysis. The activity concentration of K-40 varied from 119 ± 17 to 522 ± 74 Bq kg{sup -1}; U-238 varied from 0.31 ± 0.05 to 5.8 ± 0.3 mg kg{sup -1}; Ra-226 varied from 3.7 ± 0.3 to 43.3 ± 1.5 Bq kg{sup -1}; Pb-210 varied from 5.8 ± 2.6 to 118 ± 12 Bq kg{sup -1}; Th-232 varied from 0.67 ± 0.02 to 16.6 ± 0.4 mg kg{sup -1} and Ra-228 varied from 3.5 ± 0.6 to 64.9 ± 2.4 Bq kg{sup -1}. These results were compared with literature values for the region, indicating that they are the background of the region and no contamination was observed from NORM (Naturally Occurring Radioactive Material) industries. (author)

  3. In situ detrital zircon (U-Th)/He thermochronology

    Science.gov (United States)

    Tripathy, A.; Monteleone, B. D.; van Soest, M. C.; Hodges, K.; Hourigan, J. K.

    2010-12-01

    situ method, utilizing SIMS to determine the U-Th concentrations. The major mode is the same as the conventional dataset, with only single outliers missing from the in situ dataset. The in situ method is described as follows: Zircons are polished and imaged using cathodoluminesence to guide laser spot placement. Then, each grain is ablated with a 193nm ArF Excimer laser using 20-35µm beam sizes and depths of 10-17µm. After purification, 4He is analyzed on a ThermoScientific Helix Split Flight Tube mass spectrometer. U-Th concentrations are measured on the polished mount using a Cameca IMS 6f by placing a 60µm diameter beam directly over the He laser pit to cover the surface area contributing to the measured He. In theory, using LA-ICP-MS to obtain U-Th concentrations could be a faster, cheaper, but possibly less precise, technique. However, using laser ablation would allow pit sizes that average the U-Th concentration over the volume of material available that contributes to the measured He, thus accounting for intracrystalline α-recoil effects. Preliminary data on slabs of Sri Lankan zircon suggest this could be a viable method, but will require further exploration and refinement.

  4. 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

  5. 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

  6. 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

  7. Zircon U-Pb chronology, geochemistry and Sr-Nd-Pb isotopic compositions of the Volcanic Rocks in the Elashan area, NW China: petrogenesis and tectonic implications

    Science.gov (United States)

    Zhou, H.; Wei, J.; Shi, W.; Li, P.; Chen, M.; Zhao, X.

    2017-12-01

    Elashan area is located in the intersection of the East Kunlun Orogenic Belt (EKOB) and the West Qinling Orogenic (WQOB). We present petrology, zircon U-Pb ages, whole-rock geochemistry and Sr-Nd-Pb isotopic compositions from the andesite and felsic volcanic rocks (rhyolite and rhyolitic tuffs) in Elashan group volcanic rock. The LA-ICP-MS zircon U-Pb age data indicate that the volcanic rocks are emplaced at 250 247 Ma. The volcanic rocks have high -K and aluminum - peraluminous characteristics, A/CNK = 1.07 1.82, δ ranges from 1.56 2.95, the main body is calc-alkaline rock. They are enriched in large ion lithophile elements (LILEs) and light rare earth elements (LREEs) and depleted in some high field strength elements (HFSEs, e.g., Nb, Ta, P and Ti), while having a flat heavy REE (HREEs) pattern. The ∑REE values of 178.68 to 298.11 ppm, average 230.50 ppm. The LREE/HREE values of 4.39 to 11.78 ppm, average 6.77 ppm. REE fractionation is obvious, REE distribution curve was right smooth, and have slightly negative Eu anomalies (Eu/Eu*=0.44-0.80, average 0.60), which as similar to the island arc volcanic rocks. The volcanic rocks have initial 87Sr/86Sr ratios of 0.71028-0.71232, ɛNd(t) values of -6.7 to -7.6, with T2DM-Nd ranging from 1561 to 1640 Ma. Pb isotopic composition (206 Pb / 204 Pb)t = 18.055 18.330, (207 Pb / 204 Pb)t = 15.586 15.618, (208 Pb / 204 Pb)t = 37.677 38.332. Geochemical and Sr-Nd-Pb isotopes indicates that Elashan group volcanic magma derived mainly from the lower crust. Elashan group volcanic rocks is the productive East Kunlun block and West Qinling block collision, which makes the thicken crust caused partial melting in the study area. The source rocks is probably from metamorphic sandstone of Bayankala. But with Y-Nb and Rb-(Y+Nb), R1-R2 and Rb/10-Hf-Ta*3 diagrams showing that intermediate-acid rocks mainly formed in volcanic arc-collision environment, probably the collision event is short , therefore rocks retain the original island

  8. Multielemental analysis of 18 essential and toxic elements in amniotic fluid samples by ICP-MS: Full procedure validation and estimation of measurement uncertainty.

    Science.gov (United States)

    Markiewicz, B; Sajnóg, A; Lorenc, W; Hanć, A; Komorowicz, I; Suliburska, J; Kocyłowski, R; Barałkiewicz, D

    2017-11-01

    Amniotic fluid is the substantial factor in the development of an embryo and fetus due to the fact that water and solutes contained in it penetrate the fetal membranes in an hydrostatic and osmotic way as well as being swallowed by the fetus. Elemental composition of amniotic fluid influences the growth and health of the fetus, therefore, an analysis of amniotic fluid is important because the results would indicate abnormal levels of minerals or toxic elements. Inductively coupled plasma mass spectroscopy (ICP-MS) is often used for determination of trace and ultra-trace level elements in a wide range of matrices including biological samples because of its unique analytical capabilities. In the case of trace and ultra-trace level analysis detailed characteristics of analytical procedure as well as properties of the analytical result are particularly important. The purpose of this study was to develop a new analytical procedure for multielemental analysis of 18 elements (Al, As, Ba, Ca, Cd, Co, Cr, Cu, Mg, Mn, Ni, Pb, Sb, Se, Sr, U, V and Zn) in amniotic fluid samples using ICP-MS. Dynamic reaction cell (DRC) with two reaction gases, ammonia and oxygen, was involved in the experiment to eliminate spectral interferences. Detailed validation was conducted using 3 certified reference mterials (CRMs) and real amniotic fluid samples collected from patients. Repeatability for all analyzed analytes was found to range from 0.70% to 8.0% and for intermediate precision results varied from 1.3% to 15%. Trueness expressed as recovery ranged from 80% to 125%. Traceability was assured through the analyses of CRMs. Uncertainty of the results was also evaluated using single-laboratory validation approach. The obtained expanded uncertainty (U) results for CRMs, expressed as a percentage of the concentration of an analyte, were found to be between 8.3% for V and 45% for Cd. Standard uncertainty of the precision was found to have a greater influence on the combined standard uncertainty

  9. 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

  10. Temporal evolution of natural radionuclides distributions 238U, 234Th, 226Ra, 228Ra, 210Pb and 210Po in the Bransfield strait, Antarctica peninsula

    International Nuclear Information System (INIS)

    Lapa, Flavia Valverde

    2013-01-01

    Research on the distribution of natural radionuclides in Antarctica is rare and thus, there is great interest in to know their occurrence and factors related to its mobilization, transference and accumulation in this extremely fragile environment. Natural radionuclides have been used intensively as tracers in the ocean, helping to better understand processes as sinking and particle resuspension, water masses mixture and oceanic circulation. 234 Th (t½ = 24.1 days) is a particle-reactive radionuclide produced continuously in seawater by the decay of its soluble precursor conservative with salinity 238 U (t½ = 4.5 10 9 years). Since 234 Th presents relatively short half-life, it is used to quantify processes that occur in temporal scale varying from days to weeks. The disequilibrium 234 Th/ 238 U in the surface ocean has been applied to estimate carbon fluxes exported via sinking material. The flux of particles biologically productive out of the euphotic zone in the Southern Ocean has special attention due to its importance in the control of CO 2 atmospheric concentrations. The radionuclides 210 Pb (t½ = 22.3 years) and 210 Po (t½ = 138 days) are also particle-reactive. The disequilibrium 210 Po/ 210 Pb has been used to estimate fluxes of particles exported in the ocean in the time scale of weeks. The long-lived Ra isotopes, 226 Ra (t½ = 1,600 years) and 228 Ra (t½ = 5.75 years) are soluble in seawater, presenting unique properties that make them excellent tracers of water masses. This research work had the aim to study the distributions of natural radionuclides 238 U, 234 Th, 22 '6Ra, 22 '8Ra, 210 Pb and 210 Po in the Bransfield Strait during 2 samplings carried out in the 2011 Austral Summer (OPERANTAR XXIX and XXX). (author)

  11. VALIDACIÓN DE LA METODOLOGÍA PARA LA DETERMINACIÓN DE SB, AS, CD, CU, CR, HG, NI, PB Y ZN EN SEDIMENTOS POR ICO-MS

    Directory of Open Access Journals (Sweden)

    Hermógenes Rosas Rodríguez

    2004-01-01

    Full Text Available En este trabajo se presentan los resultados obtenidos en la validación de la técnica ICP-MS utilizada para la determinación de nueve elementos en sedimentos: Sb, As, Cd, Cu, Cr, Hg, Ni, Pb y Zn. Para ello se llevó a cabo el estudio de los siguientes parámetros de fiabilidad: precisión, exactitud y límites de detección y cuantificación. Para el análisis de estos elementos se utilizó un ICP-MS ELAN 6000 de Perkin Elmer®. El estudio de los distintos parámetros de validación fue muy satisfactorio para la mayoría de los analitos, alcanzándose límites de detección y de cuantificación muy bajos (inferiores a 1microg/l e incluso de 1 ng/l para el Cd. El método ICP-MS es exacto y preciso, obteniéndose para la mayoría de los elementos coeficientes de variación en torno al 2% y porcentajes de recuperación del 100%.

