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Sample records for plasma-mass spectrometry etv-icp-ms

  1. 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.)

  2. Electrothermal vaporisation ICP-mass spectrometry (ETV-ICP-MS) for the determination and speciation of trace elements in solid samples - A review of real-life applications from the author's lab

    Energy Technology Data Exchange (ETDEWEB)

    Vanhaecke, Frank; Resano, Martin; Moens, Luc [Laboratory of Analytical Chemistry, Ghent University, Institute for Nuclear Sciences, Proeftuinstraat 86, 9000 Ghent (Belgium)

    2002-09-01

    The use of electrothermal vaporisation (ETV) from a graphite furnace as a means of sample introduction in inductively coupled plasma mass spectrometry (ICP-MS) permits the direct analysis of solid samples. A multi-step furnace temperature programme is used to separate the vaporisation of the target element(s) and of the matrix components from one another. Sometimes, a chemical modifier is used to enable a higher thermal pre-treatment temperature, by avoiding premature analyte losses (stabilisation) or promoting the selective volatilisation of matrix components. In almost all instances, accurate results can be obtained via external calibration or single standard addition using an aqueous standard solution. Absolute limits of detection are typically 1 pg, which corresponds to 1 ng/g for a typical sample mass of 1 mg. Real-life applications carried out in the author's lab are used to illustrate the utility of this approach. These applications aim at trace element determination in industrial and environmental materials. The industrial materials analysed include different types of plastics - Carilon, polyethylene, poly(ethyleneterephtalate) and polyamide - and photo- and thermographic materials. As samples from environmental origin, plant material, animal tissue and sediments were investigated. Some applications aimed at a multi-element determination, while in other, the content of a single, but often challenging, element (e.g., Si or S) had to be measured. ETV-ICP-MS was also used in elemental speciation studies. Separation of Se-containing proteins was accomplished using polyacrylamide gel electrophoresis (PAGE). Subsequent quantification of the Se content in the protein spots was carried out using ETV-ICP-MS. As the volatilisation of methylmercury and inorganic mercury could be separated from one another with respect to time, no chromatographic or electrophoretic separation procedure was required, but ETV-ICP-MS as such sufficed for Hg speciation in fish tissue

  3. Solid phase extraction for analysis of biogenic carbonates by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS): an investigation of rare earth element signatures in otolith microchemistry

    International Nuclear Information System (INIS)

    Arslan, Zikri; Paulson, Anthony J.

    2003-01-01

    Uptake of trace elements into fish otoliths is governed by several factors such as life histories and environment in addition to stock and species differences. In an attempt to elucidate the elemental signatures of rare earth elements (REEs) in otoliths, a solid phase extraction (SPE) protocol was used in combination with electrothermal vaporization (ETV) as a sample introduction procedure for the determinations by inductively coupled plasma quadrupole mass spectrometry (ICP-MS). Effects of various parameters, such as carrier gas flow rate, atomization temperature and chemical modification, were examined for optimization of the conditions by ETV-ICP-MS. Atomization was achieved at 2800 deg. C. Lower temperatures (i.e. 2600 deg. C) resulted in severe memory problems due to incomplete atomization. Palladium was used as a chemical modifier. It was found that an increase in Pd concentration up to 0.5 μg in the injection volume (70 μl) led up to four-fold enhancement in the integrated signals. This phenomenon is attributed to the carrier effect of Pd rather than the stabilization since no significant losses were observed for high temperature drying around 700 deg. C even in the absence of Pd. Preconcentration was performed on-line at pH 5 by using a mini-column of Toyopearl AF-Chelate 650M chelating resin, which also eliminated the calcium matrix of otolith solutions. After preconcentration of 6.4 ml of solution, the concentrate was collected in 0.65 ml of 0.5% (v/v) HNO 3 in autosampler cups, and then analyzed by ETV-ICP-MS. The method was validated with the analysis of a fish otolith certified reference material (CRM) of emperor snapper, and then applied to samples. Results obtained from otoliths of fish captured in the same habitat indicated that otolith rare earth element concentrations are more dependent on environmental conditions of the habitat than on species differences

  4. 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

  5. Simultaneous electrothermal vaporization and nebulizer sample introduction system for inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Arnquist, Isaac J.; Kreschollek, Thomas E.; Holcombe, James A.

    2011-01-01

    The novel analytical application of the combination of an inline electrothermal vaporization (ETV) and nebulization source for inductively coupled plasma mass spectrometry (ICP-MS) has been studied. Wet plasma conditions are sustained during ETV introduction by 200 mL/min gas flow through the nebulizer, which is merged with the ETV transport line at the torch. The use of a wet plasma with ETV introduction avoided the need to change power settings and torch positions that normally accompany a change from wet to dry plasma operating conditions. This inline-ETV source is shown to have good detection limits for a variety of elements in both HNO 3 and HCl matrices. Using the inline-ETV source, improved limits of detection (LOD) were obtained for elements typically suppressed by polyatomic interferences using a nebulizer. Specifically, improved LODs for 51 V and 53 Cr suffering from Cl interferences ( 51 ClO + and 53 ClO + respectively) in a 1% HCl matrix were obtained using the inline-ETV source. LODs were improved by factors of 65 and 22 for 51 V and 53 Cr, respectively, using the inline-ETV source compared to a conventional concentric glass nebulizer. For elements without polyatomic interferences, LODs from the inline-ETV were comparable to conventional dry plasma ETV-ICP time-of-flight mass spectrometry results. Lastly, the inline-ETV source offers a simple means of changing from nebulizer introduction to inline-ETV introduction without extinguishing the plasma. This permits, for example, the use of the time-resolved ETV-ICP-MS signals to distinguish between an analyte ion and polyatomic isobar.