  12. In situ isotopic analyses of U and Pb in zircon by remotely operated SHRIMP II, and Hf by LA-ICP-MS: an example of dating and genetic evolution of zircon by {sup 176}Hf/{sup 177}Hf from the Ita Quarry in the Atuba Complex, SE, Brazil; Analises in situ de U e Pb em zircao por SRIMP II por controle remoto e de Hf por LA-ICP-MS: um exemplo de datacao e da evolucao genetica de zircao atraves da razao {sup 176}Hf/{sup 177} em amostra da Pedreira Ita no Complexo Atuba, SE, Brasil

    Energy Technology Data Exchange (ETDEWEB)

    Sato, K.; Siga Junior, Oswaldo; McReath, Ian; Sproesser, Walter; Basei, Miguel Angelo Stipp [Universidade de Sao Paulo (USP), SP (Brazil). Inst. de Geociencias. Centro de Pesquisas Geocronologicas], e-mail: keisato@usp.br, e-mail: osigajr@usp.br, e-mail: ianmcr@usp.br, e-mail: wmspres@usp.br, e-mail: baseimas@usp.br; Silva, Josiane Aline da [Universidade de Sao Paulo (USP), SP (Brazil). Programa de Pos-graduacao em Geoquimica e Geotectonica; Dunyi, Liu [Institute of Geology, Beijing (China); Iizuka, Takafumi; Rino, Shuji; Hirata, Takafumi [Tokyo Institute of Technology, Tokyo (Japan)

    2009-10-15

    Remotely-operated SHRIMP dating of zircon is an interesting alternative for dating of zircon crystals. Although it does not represent any technical progress of the geochronological method using the U-Pb system in zircon it is a very useful and cheap facility. The procedure was first used for mass spectrometric analyses involving two international laboratories in Sao Paulo, Brazil and Beijing, China. It was applied to samples of three gneiss-migmatitic rocks from the Ita quarry in the Atuba Complex (located between the Luis Alves and the Apiai Domain) to test previous controversial hypotheses about its evolution. The presence of important archaean and paleo proterozoic components in the complex is confirmed by analyses of zircon found in probably neo proterozoic leucosomes. Diorite intrusion also occurred during the neo proterozoic, associated with the 0.6Ga continental collisions involved in the assembly of Gondwana. The determination of Hf isotope ratios by LA-ICP/MS represents a new option for checking the relative importance of mantle ({epsilon}{sub Hf} > 0) and crustal contributions (({epsilon}{sub Hf} < 0) during the growth of the zircon crystals. While the archaean component in the complex was derived from the mantle ({epsilon}{sub Hf} + 1.5 to + 8.7) the paleo proterozoic component had a crustal contribution ({epsilon}{sub Hf} - 9.1 to -10.1). (author)

  13. 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...

  14. Electron microprobe Th-U-Pb monazite dating and metamorphic evolution of the Acaiaca Granulite Complex, Minas Gerais, Brazil

    Energy Technology Data Exchange (ETDEWEB)

    Medeiros Junior, Edgar Batista; Marques, Rodson Abreu, E-mail: edgarjr@ymail.com, E-mail: rodson.marques@ufes.br [Universidade Federal do Espirito Santo (UFES), Alegre, ES (Brazil). Departamento de Geologia; Jordt-Evangelista, Hanna; Queiroga, Glaucia Nascimento, E-mail: hanna@degeo.ufop.br, E-mail: glauciaqueiroga@yahoo.com.br [Universidade Federal de Ouro Preto (UFOP), Ouro Preto, MG (Brazil). Escola de Minas. Departamento de Geologia; Schulz, Bernhard, E-mail: bernhard.schulz@mineral.tu-freiberg.de [TU Bergakademie - Institute of Mineralogy, Freiberg - Saxony (Germany)

    2016-01-15

    The Acaiaca Complex (AC) is located in southeastern Minas Gerais state, and comprises felsic, mafic, ultramafic, and aluminous granulite as well as lower grade gneisses and mylonite. The complex is distributed over an area of ca. 36 km by 6 km, surrounded by amphibolite facies gneisses of the Mantiqueira Complex (MC). The discrepancy in the metamorphic grade between both complexes led to the present study aiming to understand the metamorphic history of the AC by means of geothermobarometry calculations and electron microprobe Th-U-Pb monazite dating. Estimates of the metamorphic conditions of the granulite based on conventional geothermobarometry and THERMOCALC resulted in temperatures around 800 deg C and pressures between of 5.0 and 9.9 kbar and a retro metamorphic path characterized by near-isobaric cooling. Part of the granulite was affected by anatexis. The melting of felsic granulite resulted in the generation of pegmatites and two aluminous lithotypes. These are: 1) garnet-sillimanite granulite with euhedral plagioclase and cordierite that show straight faces against quartz, and is the crystallization product of an anatectic melt, and 2) garnet-kyanite-cordierite granulite, which is probably the restite of anatexis, as indicated by textures and high magnesium contents. Th-U-Pb monazite geochronology of two granulite samples resulted in a metamorphic age around 2060 Ma, which is similar to the age of the MC registered in the literature. The similar Paleoproterozoic metamorphic ages of both complexes lead to the conclusion that the Acaiaca Complex may be the high grade metamorphic unit geochronological related to the lower grade Mantiqueira Complex. (author)

  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. Timing of sediment-hosted Cu-Ag mineralization in the Trans-Hudson orogen at Janice Lake, Wollaston Domain, Saskatchewan, Canada

    Science.gov (United States)

    Perelló, José; Valencia, Víctor A.; Cornejo, Paula; Clifford, John; Wilson, Alan J.; Collins, Greg

    2018-04-01

    The Janice Lake Cu-Ag mineralization in the Wollaston Domain of northern Saskatchewan is hosted by a metasedimentary sequence in the upper part of the Wollaston Supergroup of the Trans-Hudson orogen. The Wollaston Supergroup was deposited between 2070 and 1865 Ma in a foreland basin setting constructed over Archean basement of the Hearne craton. The Trans-Hudson orogen underwent final collision and peak metamorphism at 1810 Ma, during consolidation of Laurentia and its amalgamation with the Columbia supercontinent. Titanite is a common constituent of the post-peak metamorphic assemblages of Trans-Hudson lithotectonic units and accompanied disseminated sediment-hosted Cu sulfide mineralization at Janice Lake. Titanite crystals, intergrown with chalcocite over a strike-length of 2 km of Cu-bearing stratigraphy, were dated by the ID-TIMS and LA-ICP-MS U-Pb methods, returning an age range from 1780 to 1760 Ma and a weighted average age of 1775 ± 10 Ma. The titanite ages effectively date the associated chalcocite-dominated sediment-hosted Cu-Ag mineralization and its formation during initial post-orogenic uplift and cooling, 30 myr after peak metamorphism. The age-range and tectonic setting of the Janice Lake mineralization confirms that sediment-hosted Cu mineralization was an integral part of the metallogenic endowment of Columbia and that its emplacement coincided with the continental-scale Trans-Hudson orogeny rather than with diagenesis and extensional basin development 100 myr earlier.

  17. Ultratrace determination of Pb, Se and As in wine samples by electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Grindlay, Guillermo, E-mail: guillermo.grindlay@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, PO Box 99, 03080 - Alicante (Spain); Mora, Juan; Gras, Luis [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, PO Box 99, 03080 - Alicante (Spain); de Loos-Vollebregt, M.T.C. [Delft University of Technology, Fac. Applied Sciences, Julianalaan 67, 2628 BC - Delft (Netherlands)

    2009-10-12

    The determination of Pb, Se and As in wine has a great interest due to health risks and legal requirements. To perform the analysis of wine, two considerations must be taken into account: (i) the low concentration level of the analytes; and (ii) the risk of interferences due to wine matrix components. The goal of this work is to evaluate electrothermal vaporization (ETV) sample introduction for ultratrace determination of Pb, Se and As in wine samples by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained with ETV-ICP-MS were compared to those obtained with conventional liquid sample introduction in ICP-MS and electrothermal atomic absorption spectrometry (ETAAS). Analytical figures of merit of ETV sample introduction strongly depend on the amount of wine sample, on the modifier nature (i.e. Pd, ascorbic acid or citric acid) and concentration and on the temperature program. Wine matrix components exert a great influence on analyte transport efficiency. Due to this fact, the analysis of wine cannot be performed by means of external calibration but the standard addition methodology should be used. The determination of Pb and Se in wine by ETV-ICP-MS provides similar results as conventional liquid sample introduction ICP-MS. For As, the concentration values obtained with ETV sample introduction were between two and four times lower than with the conventional system. These differences are related to the lower intensity of polyatomic interferences (i.e. {sup 40}Ar{sup 35}Cl{sup +} vs. {sup 75}As{sup +}) obtained for ETV sample introduction when compared to the conventional system. Finally, no differences for Pb determination were observed between ETV sample introduction and ETAAS. Unfortunately, the limits of detection for As and Se in ETAAS were not low enough to quantify these elements in the wine samples tested.

  18. Ultratrace determination of Pb, Se and As in wine samples by electrothermal vaporization inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Grindlay, Guillermo; Mora, Juan; Gras, Luis; de Loos-Vollebregt, M.T.C.

    2009-01-01

    The determination of Pb, Se and As in wine has a great interest due to health risks and legal requirements. To perform the analysis of wine, two considerations must be taken into account: (i) the low concentration level of the analytes; and (ii) the risk of interferences due to wine matrix components. The goal of this work is to evaluate electrothermal vaporization (ETV) sample introduction for ultratrace determination of Pb, Se and As in wine samples by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained with ETV-ICP-MS were compared to those obtained with conventional liquid sample introduction in ICP-MS and electrothermal atomic absorption spectrometry (ETAAS). Analytical figures of merit of ETV sample introduction strongly depend on the amount of wine sample, on the modifier nature (i.e. Pd, ascorbic acid or citric acid) and concentration and on the temperature program. Wine matrix components exert a great influence on analyte transport efficiency. Due to this fact, the analysis of wine cannot be performed by means of external calibration but the standard addition methodology should be used. The determination of Pb and Se in wine by ETV-ICP-MS provides similar results as conventional liquid sample introduction ICP-MS. For As, the concentration values obtained with ETV sample introduction were between two and four times lower than with the conventional system. These differences are related to the lower intensity of polyatomic interferences (i.e. 40 Ar 35 Cl + vs. 75 As + ) obtained for ETV sample introduction when compared to the conventional system. Finally, no differences for Pb determination were observed between ETV sample introduction and ETAAS. Unfortunately, the limits of detection for As and Se in ETAAS were not low enough to quantify these elements in the wine samples tested.

  19. Daily ingestion of 232Th, 238U, 226Ra, 228Ra and 210Pb in vegetables by inhabitants of Rio de Janeiro City

    International Nuclear Information System (INIS)

    Santos, E.E.; Lauria, D.C.; Amaral, E.C.S.; Rochedo, E.R.

    2002-01-01

    The concentrations of the naturally occurring radionuclides 232 Th, 238 U, 210 Pb, 226 Ra and 228 Ra were determined in the vegetables (leafy vegetables, fruit, root, bean and rice) and derived products (sugar, coffee, manioc flour, wheat flour, corn flour and pasta) consumed most by the adult inhabitants of Rio de Janeiro City. A total of 88 samples from 26 different vegetables and derived products were analyzed. The highest contribution to radionuclide intake arises from bean, wheat flour, manioc flour, carrot, rice, tomato and potato consumption. The estimated daily intakes due to the consumption of vegetables and derived products are 1.9 mBq of 232 Th (0.47 μg), 2.0 mBq of 238 U (0.17 μg), 19 mBq of 226 Ra, 26 mBq of 210 Pb and 47 mBq of 228 Ra. The estimated annual effective dose due to the ingestion of vegetables and their derived products with the long-lived natural radionuclides is 14.5 μSv. Taking into account literature data for water and milk from Rio de Janeiro the dose value increases to 29 μSv, with vegetables and derived products responsible for 50% of the dose and water for 48%. 210 Pb (62%) and 228 Ra (24%) were found to be the main sources for internal irradiation

  20. Evaluation de la contamination de la chaîne trophique par les éléments traces (Cu, Co, Zn, Pb, Cd, U, V et As dans le bassin de la Lufira supérieure (Katanga/RD Congo

    Directory of Open Access Journals (Sweden)

    Katemo Manda, B.

    2010-01-01

    Full Text Available Evaluation of Contamination of the Food Chain by Trace Elements (Cu, Co, Zn, Pb, Cd, U, V and As in the Basin of the Upper Lufira (Katanga/DR Congo. Seven trace elements (Cu, Co, Zn, Cd, Pb, U, V and As were analyzed using a HR ICP-MS in samples of water, plankton, leaves of Phragmites australis, muscle and gills of three fish species (Oreochromis macrochir, Tilapia rendalli, Clarias gariepinus collected in the basin of the upper Lufira. The results indicate a high copper (70.9 ppm and cobalt (32.3 ppm content in the effluent of complex hydrometallurgical Shituru. If contamination of rivers decreases with distance from the pollution source, the values are very high in lake Tshangalele for plankton and leaves of P. australis. For fish, the results indicate that Pb, U, V, Cu, Co and Cd accumulates preferentially in the gills but Zn accumulates more in the muscles. As accumulates in the same order of magnitude in both organs. These results confirm the pollution of the basin by the effluents from Lufira complex hydrometallurgical Shituru.

  1. 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.

  2. 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...

  3. 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)

  4. Th, U, REE Backgrounds and Phytoavailability in Soils of the Padanian Plain (Northern Italy

    Directory of Open Access Journals (Sweden)

    Dario Di Giuseppe

    2014-12-01

    Full Text Available In this contribution we present ICP-MS analyses carried out on agricultural soils from the eastern-most part of the Padanian plain (Ferrara Province and on the related crop products. The aim is to provide, for the first time, backgrounds for some trace elements such as rare earth elements (REE, thorium (Th, uranium (U and to understand the related phytoavailability. In particular, detailed analyses have been done on Sorghum Vulgare plants, analyzing distinct plant parts in different vegetative periods. Results indicate that a REE concentration in plant tissues is always lower than in the related soils, precluding the occurrence of bioaccumulation and b no preferential elemental uptake and REE fractionation. In this light, the observed soil/plant relationships could be used in the definition of markers of territoriality (provenance fingerprint for agricultural products.

  5. 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...

  6. Determination of {sup 90}Sr in soil samples using inductively coupled plasma mass spectrometry equipped with dynamic reaction cell (ICP-DRC-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Feuerstein, J.; Boulyga, S.F.; Galler, P.; Stingeder, G. [Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, University of Natural Resources and Applied Life Sciences, Muthgasse 18, A-1190 Vienna (Austria); Prohaska, T. [Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, University of Natural Resources and Applied Life Sciences, Muthgasse 18, A-1190 Vienna (Austria)], E-mail: thomas.prohaska@boku.ac.at

    2008-11-15

    A rapid method is reported for the determination of {sup 90}Sr in contaminated soil samples in the vicinity of the Chernobyl Nuclear Power Plant by ICP-DRC-MS. Sample preparation and measurement procedures focus on overcoming the isobaric interference of {sup 90}Zr, which is present in soils at concentrations higher by more than six orders of magnitude than {sup 90}Sr. Zirconium was separated from strontium in two steps to reduce the interference by {sup 90}Zr{sup +} ions by a factor of more than 10{sup 7}: (i) by ion exchange using a Sr-specific resin and (ii) by reaction with oxygen as reaction gas in a dynamic reaction cell (DRC) of a quadrupole ICP-MS. The relative abundance sensitivity of the ICP-MS was studied systematically and the peak tailing originating from {sup 88}Sr on mass 90 u was found to be about 3 x 10{sup -9}. Detection limits of 4 fg g{sup -1} (0.02 Bq g{sup -1}) were achieved when measuring Sr solutions containing no Zr. In digested uncontaminated soil samples after matrix separation as well as in a solution of 5 {mu}g g{sup -1} Sr and 50 ng g{sup -1} Zr a detection limit of 0.2 pg g{sup -1} soil (1 Bq g{sup -1} soil) was determined. {sup 90}Sr concentrations in three soil samples collected in the vicinity of the Chernobyl Nuclear Power Plant were 4.66 {+-} 0.27, 13.48 {+-} 0.68 and 12.9 {+-} 1.5 pg g{sup -1} corresponding to specific activities of 23.7 {+-} 1.3, 68.6 {+-} 3.5 and 65.6 {+-} 7.8 Bq g{sup -1}, respectively. The ICP-DRC-MS results were compared to the activities measured earlier by radiometry. Although the ICP-DRC-MS is inferior to commonly used radiometric methods with respect to the achievable minimum detectable activity it represents a time- and cost-effective alternative technique for fast monitoring of high-level {sup 90}Sr contamination in environmental or nuclear industrial samples down to activities of about 1 Bq g{sup -1}.

  7. Determining the isotopic compositions of uranium and fission products in radioactive environmental microsamples using laser ablation ICP-MS with multiple ion counters

    Energy Technology Data Exchange (ETDEWEB)

    Boulyga, Sergei F.; Prohaska, Thomas [University of Natural Resources and Applied Life Sciences, Department of Chemistry, Division of Analytical Chemistry-VIRIS Laboratory, Vienna (Austria)

    2008-01-15

    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 {sup 235}U/{sup 238}U, {sup 236}U/{sup 238}U, {sup 145}Nd/{sup 143}Nd, {sup 146}Nd/{sup 143}Nd, {sup 101}Ru/({sup 99}Ru+{sup 99}Tc) and {sup 102}Ru/({sup 99}Ru+{sup 99}Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred {mu}m 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 {sup 101}Ru/({sup 99}Ru+{sup 99}Tc) and {sup 102}Ru/({sup 99}Ru+{sup 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 {sup 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 {sup 235}U/{sup 238}U and {sup 236}U/{sup 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

  8. 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)

  9. Geochemical Characteristics of Trace Elements in the No. 6 Coal Seam from the Chuancaogedan Mine, Jungar Coalfield, Inner Mongolia, China

    Directory of Open Access Journals (Sweden)

    Lin Xiao

    2016-03-01

    Full Text Available Fourteen samples of No. 6 coal seam were obtained from the Chuancaogedan Mine, Jungar Coalfield, Inner Mongolia, China. The samples were analyzed by optical microscopic observation, X-ray diffraction (XRD, scanning electron microscope equipped with an energy-dispersive X-ray spectrometer (SEM-EDS, inductively coupled plasma mass spectrometry (ICP-MS and X-ray fluorescence spectrometry (XRF methods. The minerals mainly consist of kaolinite, pyrite, quartz, and calcite. The results of XRF and ICP-MS analyses indicate that the No. 6 coals from Chuancaogedan Mine are higher in Al2O3, P2O5, Zn, Sr, Li, Ga, Zr, Gd, Hf, Pb, Th, and U contents, but have a lower SiO2/Al2O3 ratio, compared to common Chinese coals. The contents of Zn, Sr, Li, Ga, Zr, Gd, Hf, Pb, Th, and U are higher than those of world hard coals. The results of cluster analyses show that the most probable carrier of strontium in the coal is gorceixite; Lithium mainly occurs in clay minerals; gallium mainly occurs in inorganic association, including the clay minerals and diaspore; cadmium mainly occurs in sphalerite; and lead in the No. 6 coal may be associated with pyrite. Potentially valuable elements (e.g., Al, Li, and Ga might be recovered as byproducts from coal ash. Other harmful elements (e.g., P, Pb, and U may cause environmental impact during coal processing.

  10. 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

  11. Total lead (Pb) concentration in oil shale ash samples based on correlation to isotope Pb-210 gamma-spectrometric measurements

    Energy Technology Data Exchange (ETDEWEB)

    Vaasma, T.; Kiisk, M.; Tkaczyk, A.H. [University of Tartu (Estonia); Bitjukova, L. [Tallinn University of Technology (Estonia)

    2014-07-01

    Estonian oil shale consists of organic matter and mineral material and contains various amounts of heavy metals as well as natural radionuclides (from the U-238 and Th-232 series and K-40). Previous research has shown that burning oil shale in the large power plants causes these radionuclides to become enriched in different ash fractions and be partially emitted to the atmosphere via fly ash and flue gases. The activity concentrations (Bq/kg) of these nuclides in different oil shale ash fractions vary significantly. This is influenced by the boiler parameters and combustion conditions - prevailing temperatures, pressure, ash circulating mechanisms, fly ash particle size, chemical composition of ash and coexistence of macro and micro components. As with radionuclides, various heavy metals remain concentrated in the ash fractions and are released to the atmosphere (over 20 tons of Pb per year from Estonian oil shale power plants). Lead is a heavy metal with toxic influence on the nervous system, reproductive system and different organs in human body. Depending on the exposure pathways, lead could pose a long term health hazard. Ash samples are highly heterogeneous and exhibit great variability in composition and particle size. Determining the lead concentration in ash samples by modern methods like inductively coupled plasma mass spectroscopy (ICP-MS), flame atomic absorption spectrometry (FAAS), graphite furnace atomic absorption spectroscopy (GFAAS) and other techniques often requires time consuming, multistage and complex chemical sample preparation. The list of possible methods to use is lengthy, but it is a challenge to choose a suitable one to meet measurement needs and practical considerations. The detection limits, capital costs and maintenance expenses vary between the instruments. This work presents the development of an alternative measurement technique for our oil shale ash samples. Oil shale ash was collected from different boilers using pulverized fuel

  12. 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.