  6. 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Lewis, L.A.

    1998-05-01

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

  8. Determination of 241Am in sediments by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS).

    Science.gov (United States)

    Agarande, M; Benzoubir, S; Bouisset, P; Calmet, D

    2001-08-01

    Trace levels (pg kg(-1)) of 241Am in sediments were determined by isotope dilution high resolution inductively coupled plasma mass spectrometry (ID HR ICP-MS) using a microconcentric nebulizer. 241Am was isolated from major elements like Ca and Fe by different selective precipitations. In further steps. Am was first separated from other transuranic elements and purified by anion exchange and extraction chromatography prior to the mass spectrometric measurements. The ID HR ICP-MS results are compared with isotope dilution alpha spectrometry.

  9. Electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of trace amount of lanthanides and yttrium in soil with polytetrafluroethylene emulsion as a chemical modifier

    International Nuclear Information System (INIS)

    He Man; Hu, Bin; Jiang Zucheng

    2005-01-01

    A method of electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) for the determination of trace lanthanides and yttrium in soil samples with a polytetrafluorethylene (PTFE) emulsion as chemical modifier to promote the vaporization of the analytes from the graphite furnace was developed in this paper. The analytical characteristics, spectral interference and matrix effect of the analytical method were evaluated and critically compared with those of pneumatic nebulization inductively coupled plasma mass spectrometry (PN-ICP-MS). Under the optimized operation conditions, the relative detection limits of lanthanides (La-Lu) and yttrium for ETV-ICP-MS and PN-ICP-MS were 0.4-20 ng l -1 and 1.0-21 ng l -1 , respectively, the absolute detection limits for ETV-ICP-MS were 4-200 fg, which were improved by 1-2 orders of magnitude compared with PN-ICP-MS. While the analytical precision of ETV-ICP-MS is worse than that of PN-ICP-MS, with the R.S.D.s (%) of 4.1-10% for the former and 2.9-7.8% for the latter. Regarding to the matrix effect, both conventional method and stepwise dilution method were employed to observe the effect of matrix and the very similar results were obtained. It was found that the highest tolerance concentration of the matrix is 1000 mg l -1 and 800 mg l -1 for ETV-ICP-MS and PN-ICP-MS, respectively. To assess the accuracy, the proposed method was applied to the determination of trace lanthanides and yttrium in three different soil standard reference materials and one soil sample, and the determined values are in good agreement with the certified values or reference values

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. High-resolution line-scan analysis of resin-embedded sediments using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS)

    NARCIS (Netherlands)

    Hennekam, R.; Jilbert, T.; de Lange, G.J.; Reichart, G.J.

    2015-01-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) line-scanning is a promising technique for producing high-resolution (µm-scale) geochemical records on resin-embedded sediments. However, this approach has not yet been thoroughly tested on sediment samples of known elemental

  15. High-resolution line-scan analysis of resin-embedded sediments using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS)

    NARCIS (Netherlands)

    Hennekam, Rick; Jilbert, Tom; Mason, Paul R D; de Lange, Gert J.; Reichart, Gert Jan

    2015-01-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) line-scanning is a promising technique for producing high-resolution (μm-scale) geochemical records on resin-embedded sediments. However, this approach has not yet been thoroughly tested on sediment samples of known elemental

  16. Measurements of β or α emitter long lived radionuclides using inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Provitina, O.

    1993-01-01

    The measurement of long-lived radionuclides is highly important for characterizing nuclear wastes for their later storage. The main techniques for characterizing these isotopes are α spectrometry, β counting and γ spectrometry. The large period of these isotopes leads to low specific activity needing time consuming measurements in order to obtain significant signals. Moreover, the radiometric techniques are often limited by problems of interferences involving several steps of pretreatments. Among these steps, the specific extraction with crown ethers is highly selective for the separation of 99 Tc, 129 I and 135 Cs particularly. The radiometric techniques are here replaced by inductively coupled plasma mass spectroscopy (ICP-MS) the advantages of which are: few interferences, sensitivity which does not depend on the radiologic period as compared to radiochemistry. ICP-MS can then measure 237 Np in enriched uranium matrix and thereby reduce by a factor of 4 the sample pretreatment and the duration of the analysis usually performed by α spectrometry. Another technique, electrothermal vaporization (ETV), is consequently used. Crown ether extraction-ETV-ICP-MS is employed for measuring the long lived radionuclides 99 Tc and 129 I. The conditions of the extraction and the parameters of the ETV and the ICP-MS are studied and optimized. The methods optimized (extraction, electrothermal vaporization) are validated in the case of 99 Tc, in real samples. The spike method is required to quantify technetium, the quantification with calibration leading to bad results. The results obtained are in good agreement with the expected values. Extraction of technetium on anionic resin and its measurement by the spike method with pneumatic nebulization-ICP-MS is also performed on other samples. Measured values are also in agreement with expected values, but the method of extraction is more time consuming (half a day) than the extraction with crown ether (one hour). (author). 54 figs

  17. Measurements of {beta} or {alpha} emitter long lived radionuclides using inductively coupled plasma mass spectrometry; Dosage a tres bas niveau de radionucleides a longue periode emetteurs {beta} ou {alpha} par spectrometrie de masse a couplage plasma inductif

    Energy Technology Data Exchange (ETDEWEB)