  13. 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.)

  14. Conventional U-Pb dating versus SHRIMP of the Santa Barbara Granite Massif, Rondonia, Brazil

    Science.gov (United States)

    Sparrenberger, I.; Bettencourt, Jorge S.; Tosdal, R.M.; Wooden, J.L.

    2002-01-01

    The Santa Ba??rbara Granite Massif is part of the Younger Granites of Rondo??nia (998 - 974 Ma) and is included in the Rondo??nia Tin Province (SW Amazonian Craton). It comprises three highly fractionated metaluminous to peraluminous within-plate A-type granite units emplaced in older medium-grade metamorphic rocks. Sn-mineralization is closely associated with the late-stage unit. U-Pb monazite conventional dating of the early-stage Serra do Cicero facies and late-stage Serra Azul facies yielded ages of 993 ?? 5 Ma and 989 ?? 13 Ma, respectively. Conventional multigrain U-Pb isotope analyses of zircon demonstrate isotopic disturbance (discordance) and the preservation of inherited older zircons of several different ages and thus yield little about the ages of Sn-granite magmatism. SHRIMP U-Pb ages for the Santa Ba??rbara facies association yielded a 207Pb/206Pb weighted-mean age of 978 ?? 13 Ma. The textural complexity of the zircon crystals of the Santa Ba??rbara facies association, the variable concentrations of U, Th and Pb, as well as the mixed inheritance of zircon populations are major obstacles to using conventional multigrain U-Pb isotopic analyses. Sm-Nd model ages and ??Nd (T) values reveal anomalous isotopic data, attesting to the complex isotopic behaviour within these highly fractionated granites. Thus, SHRIMP U-Pb zircon and conventional U-Pb monazite dating methods are the most appropriate to constrain the crystallization age of the Sn-bearing granite systems in the Rondo??nia Tin Province.

  15. 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...

  16. 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 the H₂O₂ test and the chromatography behavior, it can be inferred that, the uAs might not be toxic organic As. Estimated daily intake ( EDI) , hazard quotient ( HQ ), and cancer risk ( CR ) caused by the total As content; the sum of inorganic As (iAs) and uAs, namely i+uAs; and iAs exposure from long term O. sinensis consumption were calculated and evaluated through equations from the US Environmental Protection Agency and the uncertainties were analyzed by Monte-Carlo Simulation (MCS). EDI total As and EDI i+uAs are approximately ten times more than EDI iAs ; HQ total As and HQ i+u As > 1 while HQ i As 1 × 10 −4 while CR iAs iAs is very low.

  17. 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

  18. Determination of Arsenic Species in Ophiocordyceps sinensis from Major Habitats in China by HPLC-ICP-MS and the Edible Hazard Assessment

    Directory of Open Access Journals (Sweden)

    Lian-Xian Guo

    2018-04-01

    Full Text Available 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, MMAV, DMAV, AsV, and AsШ—were either not detected (MMAV and DMAV or were detected as minor As species (AsB: 1.4–2.9%; AsV: 1.3–3.2%, and AsШ: 4.1–6.0%. The major components were a cluster of unknown organic As (uAs compounds with AsШ, which accounted for 91.7–94.0% of the As content. Based on the H2O2 test and the chromatography behavior, it can be inferred that, the uAs might not be toxic organic As. Estimated daily intake (EDI, hazard quotient (HQ, and cancer risk (CR caused by the total As content; the sum of inorganic As (iAs and uAs, namely i+uAs; and iAs exposure from long term O. sinensis consumption were calculated and evaluated through equations from the US Environmental Protection Agency and the uncertainties were analyzed by Monte-Carlo Simulation (MCS. EDItotal As and EDIi+uAs are approximately ten times more than EDIiAs; HQtotal As and HQi+uAs > 1 while HQiAs < 1; and CRtotal As and CRi+uAs > 1 × 10−4 while CRiAs < 1 × 10−4. Thus, if the uAs is non-toxic, there is no particular risk to local consumers and the carcinogenic risk is acceptable for consumption of O. sinensis because the concentration of toxic iAs is very low.

  19. 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)

  20. 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)

  1. 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.

  2. Levels in 223Th populated by α decay of 227U

    Science.gov (United States)

    Kalaninová, Z.; Antalic, S.; Heßberger, F. P.; Ackermann, D.; Andel, B.; Kindler, B.; Laatiaoui, M.; Lommel, B.; Maurer, J.

    2015-07-01

    Levels in 223Th populated by the α decay of 227U were investigated using α -γ decay spectroscopy. The 227U isotope was produced in the fusion-evaporation reaction 22Ne +208Pb at the velocity filter separator for heavy-ion reaction products at Gesellschaft für Schwerionenforschung in Darmstadt (Germany). Several new excited levels and γ transitions were identified in 223Th . An improved α -decay scheme of 227U was suggested. The experimental α -decay energy spectrum of 227U was compared with the Monte Carlo simulation performed using the toolkit geant4.

  3. Elemental fractionation in 785 nm picosecond and femtosecond laser ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shaheen, M.E., E-mail: mshaheen73@science.tanta.edu.eg [Department of Physics, Faculty of Sciences, Tanta University, Tanta (Egypt); Gagnon, J.E.; Fryer, B.J. [Great Lakes Institute for Environmental Research (GLIER), University of Windsor, Windsor, Ontario N9B 3P4 (Canada); Department of Earth and Environmental Sciences, University of Windsor, Windsor, Ontario N9B 3P4 (Canada)

    2015-05-01

    Elemental fractionation and ICP-MS signal response were investigated for two different pulse width laser beams originating from the same laser system. Femtosecond and picosecond laser beams at pulse widths of 130 fs and 110 ps, respectively, and wavelength of 785 nm were used to ablate NIST 610 synthetic glass and SRM 1107 Naval Brass B at the same spot for 800 to 1000 laser pulses at different repetition rates (5 to 50 Hz). Elemental fractionation was found to depend on repetition rate and showed a trend with femtosecond laser ablation that is opposite to that observed in picosecond laser ablation for most measured isotopes. ICP-MS signal intensity was higher in femtosecond than picosecond LA-ICP-MS in both NIST 610 and naval brass when ablation was conducted under the same fluence and repetition rate. The differences in signal intensity were partly related to differences in particle size distribution between particles generated by femtosecond and picosecond laser pulses and the consequent differences in transport and ionization efficiencies. The main reason for the higher signal intensity resulting from femtosecond laser pulses was related to the larger crater sizes compared to those created during picosecond laser ablation. Elemental ratios measured using {sup 66}Zn/{sup 63}Cu, {sup 208}Pb/{sup 238}U, {sup 232}Th/{sup 238}U, {sup 66}Zn/{sup 232}Th and {sup 66}Zn/{sup 208}Pb were found to change with the number of laser pulses with data points being more scattered in picosecond than femtosecond laser pulses. Reproducibility of replicate measurements of signal intensities, fractionation and elemental ratios was better for fs-LA-ICP-MS (RSD ~ 3 to 6%) than ps-LA-ICP-MS (RSD ~ 7 to 11%). - Highlights: • Fractionation and ICP-MS signal response were investigated for two different pulse widths using NIST 610 and Naval Brass. • Dependence of fractionation indices on repetition rate and pulse width. • Higher ablation rate was observed in picosecond compared to

  4. 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)

  5. Are Polyatomic Interferences, Cross Contamination, Mixing-Effect, etc., Obstacles for the Use of Laser Ablation-ICP-MS Coupling as an Operational Technique for Uranium Isotope Ratio Particle Analysis?

    International Nuclear Information System (INIS)

    Donard, A.; Pointurier, F.; Pecheyran, C.

    2015-01-01

    Analysis of ''environmental samples'', which consists in dust collected with cotton clothes wiped by inspectors on surfaces inside declared nuclear facilities, is a key tool for safeguards. Although two methods (fission tracks-TIMS and SIMS) are already used routinely to determine the isotopic composition of uranium particles, the laser ablationinductively coupled plasma mass spectrometry (LA-ICP-MS) coupling has been proven to be an interesting option thanks to its rapidity, high sensitivity and high signal/noise ratio. At CEA and UPPA, feasibility of particle analysis using a nanosecond LA device and a quadrupole ICP-MS has been demonstrated. However, despite the obvious potential of LA-ICP-MS for particle analysis, the effect of many phenomena which may bias isotope ratio measurements or lead to false detections must be investigated. Actually, environmental samples contain many types of non-uranium particles (organic debris, iron oxides, etc.) that can form molecular interferences and induce the risk of isotopic measurement bias, especially for minor isotopes (234U, 236U). The influence of these polyatomic interferences on the measurements will be discussed. Moreover, different uranium isotopic compositions can be found in the same sample. Therefore, risks of memory effect and of particle-toparticle cross-contamination by the deposition of ablation debris around the crater have also been investigated. This study has been conducted by using a femtosecond laser ablation device coupled to a high sensitivity sector field ICP-MS. Particles were fixed onto the discs with collodion and were located thanks to their fission tracks so that micrometric particles can be analyzed separately. All uranium isotope ratios were measured. Results are compared with the ones obtained with the fission tracks-TIMS technique on other deposition discs from the same sample. Performance of the method in terms of accuracy, precision, and detection limits are estimated

  6. [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.

  7. 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.

  8. 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

  9. 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)

  10. 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

    aspirated into the ICP-MS directly. The decontamination factor for 238 U is more than 10 4 . The feasibility for the determination of both elements was proved by analysisng IAEA-135 reference samples, the measured values agreed with the recommended reference value. (author)

  11. Did the Kiruna iron ores form as a result of a metasomatic or igneous process? New U-Pb and Nd data for the iron oxide apatite ores and their host rocks in the Norrbotten region of northern Sweden

    Science.gov (United States)

    Westhues, A.; Hanchar, J. M.; Whitehouse, M. J.; Fisher, C. M.

    2012-12-01

    dating of zircon from both host rock and ore samples confirms a previously documented event around 1880 - 1900 Ma in the Norrbotten region. However, U-Pb in monazite from an ore sample suggests a further event at ca. 1650 Ma, a period of known activity in Fennoscandia. Further investigation and more U-Pb data are needed to confirm those dates and how the iron mineralization is related to those two events. The combination of U-Th-Pb ages, tracer isotopes and trace element abundances at mineral scale (e.g., Lu-Hf in zircon, and Sm-Nd in monazite, apatite, titanite), along with the O isotopic composition of zircon, will be used to decipher whether the Kiruna iron ore deposits are of metasomatic or igneous origin. Overall, the study also intends to develop a predictive model for exploration of similar iron oxide apatite deposits worldwide.