    Provitina, O

    1993-10-18

    The measurement of long-lived radionuclides is highly important for characterizing nuclear wastes for their later storage. The main techniques are {alpha} spectrometry, {beta} counting and {gamma} spectrometry. The large period of these isotopes leads to low specific activity needing time consuming measurements. Moreover, the radiometric techniques are often limited by problems of interferences involving several steps of pretreatments. Among these steps, the specific extraction with crown ethers is highly selective for the separation of {sup 99}Tc, {sup 129}I and {sup 135}Cs. The radiometric techniques are here replaced by inductively coupled plasma mass spectroscopy (ICP-MS) the advantages of which are: few interferences, sensitivity which does not depend on the radiologic period as compared to radiochemistry. ICP-MS can then measure {sup 237}Np in enriched uranium matrix and reduce by a factor of 4 the sample pretreatment and the duration of the analysis usually performed by {alpha} spectrometry. Another technique, electrothermal vaporization (ETV), is consequently used. Crown ether extraction-ETV-ICP-MS is employed for measuring the long lived radionuclides {sup 99}Tc and {sup 129}I. The conditions of the extraction and the parameters of the ETV and the ICP-MS are studied and optimized. The methods optimized (extraction, electrothermal vaporization) are validated in the case of {sup 99}Tc, in real samples. The spike method is required to quantify technetium, the quantification with calibration leading to bad results. The results obtained are in good agreement with the expected values. Extraction of technetium on anionic resin and its measurement by the spike method with pneumatic nebulization-ICP-MS is also performed on other samples. Measured values are also in agreement with expected values, but the method of extraction is more time consuming (half a day) than the extraction with crown ether (one hour). (author). 54 figs., 38 tabs.

  18. Imaging of Selenium by Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) in 2-D Electrophoresis Gels and Biological Tissues.

    Science.gov (United States)

    Cruz, Elisa Castañeda Santa; Susanne Becker, J; Sabine Becker, J; Sussulini, Alessandra

    2018-01-01

    Selenium and selenoproteins are important components of living organisms that play a role in different biological processes. Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is a powerful analytical technique that has been employed to obtain distribution maps of selenium in biological tissues in a direct manner, as well as in selenoproteins, previously separated by their molecular masses and isoelectric points using two-dimensional polyacrylamide gel electrophoresis (2-D PAGE). In this chapter, we present the protocols to perform LA-ICP-MS imaging experiments, allowing the distribution visualization and determination of selenium and/or selenoproteins in biological systems.

  19. Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives

    DEFF Research Database (Denmark)

    Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente

    2006-01-01

    Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material, t...... analysis of bromine-containing preservatives in commercially available cosmetic products.......Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material...... at an intermediate and at a high linear velocity. The precision was better than 2.2% R.S.D. and regression analysis showed that a linear response was achieved at both flow rates (R2 > 0.9993, n = 36). The analysis time was less than 4.5 min at a flow rate of 50 microL min(-1) and limits of detection...

  20. 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.

  1. Evaluation of pyrolysis curves for volatile elements in aqueous standards and carbon-containing matrices in electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, A.F. [Delft University of Technology, Faculty of Applied Sciences, DelftChemTech, Julianalaan 136, 2628 BL Delft (Netherlands); Universidade Federal de Santa Catarina, Departamento de Quimica, 88040-900 Florianopolis, SC (Brazil); Welz, B. [Universidade Federal de Santa Catarina, Departamento de Quimica, 88040-900 Florianopolis, SC (Brazil); Loos-Vollebregt, M.T.C. de [Delft University of Technology, Faculty of Applied Sciences, DelftChemTech, Julianalaan 136, 2628 BL Delft (Netherlands)], E-mail: m.t.c.deloos-vollebregt@tudelft.nl

    2008-07-15

    Pyrolysis curves in electrothermal atomic absorption spectrometry (ET AAS) and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) have been compared for As, Se and Pb in lobster hepatopancreas certified reference material using Pd/Mg as the modifier. The ET AAS pyrolysis curves confirm that the analytes are not lost from the graphite furnace up to a pyrolysis temperature of 800 deg. C. Nevertheless, a downward slope of the pyrolysis curve was observed for these elements in the biological material using ETV-ICP-MS. This could be related to a gain of sensitivity at low pyrolysis temperatures due to the matrix, which can act as carrier and/or promote changes in the plasma ionization equilibrium. Experiments with the addition of ascorbic acid to the aqueous standards confirmed that the higher intensities obtained in ETV-ICP-MS are related to the presence of organic compounds in the slurry. Pyrolysis curves for As, Se and Pb in coal and coal fly ash were also investigated using the same Pd/Mg modifier. Carbon intensities were measured in all samples using different pyrolysis temperatures. It was observed that pyrolysis curves for the three analytes in all slurry samples were similar to the corresponding graphs that show the carbon intensity for the same slurries for pyrolysis temperatures from 200 deg. C up to 1000 deg. C.

  2. 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.

  3. Quantification of trace amounts of rare earth elements in high purity gadolinium oxide by sector field inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Pedreira, W.R.; Silva Queiroz, C.A. da; Abrao, A.; Pimentel, M.M.

    2004-01-01

    In recent years, rare earth elements (REEs) have received much attention in the fields of geochemistry and industry. Gadolinium oxide is used for many different high technology applications such as infrared absorbing automotive glass, petroleum cracking catalyst, gadolinium-yttrium garnets, microwave applications, and color TV tube phosphors. It can also be used in optical glass manufacturing and in the electronic industry. Rapid and accurate determinations of the rare earth elements are increasingly required as industrial demands expand. In general, the inductively coupled plasma mass spectrometry (ICP-MS) presents some advantages for trace element analysis, due to high sensitivity and resolution, when compared with other analytical techniques. In this work, sector field inductively coupled plasma mass spectrometry was used. Sixteen elements (Sc, Y, and 14 lanthanides) were determined selectively with the ICP-MS system using a concentration gradient method. The detection limits with the ICP-MS system were about 0.2-8 pg ml -1 . The recovery percentage ranged from 95 to 100% for different rare earth elements. The %R.S.D. of the methods varying between 1.5 and 2.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two high pure gadolinium oxides samples (IPEN and JMC) was performed. IPEN's material is highly pure (>99.99%) and was successfully analyzed without spectral interference

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

    International Nuclear Information System (INIS)

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

    1995-01-01

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

  6. 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.

  7. 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...

  8. Rapid and sensitive determination of radiocesium (Cs-135, Cs-137) in the presence of excess barium by electrothermal vaporization-inductively coupled plasma-mass spectrometry (ETV-ICP-MS) with potassium thiocyanate as modifier

    International Nuclear Information System (INIS)

    Song, M.; Probst, T.U.; Berryman, N.G.

    2001-01-01

    An electrothermal vaporization-inductively coupled plasma-mass spectrometric (ETV-ICP-MS) method based on selective volatilization of cesium with KSCN as modifier has been developed for determination of radiocesium, i.e. 135 Cs and 137 Cs, in the presence of isobaric barium. A 10000 times excess of barium, which was volatilized at a temperature of 1100 C, resulted only in a 1% signal increase in the signal of mass 135 amu. The recommended concentration of KSCN is 0.3 mM, and pretreatment and volatilization temperatures are 400 C and 1100 C, respectively. A ramp time of 1 s is recommended for the volatilization step. The achieved limit of detection for 135 Cs is 0.2 pg/mL (10 μBq/mL) and 4 fg (0.2 μBq) absolute for a sample volume of 20 μL. This means a limit of detection for 137 Cs of 0.2 pg/mL (0.6 Bq/mL) and of 4 fg (0.01 Bq) absolute. Signal variations of 135 Cs and 137 Cs, respectively, in spiked samples with various matrices were investigated. (orig.)

  9. Tissue gadolinium deposition in hepatorenally impaired rats exposed to Gd-EOB-DTPA: evaluation with inductively coupled plasma mass spectrometry (ICP-MS).

    Science.gov (United States)

    Sato, Tomohiro; Tamada, Tsutomu; Watanabe, Shigeru; Nishimura, Hirotake; Kanki, Akihiko; Noda, Yasufumi; Higaki, Atsushi; Yamamoto, Akira; Ito, Katsuyoshi

    2015-06-01

    This study was undertaken to quantify tissue gadolinium (Gd) deposition in hepatorenally impaired rats exposed to gadolinium ethoxybenzyl diethylenetriamine pentaacetic acid (Gd-EOB-DTPA) by means of inductively coupled plasma mass spectrometry (ICP-MS) and to compare differences in Gd distribution among major organs as possible triggers for nephrogenic systemic fibrosis. Five hepatorenally impaired rats (5/6-nephrectomized, with carbon-tetrachloride-induced liver fibrosis) were injected with Gd-EOB-DTPA. Histological assessment was conducted and Gd content of the skin, liver, kidneys, lungs, heart, spleen, diaphragm, and femoral muscle was measured by inductively coupled plasma mass spectrometry (ICP-MS) at 7 days after last injection. In addition, five renally impaired rats were injected with Gd-EOB-DTPA and the degree of tissue Gd deposition was compared with that in the hepatorenally impaired rats. ICP-MS analysis revealed significantly higher Gd deposition in the kidneys, spleen, and liver (p = 0.009-0.047) in the hepatorenally impaired group (42.6 ± 20.1, 17.2 ± 6.1, 8.4 ± 3.2 μg/g, respectively) than in the renally impaired group (17.2 ± 7.7, 5.4 ± 2.1, 2.8 ± 0.7 μg/g, respectively); no significant difference was found for other organs. In the hepatorenally impaired group, Gd was predominantly deposited in the kidneys, followed by the spleen, liver, lungs, skin, heart, diaphragm, and femoral muscle. Histopathological investigation revealed hepatic fibrosis in the hepatorenally impaired group. Compared with renally impaired rats, tissue Gd deposition in hepatorenally impaired rats exposed to Gd-EOB-DTPA was significantly increased in the kidneys, spleen, and liver, probably due to the impairment of the dual excretion pathways of the urinary and biliary systems.

  10. A validated inductively coupled plasma mass spectrometry (ICP-MS) method for the quantification of total platinum content in plasma, plasma ultrafiltrate, urine and peritoneal fluid.

    Science.gov (United States)

    Lemoine, Lieselotte; Thijssen, Elsy; Noben, Jean-Paul; Adriaensens, Peter; Carleer, Robert; Speeten, Kurt Van der