  12. 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.

  13. 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.

  14. 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.

  15. 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)

  16. U-Pb geochronology of zircons form lunar Breccia 73217 using a sensitive high mass-resolution ion microprobe

    International Nuclear Information System (INIS)

    Compston, W.; Williams, I.S.

    1984-01-01

    U-Pb age determinations on four lunar zircons from existing thin-sections of one highland breccia, 73217, using the recently constructed ion microprobe SHRIMP, are reported. The analytical reproducibility of SHRIMP is demonstrated, and procedures for measuring Pb/U, Th/U, and corecting for initial Pb are explained. Electron microprobe analyses for the zircons are also reported. The results show that the four zircons survived the lunar cataclysm without any identifiable effects on their U-Pb systematics. All four indicate a single age of 4356 +23 or -14 m.y. The zircons have experienced small variable amounts of Pb loss since crystallization, from almost zero up to about 10 percent. If this occurred during one later event, then age of the latter is between 1100 and 2300 m.y. 18 references

  17. The Effect of fO2 on Partition Coefficients of U and Th between Garnet and Silicate Melt

    Science.gov (United States)

    Huang, F.; He, Z.; Schmidt, M. W.; Li, Q.

    2014-12-01

    Garnet is one of the most important minerals controlling partitioning of U and Th in the upper mantle. U is redox sensitive, while Th is tetra-valent at redox conditions of the silicate Earth. U-series disequilibria have provided a unique tool to constrain the time-scales and processes of magmatism at convergent margins. Variation of garnet/meltDU/Th with fO2 is critical to understand U-series disequilibria in arc lavas. However, there is still no systematic experimental study about the effect of fO2 on partitioning of U and Th between garnet and melt. Here we present experiments on partitioning of U, Th, Zr, Hf, Nb, Ta, and REE between garnet and silicate melts at various fO2. The starting material was hydrous haplo-basalt. The piston cylinder experiments were performed with Pt double capsules with C-CO, MnO-Mn3O4 (MM), and hematite-magnetite (HM) buffers at 3 GPa and 1185-1230 oC. The experiments produced garnets with diameters > 50μm and quenched melt. Major elements were measured by EMPA at ETH Zurich. Trace elements were determined using LA-ICP-MS at Northwestern University (Xi'an, China) and SIMS (Cameca1280 at the Institute of Geology and Geophysics, Beijing, China), producing consistent partition coefficient data for U and Th. With fO2 increasing from CCO to MM and HM, garnet/meltDU decreases from 0.041 to 0.005, while garnet/meltDTh ranges from 0.003 to 0.007 without correlation with fO2. Notably, garnet/meltDTh/U increases from 0.136 at CCO to 0.41 at HM. Our results indicate that U is still more compatible than Th in garnet even at the highest fO2 considered for the subarc mantle wedge (~NNO). Therefore, we predict that if garnet is the dominant phase controlling U-Th partitioning during melting of the mantle wedge, melts would still have 230Th excess over 238U. This explains why most young continental arc lavas have 230Th excess. If clinopyroxene is the dominant residual phase during mantle melting, U could be more incompatible than Th at high fO2

  18. Laser ablation ICP-mass spectrometry determination of Th230 in soils at the Gunnison, Colorado UMTRA site

    International Nuclear Information System (INIS)

    Anderson, M.S.; Braymen, S.; McIntosh, R.

    1994-01-01

    This report describes an innovative technology, laser ablation-inductively couple plasma-mass spectrometry (LA-ICP-MS), operated in a mobile laboratory, to rapidly detect thorium 230 activity levels in soil samples. This technology was demonstrated on-site during November 1993 at the Gunnison, Colorado, UMTRA project site in support of their remediation effort. The LA-ICP-MS sampling and analysis technique was chosen because of the capability for rapid analysis, approximately three samples per hour, with minimal sample preparation

  19. 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

  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. Determination of Sediment Profile for 210Pb, Pb, U and Th from Sultan Abu Bakar Dam Due to Soil Erosion from Highland Agriculture Area, Cameron Highlands, Malaysia

    OpenAIRE

    Zaini Hamzah; Seh D. Riduan; Ahmad Saat

    2011-01-01

    Problem statement: Sultan Abu Bakar Dam in Cameron Highlands act as a catchments to accumulate all eroded soil carried by the run off flow through Bertam River, the main river that passes through the highland agriculture area. All suspended solid that carried out by the river contain various kind of hazard potential to the environment. U, Th and Pb are the potential hazard elements carried out by water and accumulate at the dam. Approach: Five sampling point were selected where five 30cm core...

  2. 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

  3. 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.

  4. 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).

  5. 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.)

  6. 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

  7. 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

  8. Determination of the total drug-related chlorine and bromine contents in human blood plasma using high performance liquid chromatography-tandem ICP-mass spectrometry (HPLC-ICP-MS/MS).

    Science.gov (United States)

    Klencsár, Balázs; Bolea-Fernandez, Eduardo; Flórez, María R; Balcaen, Lieve; Cuyckens, Filip; Lynen, Frederic; Vanhaecke, Frank

    2016-05-30

    A fast, accurate and precise method for the separation and determination of the total contents of drug-related Cl and Br in human blood plasma, based on high performance liquid chromatography - inductively coupled plasma - tandem mass spectrometry (HPLC-ICP-MS/MS), has been developed. The novel approach was proved to be a suitable alternative to the presently used standard methodology (i.e. based on a radiolabelled version of the drug molecule and radiodetection), while eliminating the disadvantages of the latter. Interference-free determination of (35)Cl has been accomplished via ICP-MS/MS using H2 as reaction gas and monitoring the (35)ClH2(+) reaction product at mass-to-charge ratio of 37. Br could be measured "on mass" at a mass-to-charge of 79. HPLC was relied on for the separation of the drug-related entities from the substantial amount of inorganic Cl. The method developed was found to be sufficiently precise (repeatability 0.990) from the limit of quantification (0.05 and 0.01 mg/L for Cl and Br in blood plasma, respectively) to at least 5 and 1mg/L for Cl and Br, respectively. Quantification via either external or internal standard calibration provides reliable results for both elements. As a proof-of-concept, human blood plasma samples from a clinical study involving a newly developed Cl- and Br-containing active pharmaceutical ingredient were analysed and the total drug exposure was successfully described. Cross-validation was achieved by comparing the results obtained on Cl- and on Br-basis. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. U-Th-Pb systematics of some granitoids from the northeastern Yilgarn Block, Western Australia and implications for uranium source rock potential

    Energy Technology Data Exchange (ETDEWEB)

    Stuckless, J S; Nkomo, I T [Geological Survey, Denver, CO (USA); Bunting, J A [Geological Survey of Western Australia, Perth

    1981-11-01

    The Mount Boreas-type granite and spatially associated syenitic granitoid of Western Australia yield Pb-Pb ages of 2370 +- 100 Ma and 2760 +- 210 Ma, respectively. Th-Pb ages, although less precise, are concordant with these ages, and therefore the apparent ages are interpreted to be the crystallisation ages for these two units. U-Pb ages are variable and for the most part anomalously old, which suggests a Cainozoic uranium loss. However, this loss is generally small (3..mu..g/g); therefore, neither granitoid in its fresh state provides a good source for nearby calcrete-hosted uranium deposits. The possibility remains that the Mount Boreas-type granite that has been completely weathered during the Tertiary could have been a source for the calcrete-type uranium deposits in W.A. Although the Mount Boreas-type granite is highly fractionated, it does not bear a strong geochemical imprint of a sedimentary precursor. This feature contrasts it with apparently fresh granitoids from other parts of the world that have lost large amounts of uranium (approx. 20..mu..g/g) and are associated with large roll-type and other low temperature-type uranium deposits.

  10. 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.

  11. 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...

  12. Chemical U-Th-Pb dating of monazite by 3D-Micro x-ray fluorescence analysis with synchrotron radiation

    DEFF Research Database (Denmark)

    Schmitz, Susanne; Möller, Andreas; Wilke, Max

    2009-01-01

    A confocal set-up for three-dimensional (3D) micro X-ray fluorescence (micro-XRF) was used at the mySpot beamline at BESSY II, which allows compositional depth profiling for various applications. We present results obtained with a confocal 3D micro-XRF set-up for chemical age dating using the U, Th...... and Pb concentrations of monazite within rock thin sections. The probing volume was determined to be approximately 21 × 21 × 24 µm3 for W-La using an excitation energy of 19 keV. The relative detection limits particularly for Pb are below 10 ppm (for counting times of 1000 s). Therefore, this 3D micro...... of ages, varying from 20 Ma to 1.82 Ga. Reference materials (GM3, F6, 3345) can be reproduced within error. The spread in the ages of all points determined by 3D micro-XRF is within 8 % of the isotopic reference value. The average 3D micro-XRF dates reproduce the reference ages with discrepancies between...

  13. 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)

  14. 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

  15. Determination of 230Th/232Th and correct methods by High Resolution Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Xie Shengkai; Guo Dongfa; Tan Jing; Zhang Yanhui; Huang Qiuhong; Gao Aiguo

    2013-01-01

    It is very important for the rapid and reliable determination of 230 Th/ 232 Th in the thorium-230 dating. A method of measuring 230 Th/ 232 Th in natural samples by high resolution inductively coupled plasma mass spectrometer (HR-ICP-MS) was developed on the base of our former work. The precise and accurate of natural 230 Th in geology samples is challenging, as the peak tailing to the high intensity of neighboring peak at 232 Th and the mass discrimination of the instrument. The peak tailing of 238 U to 236 U was used to decrease the peak tailing effect of 232 Th to 230 Th. The mass discrimination factor K between ture and measured isotope ratio was calculated after measuring different 230 Th/ 232 Th ratio solutions. Lab used standard samples was digested in mixed acids of HN0 3 -HF-HCI-HCl0 4 , and separated by the Bio-rad AG 1 × 8 Cl - resin. The measurement method of blank-standard-blank-sample procession was used to determinate the 230 Th/ 232 Th. The measured result of 230 Th/ 232 Th was at (7.29 ± 0.34) × 10 -6 , which agreed with the reference value of (7.33 ± 0.17) × 10 -6 . (authors)

  16. 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...