    2018-04-15

    Oxaliplatin is a platinum (Pt) 1 containing antineoplastic agent that is applied in current clinical practice for the treatment of colon and appendiceal neoplasms. A fully validated, highly sensitive, high throughput inductively coupled plasma mass spectrometry (ICP-MS) method is provided to quantify the total Pt content in plasma, plasma ultrafiltrate, urine and peritoneal fluid. In this ICP-MS approach, the only step of sample preparation is a 1000-fold dilution in 0.5% nitric acid, allowing the analysis of 17 samples per hour. Detection of Pt was achieved over a linear range of 0.01-100 ng/mL. The limit of quantification was 18.0 ng/mL Pt in plasma, 8.0 ng/mL in ultrafiltrate and 6.1 ng/mL in urine and peritoneal fluid. The ICP-MS method was further validated for inter-and intraday precision and accuracy (≤15%), recovery, robustness and stability. Short-term storage of the biofluids, for 14 days, can be performed at -4 °C, -24 °C and -80 °C. As to long-term stability, up to 5 months, storage at -80 °C is encouraged. Furthermore, a timeline assessing the total and unbound Pt fraction in plasma and ultrafiltrate over a period of 45 h is provided. Following an incubation period of 5 h at 37 °C, 19-21% of Pt was recovered in the ultrafiltrate, emphasizing the extensive and rapid binding of oxaliplatin-derived Pt to plasma proteins. The described method can easily be implemented in a routine setting for pharmacokinetic studies in patients treated with oxaliplatin-based hyperthermic intraperitoneal perioperative chemotherapy. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Inductively coupled plasma source mass spectrometry

    International Nuclear Information System (INIS)

    Price Russ, G. III

    1993-01-01

    Inductively coupled plasma source mass spectrometry (ICP-MS) is a relatively new (5 y commercial availability) technique for simultaneously determining the concentration and isotopic composition of a large number of elements at trace levels. The principle advantages of ICP-MS are the ability to measure essentially all the metallic elements at concentrations as low as 1 part in 10 12 by weight, to analyse aqueous samples directly, to determine the isotopic composition of essentially all the metallic elements, and to analyse samples rapidly (minutes). The history of the development of ICP-MS and discussions of a variety of applications have been discussed in detail in Date and Gray (1988). Koppenaal (1988, 1990) has reviewed the ICP-MS literature. In that ICP-MS is a relatively new and still evolving technique, this chapter will discuss potential capability more than proven performance. (author). 24 refs

  12. 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)

  13. 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)

  14. Ion sampling and transport in Inductively Coupled Plasma Mass Spectrometry

    Science.gov (United States)

    Farnsworth, Paul B.; Spencer, Ross L.

    2017-08-01

    Quantitative accuracy and high sensitivity in inductively coupled plasma mass spectrometry (ICP-MS) depend on consistent and efficient extraction and transport of analyte ions from an inductively coupled plasma to a mass analyzer, where they are sorted and detected. In this review we examine the fundamental physical processes that control ion sampling and transport in ICP-MS and compare the results of theory and computerized models with experimental efforts to characterize the flow of ions through plasma mass spectrometers' vacuum interfaces. We trace the flow of ions from their generation in the plasma, into the sampling cone, through the supersonic expansion in the first vacuum stage, through the skimmer, and into the ion optics that deliver the ions to the mass analyzer. At each stage we consider idealized behavior and departures from ideal behavior that affect the performance of ICP-MS as an analytical tool.

  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. Inductively coupled plasma- mass spectrometry. Chapter 13

    International Nuclear Information System (INIS)

    Mahalingam, T.R.

    1997-01-01

    Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) is a new technique for elemental and isotopic analysis which is currently attracting a great deal of interest. This relatively new technique has found wide applications in different fields of research viz., nuclear, geological, biological and environmental sciences

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-07-04

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

  18. 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)

  19. Applications of inductively coupled plasma mass spectrometry and laser ablation inductively coupled plasma mass spectrometry in materials science

    International Nuclear Information System (INIS)

    Becker, Johanna Sabine

    2002-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) have been applied as the most important inorganic mass spectrometric techniques having multielemental capability for the characterization of solid samples in materials science. ICP-MS is used for the sensitive determination of trace and ultratrace elements in digested solutions of solid samples or of process chemicals (ultrapure water, acids and organic solutions) for the semiconductor industry with detection limits down to sub-picogram per liter levels. Whereas ICP-MS on solid samples (e.g. high-purity ceramics) sometimes requires time-consuming sample preparation for its application in materials science, and the risk of contamination is a serious drawback, a fast, direct determination of trace elements in solid materials without any sample preparation by LA-ICP-MS is possible. The detection limits for the direct analysis of solid samples by LA-ICP-MS have been determined for many elements down to the nanogram per gram range. A deterioration of detection limits was observed for elements where interferences with polyatomic ions occur. The inherent interference problem can often be solved by applying a double-focusing sector field mass spectrometer at higher mass resolution or by collision-induced reactions of polyatomic ions with a collision gas using an ICP-MS fitted with collision cell. The main problem of LA-ICP-MS is quantification if no suitable standard reference materials with a similar matrix composition are available. The calibration problem in LA-ICP-MS can be solved using on-line solution-based calibration, and different procedures, such as external calibration and standard addition, have been discussed with respect to their application in materials science. The application of isotope dilution in solution-based calibration for trace metal determination in small amounts of noble metals has been developed as a new calibration strategy. This review discusses new

  20. 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

  1. 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...

  2. UV and IR laser ablation for inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Smith, M.R.; Koppenaal, D.W.; Farmer, O.T.

    1993-06-01

    Laser ablation particle plume compositions are characterized using inductively coupled plasma mass spectrometry (ICP/MS). This study evaluates the mass response characteristics peculiar to ICP/MS detection as a function of laser fluence and frequency. Evaluation of the ICP/MS mass response allows deductions to be made concerning how representative the laser ablation produced particle plume composition is relative to the targeted sample. Using a black glass standard, elemental fractionation was observed, primarily for alkalis and other volatile elements. The extent of elemental fractionation between the target sample and the sampled plume varied significantly as a function of laser fluences and IR and UV laser frequency

  3. Spectrochemical pure cerium dioxide preparation and its quality control by inductively coupled plasma and mass spectrometry (ICP/MS)

    International Nuclear Information System (INIS)

    Da Silva Queiroz, C.A.; De Souza, J.E.; Abrao, A.