  17. 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

  18. Development of Analytical methods for the evaluation of the impact of phosphate fertilizer industry on marine environment

    International Nuclear Information System (INIS)

    Aoun, M.

    2014-01-01

    Phosphate industries are considered an important potential source of natural radionuclides and heavy metals contamination in the environment. The objective of this work was to assess the marine environmental metallic and radiological pollution and the toxicological impact caused by a large production plant of phosphate fertilizer located on the eastern coast of the Mediterranean Sea, 40 km north of the capital of Lebanon: Beirut. Since 1957 this industry has been producing a large set of phosphate based fertilizers. Phosphogypsum, by-product resulting in the industrial procedure, is released directly in the marine environment. Natural radionuclides (238U, 235U, 226Ra, 232Th, 210Po, 210Pb, and 40K) and anthropogenic 137Cs were measured by alpha and gamma spectrometry in seawater, sediment, coastal sediment and biota. An alpha spectrometer with a passive ion implanted silicon detector was used for the determination of 238U, 234Uin sea water and 210Poin biota samples. 238U, 235U, 232Th, 226Ra,210Pb,137Cs and 40Kin biota and sediments were analyzed by a gamma spectrometer from Canberra, equipped with an extended range low-level coaxial high purity germanium detector with beryllium window.In addition, the radiation exposure of the population surrounding the industrial plant and the internal exposure and potential risks to human due to 210Poand 210Pbassociated with the consumption of fish have been estimated. The internal exposure due to the consumption of fish is important from the radioecology and radioprotection perspectives, and the data for most species studied, are reported for the first time in Lebanon. A multi-elemental method for simultaneous determination of trace elements in seaweeds based on the use of the new approach of collision reaction interface for the ICP-MS determination was optimized. The performance characteristics including linearity, limits of detection and quantification, repeatability, accuracy and truenesswere evaluated. Investigations on the

  19. 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.

  20. 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.

  1. 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)

  2. 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

  3. Preconcentration of uranium, thorium, zirconium, titanium, molybdenum and vanadium with oxine supported on microcrystalline naphthalene and their determinations by ICP-AES

    International Nuclear Information System (INIS)

    Kumar, Naveen; Kumar, Sanjay; Kumar, Vijay; Nandakishore, S.S.; Bangroo, P.N.

    2013-01-01

    As an effective technique for separation and preconcentration of trace elements, solid-liquid extraction with microcrystalline naphthalene has received great attention in recent years. The application of the adsorption of the metal complexes on microcrystalline naphthalene has greatly enhanced the utility of solid-liquid extraction in trace analysis. A survey of the literature revealed that single element detection techniques such as spectrophotometry, atomic absorption spectrometry, and polarography were mostly combined with this separation method. However, multi-element simultaneous detection techniques, like ICP-AES and ICP-MS were seldom used as the detectors in this solid-liquid extraction method. The aim of this work was to attempt to adopt the reagent oxine for the separation and subsequent determination of U, Th, Zr, Ti, Mo and V by ICP-AES, after adsorption of their oxinate complexes on microcrystalline naphthalene

  4. 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.

  5. 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

  6. Rapid Analysis of U isotopic ratios in Food Stuff samples using Fusion and ICP-MS measurement: For radiation monitoring program in the vicinity of nuclear facilities

    Energy Technology Data Exchange (ETDEWEB)

    Lim, Jong Myoung; Park, Ji Young; Jung, Yoon Hee; Kim, Hyun Cheol; Kim, Won Young; Chung, Gun Ho; Kang, Mun Ja [KAERI, Daejeon (Korea, Republic of)

    2016-05-15

    In this study, a rapid digestion and separation method for U isotopes was developed in food stuff matrix such as cabbage and rice. As an attempt to reduce social costs and apprehension arising from the radioactivity in food, an accurate and rapid assessment of radioactivity is highly desirable. Hence, it is very important to develop a series of evaluation of rapid procedures for efficient radioactivity management in food. Contrary to the α-spectrometry method, a measurement technique using ICP-MS with an advanced sample introduction and mass counting system allows radioactivity in many samples to be measured with a short time period with a high degree of accuracy and precision. In order to satisfy the method detectable activity (MDA) for the regulation of radioactivity monitoring program the analysis of U isotopes always require the extremely large sample amount. These procedures make usually the food stuff sample to carbonize during dry ashing process. The ashed residues have been especially complicated into a liquid phase because of their carbonization. This process are very time consuming and not fully recovered target isotopes.

  7. 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

  8. 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.

  9. Effect of organic matrices on the determination of the trace element chemistry (Mg, Sr, Mg/Ca, Sr/Ca) of aragonitic bivalve shells (Arctica islandica). Comparison of ICP-OES and LA-ICP-MS data

    International Nuclear Information System (INIS)

    Schoene, Bernd R.; Zhang, Zengjie; Jacob, Dorrit; Soldate, Analia; Gillikin, David P.; Tuetken, Thomas; Garbe-Shoenberg, Dieter; McConnaughey, Ted

    2010-01-01

    The element chemistry of biogenic carbonates can provide important data on past environments. However, the Sr/Ca and Mg/Ca ratios as well as the Mg and Sr concentrations of biological carbonates, especially aragonitic bivalves often depart from apparent thermodynamic equilibrium. When measured in situ by means of LA-ICP-MS, the Mg concentration is often substantially enriched (two- to threefold) near the organic-rich, annual growth lines. To test the hypothesis that some organic components exert a major influence on the skeletal metal content, the element chemistry of different shell components (insoluble organic matrix, IOM; dissolved CaCO 3 and soluble organics, SOM) of Arctica islandica was measured by means of ICP-OES and LA-ICP-MS. The ICP-OES data indicate that the IOM is strongly enriched in Mg (130 ppm) and depleted in Sr and Ca (10 ppm and 0.22 wt%, respectively) when compared to the whole biomineral (Mg: 68 to 99 ppm, Sr: 860 to 1,060 ppm, Ca: ∼35.72 wt%). Although the average relative abundance of the IOM barely exceeds 0.46 wt%, its chemical composition in combination with its heterogeneous distribution across the shell can significantly increase estimates of the Mg concentration if measured in situ by LA-ICP-MS. Depending on the distribution of the IOM, the Ca concentration may be significantly lower locally than the average Ca concentration of the whole shell (35.72 wt%). If this remains undetected, the Mg concentration of shell portions with higher than average IOM content is overestimated by LA-ICP-MS and, conversely, the Mg concentration is underestimated in shell portions with lower than average IOM content. Removal of the IOM prior to the chemical analysis by LA-ICP-MS or mathematical correction for the IOM-derived magnesium concentrations is therefore strongly advised. The different chemistry of the IOM may also exert a major control on the trace element to calcium ratios. Shell portions enriched in IOM will show up to 200 times higher Mg

  10. 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.

  11. 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.

  12. 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)

  13. 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

  14. 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%.

  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. 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.

  17. A feasibility study of U-Pb and Pb-Pb dating of kimberlites using groundmass mineral fractions and whole-rock samples

    International Nuclear Information System (INIS)

    Kramers, J.D.; Smith, C.B.

    1983-01-01

    This paper describes partly successful attempts to determine emplacement ages of kimberlites by U-Pb and Pb-Pb methods involving groundmass minerals with high U content (notably perovskite) and whole-rock kimberlite samples. U/Pb ratios in perovskite in the matrix of kimberlites can be two orders of magnitude larger than in the rest of the kimberlite material, and with simple mineral separation techniques moderate success was achieved in U-Pb dating of fresh samples of younger kimberlites (around 100 Ma). The differences in U/Pb ratios between kimberlite samples from different parts of the same pipe have also been found to be large enough, in some cases, to allow reasonably accurate U-Pb age determination. In older kimberlites the U-Pb ages obtained were mostly imcompatible with geological constraints and results obtained by other methods. However, for such pipes use of Pb-Pb systematics yields realistic age limits in some cases

  18. 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.

  19. 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

  20. Multielement determination and speciation of major-to-trace elements in black tea leaves by ICP-AES and ICP-MS with the aid of size exclusion chromatography

    International Nuclear Information System (INIS)

    Matsuura, Hirotaka; Hokura, Akiko; Katsuki, Fumie; Itoh, Akihide; Haraguchi, Hiroki

    2001-01-01

    A multielement determination of major-to-trace elements in black tea leaves and their tea infusions was carried out by ICP-AES (inductively coupled plasma atomic emission spectrometry) and ICP-MS (inductively coupled plasma mass spectrometry). Tea infusions were prepared as usual tea beverage by brewing black tea leaves in boiling water for 5 min. About 40 elements in tea leaves and tea infusions could be determined over the wide concentration range in 8 orders of magnitude. The extraction efficiency of each element was estimated as the ratio of its concentration in tea infusions to that in tea leaves. From the experimental results for the extraction efficiencies, the elements in black tea leaves were classified into three characteristic groups: (i) highly-extractable elements (>55%): Na, K, Co, Ni, Rb, Cs and Tl, (ii) moderately-extractable elements (20-55%): Mg, Al, P, Mn and Zn, and (iii) poorly-extractable elements (<20%): Ca, Fe, Cu, Sr, Y, Zr, Mo, Sn, Ba and lanthanoid elements. Furthermore, speciation of major-to-trace elements in tea infusions was performed by using a combined system of size exclusion chromatography (SEC) and ICP-MS (or ICP-AES). As a result, many diverse elements were found to be present as complexes associated with large organic molecules in tea infusions. (author)

  1. 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

  2. Bioaccumulation of Uranium and Thorium by Lemna minor and Lemna gibba in Pb-Zn-Ag Tailing Water.

    Science.gov (United States)

    Sasmaz, Merve; Obek, Erdal; Sasmaz, Ahmet

    2016-12-01

    This study focused on the ability of Lemna minor and Lemna gibba to remove U and Th in the tailing water of Keban, Turkey. These plants were placed in tailing water and individually fed to the reactors designed for these plants. Water and plant samples were collected daily from the mining area. The plants were ashed at 300°C for 1 day and analyzed by ICP-MS for U and Th. U was accumulated as a function of time by these plants, and performances between 110 % and 483 % for L. gibba, and between 218 % and 1194 % for L. minor, were shown. The highest Th accumulations in L. minor and L. gibba were observed at 300 % and 600 % performances, respectively, on the second day of the experiment. This study indicated that both L. gibba and L. minor demonstrated a high ability to remove U and Th from tailing water polluted by trace elements.