    1998-01-01

    Full text: A simple and economic procedure for the purification until 500 g CeO 2 batch is presented. The purified material will be used as spectrochemical standard. It is obtained by association of the fractional precipitation technique in the system REC 3 /H 2 O 2 /NH 4 OH to enrich the cerium up to 90% and then refined by ion exchange up to 99.9% CeO2. The 99,9% CeO 2 warranty control of purity was accomplished by inductively coupled plasma and mass spectrometry (ICP/ MS) and compared with activation analysis data, exhibiting impurities traces of same values of the international spec pure standard. The following results (average values) for the contaminant rare earths are (ppm):La(36), Pr(19), Nd(161), Sm(11), Eu(5,3),Gd(113),Tb(89),Dy(2),Ho(0.05),Er(1), Tm(0), Yb(11), Lu (19) and Y(2.1), respectively

  4. 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)

  5. 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....

  6. Measurement of inclusion size by laser ablation ICP mass spectrometry

    International Nuclear Information System (INIS)

    Karasev, Andrey V.; Suito, Hideaki

    2004-01-01

    By using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), the measurement of particle size has been made for one component oxide (Al 2 O 3 and MgO) and multicomponent oxide (12CaO·7Al 2 O 3 and CaO-Al 2 O 3 -MgO) located on surface of iron or glass sample. The method of particle size estimation by LA-ICP-MS has been developed coupled with a new method of making samples with particles. The size calibration lines for Al 2 O 3 , MgO and CaO particles have been obtained. The results of particle size measurement by LA-ICP-MS are compared with those by SEM and single-particle optical sensing (SPOS) methods. It was confirmed that LA-ICP-MS has the perspective to be used for the quick measurement of inclusion composition and size in metal and other materials. The size frequency distributions of Al 2 O 3 particles measured by LA-ICP-MS in iron samples with particles agree reasonably well with those by SEM and SPOS in the range of particle diameter from 2 to 20 μm. The size of Al 2 O 3 , MgO and complex oxide (12CaO·7Al 2 O 3 and CaO-Al 2 O 3 -MgO) particles measured by LA-ICP-MS is in good agreement with that by SEM in the range of particle diameter from 10 to 40 μm. (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. Tissue gadolinium deposition in renally impaired rats exposed to different gadolinium-based MRI contrast agents: evaluation with inductively coupled plasma mass spectrometry (ICP-MS).

    Science.gov (United States)

    Sato, Tomohiro; Ito, Katsuyoshi; Tamada, Tsutomu; Kanki, Akihiko; Watanabe, Shigeru; Nishimura, Hirotake; Tanimoto, Daigo; Higashi, Hiroki; Yamamoto, Akira

    2013-10-01

    To quantify tissue gadolinium (Gd) deposition in renally impaired rats exposed to Gd-EOB-DTPA and other Gd-based MRI contrast agents by means of inductively coupled plasma mass spectrometry (ICP-MS), and to compare the differences in distribution among major organs as possible triggers for nephrogenic systemic fibrosis (NSF). A total of 15 renally impaired rats were injected with Gd-EOB-DTPA, Gd-DTPA-BMA and Gd-HP-DO3A. Gd contents of skin, liver, kidney, lung, heart, spleen, diaphragm and femoral muscle were measured by inductively coupled plasma mass spectrometry (ICP-MS). Histological assessment was also conducted. Tissue Gd deposition in all organs was significantly higher (P=0.005~0.009) in the Gd-DTPA-BMA group than in the Gd-HP-DO3A and Gd-EOB-DTPA groups. In the Gd-DTPA-BMA group, Gd was predominantly deposited in kidney (1306±605.7μg/g), followed by skin, liver, lung, spleen, femoral muscle, diaphragm and heart. Comparing Gd-HP-DO3A and Gd-EOB-DTPA groups, Gd depositions in the kidney, liver and lung were significantly lower (P=0.009~0.011) in the Gd-EOB-DTPA group than in the Gd-HP-DO3A group although no significant differences were seen for any other organs. Gd-EOB-DTPA is a stable and safe Gd-based contrast agent (GBCA) showing lower Gd deposition in major organs in renally impaired rats, compared with other GBCAs. This fact suggests that the risk of NSF onset would be low in the use of Gd-EOB-DTPA. Copyright © 2013 Elsevier Inc. All rights reserved.

  9. Optimization of a single-drop microextraction method for multielemental determination by electrothermal vaporization inductively coupled plasma mass spectrometry following in situ vapor generation

    International Nuclear Information System (INIS)

    Gil, Sandra; Loos-Vollebregt, Margaretha T.C. de; Bendicho, Carlos

    2009-01-01

    A headspace single-drop microextraction (HS-SDME) method has been developed in combination with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) for the simultaneous determination of As, Sb, Bi, Pb, Sn and Hg in aqueous solutions. Vapor generation is carried out in a 40 mL volume closed-vial containing a solution with the target analytes in hydrochloric acid and potassium ferricyanide medium. Hydrides (As, Sb, Bi, Pb, Sn) and Hg vapor are trapped onto an aqueous single drop (3 μL volume) containing Pd(II), followed by the subsequent injection in the ETV. Experimental variables such as medium composition, sodium tetrahydroborate (III) volume and concentration, stirring rate, extraction time, sample volume, ascorbic acid concentration and palladium amount in the drop were fully optimized. The limits of detection (LOD) (3σ criterion) of the proposed method for As, Sb, Bi, Pb, Sn and Hg were 0.2, 0.04, 0.01, 0.07, 0.09 and 0.8 μg/L, respectively. Enrichment factors of 9, 85, 138, 130, 37 and 72 for As, Sb, Bi, Pb, Sn and Hg, respectively, were achieved in 210 s. The relative standard deviations (N = 5) ranged from 4 to 8%. The proposed HS-SDME-ETV-ICP-MS method has been applied for the determination of As, Sb, Bi, Pb, Sn and Hg in NWRI TM-28.3 certified reference material.

  10. Application of high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS) for determination of chromium compounds in the air at the workplace.

    Science.gov (United States)

    Stanislawska, Magdalena; Janasik, Beata; Wasowicz, Wojciech

    2013-12-15

    The toxicity and bioavailability of chromium species are highly dependable on the form or species, therefore determination of total chromium is insufficient for a complete toxicological evaluation and risk assessment. An analytical method for determination of soluble and insoluble Cr (III) and Cr (VI) compounds in welding fume at workplace air has been developed. The total chromium (Cr) was determined by using quadruple inductively coupled plasma mass spectrometry (ICP-MS) equipped with a dynamic reaction cell (DRC(®)). Soluble trivalent and hexavalent chromium compounds were determined by high performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC-ICP-MS). A high-speed, reversed-phase CR C8 column (PerkinElmer, Inc., Shelton, CT, USA) was used for the speciation of soluble Cr (III) and soluble Cr (VI). The separation was accomplished by interaction of the chromium species with the different components of the mobile phase. Cr (III) formed a complex with EDTA, i.e. retained on the column, while Cr (VI) existed in the solutions as dichromate. Alkaline extraction (2% KOH and 3% Na2CO3) and anion exchange column (PRP-X100, PEEK, Hamilton) were used for the separation of the total Cr (VI). The results of the determination of Cr (VI) were confirmed by the analysis of the certified reference material BCR CRM 545 (Cr (VI) in welding dust). The results obtained for the certified material (40.2±0.6 g kg(-1)) and the values recorded in the examined samples (40.7±0.6 g kg(-1)) were highly consistent. This analytical method was applied for the determination of chromium in the samples in the workplace air collected onto glass (Whatman, Ø 37 mm) and membrane filters (Sartorius, 0.8 μm, Ø 37 mm). High performance liquid chromatography with inductively coupled plasma mass spectrometry is a remarkably powerful and versatile technique for determination of chromium species in welding fume at workplace air. Crown Copyright © 2013 Published by

  11. Ultra-trace determination of Strontium-90 in environmental soil samples from Qatar by collision/reaction cell-inductively coupled plasma mass spectrometry (CRC-ICP-MS/MS)

    Energy Technology Data Exchange (ETDEWEB)

    Al-Meer, S. H.; Amr, M. A. [Central Laboratories Unit, Qatar University, Doha (Qatar); Helal, A.I. [Atomic Energy Authority, Cairo (Egypt); Al-Kinani, A.T. [Minstery of Environment, Doha (Qatar)

    2013-07-01

    Because of the very low level of {sup 90}Sr in the environmental soil samples and its determination by beta counting may take several weeks, we developed a procedure for ultra-trace determination of {sup 90}Sr using collision reaction cell-inductively coupled plasma tandem mass spectrometry (CRC-ICP-MS/MS, Agilent 8800). Soil samples were dried at 105 deg. C and then heated in a furnace at 550 deg. C to remove any organics present. 500 g of each soil samples were aliquoted into 2000 ml glass beakers. Each Soils samples were soaked in 2 ppm Sr solution carrier to allow determination of chemical yield. The solid to liquid ratio was 1:1. Finally the soil samples were dried at 105 deg. C. Five hundred milliliters concentrated nitric acid and 250 ml hydrochloric acid volumes were added on 500 g soil samples. The samples were digested on hot plate at 80 deg. C to prevent spraying with continuous manual mixing. The leachate solution was separated. The solids were rinsed with 500 ml deionized water, warmed on a hot plate and the leachate plus previous leachate were filtered and the total volume was reduced to 500 ml by evaporation. Final leachate volume was transferred to a centrifuge tubes. The centrifuge tubes were centrifuged at 3,500 rpm for 10 min. The leachate was transferred to a 1 L beaker and heated on a hot plate to evaporate the leachate to dryness. The reside was re-dissolved in 100 ml of 2% HNO{sub 3} and reduced by evaporation to 10 mL. The solution was measured directly by CRC-ICP-MS/MS by setting the first quadruple analyzer to m/z 90 and introducing oxygen gas into the reaction cell for elimination isobar interference from zirconium-90. The method was validated by measurements of standard reference materials and applied on environmental soil samples. The overall time requirement for the measurement of strontium-90 by CRC-ICP-MS/MS is 2 days, significantly shorter than any radioanalytical protocol currently available. (authors)

  12. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2009-07-01

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

  14. Ion-pair chromatography coupled to inductively coupled plasma-mass spectrometry (IPC-ICP-MS) as a method for thiomolybdate speciation in natural waters.