  3. Pleistocene apparent ages by U-Pb isotope and U-series methods for uranium ore in Dakota Sandstone near Gallup, New Mexico

    International Nuclear Information System (INIS)

    Ludwig, K.R.; Szabo, B.J.; Granger, H.C.

    1977-01-01

    Radiometric dates of a high-grade uranium ore from the Hogback No. 4 mine in Dakota Sandstone near Gallup, N. Mex., indicate a late Pleistocene age of mineralization. The 206 Pb/ 238 U and 207 Pb/ 235 U apparent ages of about 70,000 y and 100,000 y, respectively, are discordant, but are in broad agreement with the discordant 230 Th/ 238 U and 230 Pa/ 235 U apparent ages of 130,000 y and 78,000 y, respectively. Although it is not clear how the analyzed sample relates to the main period of mineralization at this mine, these dates are consistent with previous age limits suggested for Dakota Sandstone uranium ores

  4. 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...

  5. 230Th-238U radioactive disequilibria in tholeiites from the FAMOUS zone (Mid-Atlantic Ridge, 36050'N): Th and Sr isotopic geochemistry

    International Nuclear Information System (INIS)

    Condomines, M.; Morand, P.; Allegre, C.J.

    1981-01-01

    We analyzed, U, Th and 230 Th/ 232 Th activity ratios for a few tholeiites from the Mid-Atlantic Ridge FAMOUS zone at 36 0 50'N. The results show a fairly wider scatter for both Th/U and ( 230 Th/ 232 Th) ratios. Seawater contamination appears to be responsible for this scatter and, for the uranium, produces an increase in content yielding a ( 234 U/ 238 U) ratio greater than 1 and, for the Th, an increase of the ( 230 Th/ 232 Th) ratio which is a very sensitive indicator for contamination. Also, the latter often is selective: U, Th and Sr are not affected in the same manner. When discarding all data for contaminated samples, the FAMOUS zone appears to be very homogeneous with a Th/U ratio value of 3.05 and a ( 230 Th/ 232 Th) ratio value of 1.24. Comparison with other active volcanic areas reveals a negative correlation between ( 230 Th/ 232 Th) and 87 Sr/ 86 Sr ratios for present lavas which is indicative of a consistency in Th-U and Rb-Sr fractionation in the source regions of these magmas. The Th isotopic geochemistry can thus provide useful information for the study of present volcanism, information as valuable as that from Sr, Pb or Nd isotopes. (orig.)

  6. 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)

  7. 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.

  8. Brittle-ductile deformation effects on zircon crystal-chemistry and U-Pb ages: an example from the Finero Mafic Complex (Ivrea-Verbano Zone, western Alps)

    Science.gov (United States)

    Langone, Antonio; José Alberto, Padrón-Navarta; Zanetti, Alberto; Mazzucchelli, Maurizio; Tiepolo, Massimo; Giovanardi, Tommaso; Bonazzi, Mattia

    2016-04-01

    A detailed structural, geochemical and geochronological survey was performed on zircon grains from a leucocratic dioritic dyke discordantly intruded within meta-diorites/gabbros forming the External Gabbro unit of the Finero Mafic Complex. This latter is nowadays exposed as part of a near complete crustal section spanning from mantle rocks to upper crustal metasediments (Val Cannobina, Ivrea-Verbano Zone, Italy). The leucocratic dyke consists mainly of plagioclase (An18-24Ab79-82Or0.3-0.7) with subordinate amounts of biotite, spinel, zircon and corundum. Both the leucocratic dyke and the surrounding meta-diorites show evidence of ductile deformation occurred under amphibolite-facies conditions. Zircon grains (up to 2 mm in length) occur mainly as euhedral grains surrounded by fine grained plagioclase-dominated matrix and pressure shadows, typically filled by oxides. Fractures and cracks within zircon are common and can be associated with grain displacement or they can be filled by secondary minerals (oxides and chlorite). Cathodoluminescence (CL) images show that zircon grains have internal features typical of magmatic growth, but with local disturbances. However EBSD maps on two selected zircon grains revealed a profuse mosaic texture resulting in an internal misorientation of ca. 10o. The majority of the domains of the mosaic texture are related to parting and fractures, but some domains show no clear relation with brittle features. Rotation angles related to the mosaic texture are not crystallographically controlled. In addition, one of the analysed zircons shows clear evidence of plastic deformation at one of its corners due to indentation. Plastic deformation results in gradual misorientations of up to 12o, which are crystallographically controlled. Trace elements and U-Pb analyses were carried out by LA-ICP-MS directly on petrographic thin sections and designed to cover the entire exposed surface of selected grains. Such investigations revealed a strong

  9. A Procedure for the Sequential Determination of Radionuclides in Phosphogypsum Liquid Scintillation Counting and Alpha Spectrometry for 210Po, 210Pb, 226Ra, Th and U Radioisotopes

    International Nuclear Information System (INIS)

    2014-01-01

    Since 2004, the Environment Programme of the IAEA has included activities aimed at the development of a set of procedures for the determination of radionuclides in terrestrial environmental samples. Reliable, comparable and 'fit for purpose' results are essential requirements for any decision based on analytical measurements. For the analyst, tested and validated analytical procedures are extremely important tools for the production of such analytical data. For maximum utility, such procedures should be comprehensive, clearly formulated, and readily available to both the analyst and the customer for reference. In this publication, a combined procedure for the sequential determination of 210Po, 210Pb, 226Ra, Th and U radioisotopes in phosphogypsum is described. The method is based on the dissolution of small amounts of phosphogypsum by microwave digestion, followed by sequential separation of 210Po, 210Pb, Th and U radioisotopes by selective extraction chromatography using Sr, TEVA and UTEVA resins. Radium-226 is separated from interfering elements using Ba(Ra)SO4 co-precipitation. Lead-210 is determined by liquid scintillation counting. The alpha source of 210Po is prepared by autodeposition on a silver plate. The alpha sources of Th and U are prepared by electrodeposition on a stainless steel plate. A comprehensive methodology for the calculation of results, including the quantification of measurement uncertainty, was also developed. The procedure is introduced as a recommended procedure and validated in terms of trueness, repeatability and reproducibility in accordance with ISO guidelines

  10. 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...

  11. Determination of trace levels of iodine in table salt by ICP-TOF MS

    International Nuclear Information System (INIS)

    Waqar, F.; Muhammad, B.; Hakim, M.; Jan, S.

    2012-01-01

    An ion exchange method was established for the effective removal of sodium matrix for iodine determination by ICP-TOF-MS technique. Since the direct determination of trace level analytes in the presence of heavy matrix is not recommended by this technique. Therefore, the removal of matrix is essentially required to achieve better detection limits and to avoid memory effects. The extraction system was designed for the removal of matrix prior to the analysis by ICP-MS, various parameters were optimized to achieve efficient removal of matrix. The accuracy of the method was evaluated by spiking salt samples with known amount of iodine (50 mu g/g) and % recoveries were calculated. The recoveries obtained were > 98% with relative standard deviation (RSD) < 5%. The established method was applied for the analysis of commercially available iodized table salt samples. The results and % recoveries are given. The most commonly used iodo metric titration method is not satisfactory as it has 5-10 % quantitative error. Our method is reliable and could be conveniently applied for the determination of iodine in table salt samples. (Orig./A.B.)

  12. Temporal evolution of natural radionuclides distributions {sup 238}U, {sup 234}Th, {sup 226}Ra, {sup 228}Ra, {sup 210}Pb and {sup 210}Po in the Bransfield strait, Antarctica peninsula; Evolucao temporal das distribuicoes dos radionuclideos naturais {sup 238}U, {sup 234}Th, {sup 226}Ra, {sup 228}Ra, {sup 210}Pb and {sup 210}Po no estreito de Bransfiel, peninsula Antartica

    Energy Technology Data Exchange (ETDEWEB)

    Lapa, Flavia Valverde

    2013-07-01

    Research on the distribution of natural radionuclides in Antarctica is rare and thus, there is great interest in to know their occurrence and factors related to its mobilization, transference and accumulation in this extremely fragile environment. Natural radionuclides have been used intensively as tracers in the ocean, helping to better understand processes as sinking and particle resuspension, water masses mixture and oceanic circulation. {sup 234}Th (t½ = 24.1 days) is a particle-reactive radionuclide produced continuously in seawater by the decay of its soluble precursor conservative with salinity {sup 238}U (t½ = 4.5 10{sup 9} years). Since {sup 234}Th presents relatively short half-life, it is used to quantify processes that occur in temporal scale varying from days to weeks. The disequilibrium {sup 234}Th/{sup 238}U in the surface ocean has been applied to estimate carbon fluxes exported via sinking material. The flux of particles biologically productive out of the euphotic zone in the Southern Ocean has special attention due to its importance in the control of CO{sub 2} atmospheric concentrations. The radionuclides {sup 210}Pb (t½ = 22.3 years) and {sup 210}Po (t½ = 138 days) are also particle-reactive. The disequilibrium {sup 210}Po/{sup 210}Pb has been used to estimate fluxes of particles exported in the ocean in the time scale of weeks. The long-lived Ra isotopes, {sup 226}Ra (t½ = 1,600 years) and {sup 228}Ra (t½ = 5.75 years) are soluble in seawater, presenting unique properties that make them excellent tracers of water masses. This research work had the aim to study the distributions of natural radionuclides {sup 238}U, {sup 234}Th, {sup 22}'6Ra, {sup 22}'8Ra, {sup 210}Pb and {sup 210}Po in the Bransfield Strait during 2 samplings carried out in the 2011 Austral Summer (OPERANTAR XXIX and XXX). (author)

  13. Dating of zircon from high-grade rocks: Which is the most reliable method?

    Directory of Open Access Journals (Sweden)

    Alfred Kröner

    2014-07-01

    Full Text Available Magmatic zircon in high-grade metamorphic rocks is often characterized by complex textures as revealed by cathodoluminenscence (CL that result from multiple episodes of recrystallization, overgrowth, Pb-loss and modifications through fluid-induced disturbances of the crystal structure and the original U-Th-Pb isotopic systematics. Many of these features can be recognized in 2-dimensional CL images, and isotopic analysis of such domains using a high resolution ion-microprobe with only shallow penetration of the zircon surface may be able to reconstruct much of the magmatic and complex post-magmatic history of such grains. In particular it is generally possible to find original magmatic domains yielding concordant ages. In contrast, destructive techniques such as LA-ICP-MS consume a large volume, leave a deep crater in the target grain, and often sample heterogeneous domains that are not visible and thus often yield discordant results which are difficult to interpret. We provide examples of complex magmatic zircon from a southern Indian granulite terrane where SHRIMP II and LA-ICP-MS analyses are compared. The SHRIMP data are shown to be more precise and reliable, and we caution against the use of LA-ICP-MS in deciphering the chronology of complex zircons from high-grade terranes.

  14. 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

  15. Transfer of 238U, 230Th, 226Ra, and 210Pb from soils to tree and shrub species in a Mediterranean area

    International Nuclear Information System (INIS)

    Blanco Rodriguez, P.; Vera Tome, F.; Lozano, J.C.; Perez Fernandez, M.A.

    2010-01-01

    The soil-to-plant transfer factors of natural uranium isotopes ( 238 U and 234 U), 230 Th, 226 Ra, and 210 Pb were studied in a disused uranium mine located in the Extremadura region in the south-west of Spain. The plant samples included trees (Quercus ilex, Quercus suber, and Eucalyptus cameldulensis) and one shrub (Cytisus multiflorus). All of them are characteristic of Mediterranean environments. The activity concentrations in leaves and fruit were determined for the tree species at different stages of growth. For the shrub, the total above-ground fraction was considered in three seasons. For old leaves and fruit, the highest activity concentrations were found in Eucalyptus cameldulensis for all the radionuclides studied, except in the case of 230 Th that presented similar activity concentrations in all of the tree species studied. In every case, the transfer to fruit was less than the transfer to leaves. In the shrub, the results depended on the season of sampling, with the highest value obtained in spring and the lowest in autumn. Important correlations were obtained for 238 U and 226 Ra between the activity ratio in soils with that in leaves or fruit.

  16. The Pan-African Kekem gabbro-norite (West-Cameroon), U-Pb zircon age, geochemistry and Sr-Nd isotopes: Geodynamical implication for the evolution of the Central African fold belt

    Science.gov (United States)

    Kwékam, Maurice; Affaton, Pascal; Bruguier, Olivier; Liégeois, Jean-Paul; Hartmann, Gerald; Njonfang, Emmanuel

    2013-08-01

    The Kekem shoshonitic gabbro-norite association is part of the high-K calc-alkaline (HKCA) post-collisional magmatism, a major feature of the Pan-African Belt in Cameroon. LA-ICP-MS U-Pb zircon analyses provide an age of 576 ± 4 Ma for the Kekem complex. This age is interpreted as dating the emplacement of the massif during the waning stage of the Pan-African orogeny. The latter is related to dextral movements along the Central Cameroon Shear Zone (CCSZ). The REE patterns display enriched LREE (LaN/YbN = 14.2-23.5) while HREE present a nearly flat profile (DyN/YbN = 1.3-1.7), and the La/Sm and Sm/Yb ratios led to propose that the Kekem gabbro-norites have been derived from the partial melting of a garnet-spinel lherzolite mantle source. The negative Nb-Ta and Ti anomalies and the positive Pb anomalies indicate that this mantle source was modified by contribution of a subduction-related material. The low Ce/Pb (2.6-10.4) and Th/Yb ratios associated to high Ba/La ratios, indicate that source enrichment could be related to slab derived fluids. As a whole, the Kekem geochemical features suggest that primary gabbro-noritic magmas derived from a subduction-modified mantle source (metasomatised lithospheric mantle). Moderately high 86Sr/87Sr initial ratios (0.7068-0.7082), low ɛNd (-5 to -9) and old Nd TDM model ages (1.6-1.8 Ga) are interpreted to result from contamination of Neoproterozoic mantle by the Paleoproterozoic crust. The ca. 576 Ma movements along the CCSZ are related to a Neoproterozoic metacratonization of the northern margin of the Congo craton during the Pan-African orogeny. This metacratonization led to vertical planar lithospheric delamination along lithospheric transcurrent faults, asthenospheric uprise and partial melting of the Paleoproterozoic lithospheric mantle.

  17. Ediacaran ( 620 Ma) high grade regional metamorphism in the northern Arabian Nubian Shield: U/Th-Pb monazite ages of the Elat schist

    Science.gov (United States)

    Elisha, Bar; Katzir, Yaron; Kylander-Clark, Andrew

    2017-04-01

    Ediacaran times witnessed a hemisphere-scale orogenesis forming the extensive Pan-African mountain ranges and resulting in the final assembly of Gondwana supercontinent. The Elat metamorphic basement (S Israel) located at the northernmost tip of a major Pan-African orogenic suture, the Arabian Nubian Shield (ANS), comprises amphibolite facies schists and gneisses and was most likely shaped by this major continental collision. However the timing, number and duration of metamorphic events in Elat and elsewhere in the ANS are non-conclusive and a major emphasis was given to pre-Ediacaran island-arc related tectonics. This is mostly because U-Pb dating of zircon, widely used in Elat and elsewhere, is very successful in constraining the ages of the igneous and sedimentary protoliths, but is 'blind' to metamorphism at grades lower than granulite. Here U/Th-Pb dating of monazite, a precise chronometer of metamorphic mineral growth, is systematically applied to the Elat schist and unveils the tectono-metamorphic evolution of the Elat basement. Previous U-Pb dating of detrital zircon has shown that the sedimentary protoliths of the Elat schist are the oldest basement components (≥800 Ma), and detailed structural observations of the schists portrayed a complex deformation history including four successive phases (Shimron, 1972). The earliest three phases were defined as ductile and penetrative, but some of the available geochronological data apparently contradict field relations. In-situ analysis of metamorphic monazites by LASS (Laser Ablation Split Stream) involves simultaneous measurement of U/Th-Pb isotope ratios and REE contents in a single 10 μm sized grain or domain, thus allowing determining the age of specific texture and metamorphic assemblage. Monazite dating of the Elat schist yielded two concordant age clusters at 712±6 and 613±5 Ma. The corresponding REE patterns of the dated monazite grains indicate that porphyroblast growth, either garnet or staurolite

  18. 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...

  19. Zircon U-Pb geochronology and geochemistry of granites in the Zhuguangshan complex, South China: Implications for uranium mineralization

    Science.gov (United States)

    Zhang, Long; Chen, Zhenyu; Li, Xiaofeng; Li, Shengrong; Santosh, M.; Huang, Guolong

    2018-05-01

    The Zhuguangshan complex, composed of Caledonian, Indosinian, and Yanshanian granites, and Cretaceous mafic dykes, is one of the most important granite-hosted uranium producers in South China. Here we present LA-ICP-MS zircon U-Pb and hornblende 40Ar/39Ar geochronology and whole-rock and biotite geochemistry for the granites in this complex to evaluate the magmatism and its constraints on uranium mineralization. Samples collected from the Fuxi, Youdong, Longhuashan, Chikeng, Qiling, and Sanjiangkou intrusions yield zircon weighted 206Pb/238U ages of 426.7 ± 5.4 Ma, 226.4 ± 3.5 Ma, 225.0 ± 2.7 Ma, 152.2 ± 3.0 Ma, 153.9 ± 2.1 Ma, and 155.2 ± 2.1 Ma, respectively. A new Ar-Ar dating of the hornblende of the diabase from the Changjiang uranium ore field yields a plateau age of 145.1 ± 1.5 Ma. These results coupled with published geochronological data indicate that six major magmatic events occurred in the study area at 420-435 Ma, 225-240 Ma, 150-165 Ma, 140 Ma, 105 Ma, and 90 Ma. Both U-bearing and barren granites occur in this complex, and they display differences in whole-rock and biotite geochemistry. The barren granites show higher Al2O3, CaO, TFMM, Rb, Zr, Ba, SI, Mg#, (La/Yb)N, and Eu/Eu*, but lower SiO2, ALK, Rb, DI, Rb/Sr, and TiO2/MgO than those of the U-bearing granites. Biotites in the U-bearing granites are close to the Fe-rich siderophyllite-annite end member with Fe/(Fe + Mg) ratios higher than 0.66, whereas those in the barren granites are relatively close to the Mg-rich eastonite-phlogopite end member with Fe/(Fe + Mg) ratios uranium ore potential of the granites in the Zhuguangshan complex. The geochemical variations of U-bearing and barren granites can serve as a potential detector for granite-hosted uranium deposits.

  20. 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.

  1. Significance of zircon U-Pb ages from the Pescadero felsite, west-central California coast ranges

    Science.gov (United States)

    McLaughlin, Robert J.; Moore, Diane E.; ,; Martens, UWE C.; Clark, J.C.

    2011-01-01

    Weathered felsite is associated with the late Campanian–Maastrichtian Pigeon Point Formation near Pescadero, California. Poorly exposed, its age and correlation are uncertain. Is it part of the Pigeon Point section west of the San Gregorio–Hosgri fault? Does it rest on Nacimiento block basement? Is it dextrally offset from the Oligocene Cambria Felsite, ∼185 km to the southeast? Why is a calc-alkaline hypabyssal igneous rock intrusive into the outboard accretionary prism? To address these questions, we analyzed 43 oscillatory-zoned zircon crystals from three incipiently recrystallized pumpellyite ± prehnite ± laumontite-bearing Pescadero felsite samples by sensitive high-resolution ion microprobe–reverse geometry (SHRIMP-RG) and laser ablation–inductively coupled plasma–mass spectrometry (LA-ICP-MS) techniques. Thirty-three zircons gave late Mesozoic U-Pb ages, with single-grain values ranging from 81 to 167 Ma; ten have pre-Mesozoic, chiefly Proterozoic ages. A group of the four youngest Pescadero zircons yielded an apparent maximum igneous age of ca. 86–90 Ma. Reflecting broad age scatter and presence of partly digested sandstone inclusions, we interpret the rest of the zircons (perhaps all) as xenocrysts. Twenty-three zircons were separated and analyzed from two samples of the similar Cambria Felsite, yielding a unimodal 27 Ma U-Pb age. Clearly, the origin of the Upper Oligocene Cambria Felsite is different from that of the Upper Cretaceous Pescadero felsite; these rocks are not correlated, and do not constrain displacement along the San Gregorio–Hosgri fault. Peak ages differ slightly, but relative probability curves for Mesozoic and pre-Mesozoic Pescadero zircons compare well, for example, with abundant U-Pb age data for detrital zircons from Franciscan metaclastic strata ∼100 km to the east in the Diablo Range–San Francisco Bay area, San Joaquin Great Valley Group turbidites, Upper Cretaceous Nacimiento block Franciscan strata, and Upper

  2. 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 retenti