    Science.gov (United States)

    Lohmayer, Regina; Reithmaier, Gloria Maria Susanne; Bura-Nakić, Elvira; Planer-Friedrich, Britta

    2015-03-17

    Molybdenum precipitates preferentially under reducing conditions; therefore, its occurrence in sediment records is used as an indicator of paleoredox conditions. Although thiomolybdates (MoO4-xSx(2-) with x = 1-4) supposedly are necessary intermediates in the process of molybdenum precipitation under anoxic conditions, there is no information about their abundance in natural environments, because of a lack of element-specific methods with sufficiently low detection limits. Here, we optimized ion-pair chromatographic separation for coupling to an inductively coupled plasma-mass spectrometry detector (IPC-ICP-MS). 2-Propanol (10%-25% gradient) replaced the previously used acetonitrile (25%-75%) as the solvent, to reduce the carbon load into the plasma. In synthetic solutions, formation of thiomolybdates was found to occur spontaneously in the presence of excess sulfide and the degree of thiolation was highest at pH 7. Excess hydroxyl led to a transformation of thiomolybdates to molybdate. Under acidic to neutral conditions, precipitation of molybdenum and hydrolysis of tetrathiomolybdate were observed. Flash-freezing was found to be suitable to stabilize tetrathiomolybdate, with 2 mM) negatively affected the detection of molybdate, which eluted mainly in the dead volume, but had no negative effect on higher thiolated molybdates. Detection limits were ∼10 nM. With the newly developed IPC-ICP-MS method, thiomolybdates were found to form spontaneously in euxinic marine waters after adding a molybdate spike and occur naturally in sulfidic geothermal waters.

  15. The use of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of toxic and essential elements in different types of food samples

    Science.gov (United States)

    Voica, C.; Dehelean, A.; Kovacs, M. H.

    2012-02-01

    Food is the primary source of essential elements for humans and it is an important source of exposure to toxic elements. In this context, levels of essential and toxic elements must be determined routinely in consumed food products. The content of trace elements (As, Pb, Cu, Cd, Zn, Sn, Hg) in different types of food samples (e.g. rice, bread, sugar, cheese, milk, butter, wheat, coffee, chocolate, biscuits pasta, etc.) was determined, using inductively coupled plasma mass spectrometry (ICP-MS). Trace element contents in some foods were higher than maximum permissible levels of toxic metals in human food (Cd in bread, Zn in cheese, Cu in coffee, Hg in carrots and peppers).

  16. 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

  17. Chemical speciation analysis for bromine in tap water by ion chromatography/inductively coupled plasma-mass spectrometry and electrospray ionization-mass spectrometry

    International Nuclear Information System (INIS)

    Kurata, Keigo; Suzuki, Yoshinari; Furuta, Naoki

    2010-01-01

    Bromide compounds in tap water were measured by using a hyphenated technique of ion chromatography coupled with inductively coupled plasma - mass spectrometry (IC/ICP-MS) and electrospray ionization mass spectrometry (ESI-MS). We identified bromide ion (Br - ), bromate ion (BrO 3 - ), bromochloroacetic acid (BCAA), dibromoacetic acid (DBAA) and bromodichloroacetic acid (BDCAA) by standard addition methods with IC/ICP-MS. Moreover, we identified BCAA and BDCAA by ESI-MS after separation with IC. Br - , BrO 3 - , BCAA, DBAA and BDCAA in tap water collected from around Tokyo area were quantified by IC/ICP-MS. The maximum concentration of BrO 3 - (1.8 ng mL -1 ) was observed in tap water collected from Bunkyo-ku, although this concentration was lower than 10 ng mL -1 , which is the regulated concentration in Japan. DBAA, which is regulated by United States Environmental Protection Agency, was detected in tap water collected from all sites, except for Ome. However, since BrO 3 - and DBAA are toxic, it is necessary to continue monitoring bromide compounds in tap water. (author)

  18. Mass spectrometry of long-lived radionuclides

    International Nuclear Information System (INIS)

    Becker, Johanna Sabine.

    2003-01-01

    The capability of determining element concentrations at the trace and ultratrace level and isotope ratios is a main feature of inorganic mass spectrometry. The precise and accurate determination of isotope ratios of long-lived natural and artificial radionuclides is required, e.g. for their environmental monitoring and health control, for studying radionuclide migration, for age dating, for determining isotope ratios of radiogenic elements in the nuclear industry, for quality assurance and determination of the burn-up of fuel material in a nuclear power plant, for reprocessing plants, nuclear material accounting and radioactive waste control. Inorganic mass spectrometry, especially inductively coupled plasma mass spectrometry (ICP-MS) as the most important inorganic mass spectrometric technique today, possesses excellent sensitivity, precision and good accuracy for isotope ratio measurements and practically no restriction with respect to the ionization potential of the element investigated--therefore, thermal ionization mass spectrometry (TIMS), which has been used as the dominant analytical technique for precise isotope ratio measurements of long-lived radionuclides for many decades, is being replaced increasingly by ICP-MS. In the last few years instrumental progress in improving figures of merit for the determination of isotope ratio measurements of long-lived radionuclides in ICP-MS has been achieved by the application of a multiple ion collector device (MC-ICP-MS) and the introduction of the collision cell interface in order to dissociate disturbing argon-based molecular ions, to reduce the kinetic energy of ions and neutralize the disturbing noble gas ions (e.g. of 129 Xe + for the determination of 129 I). The review describes the state of the art and the progress of different inorganic mass spectrometric techniques such as ICP-MS, laser ablation ICP-MS vs. TIMS, glow discharge mass spectrometry, secondary ion mass spectrometry, resonance ionization mass

  19. Quantification of low molecular weight selenium metabolites in human plasma after treatment with selenite in pharmacological doses by LC-ICP-MS

    DEFF Research Database (Denmark)

    Flouda, Konstantina; Dersch, Julie Maria; Gabel-Jensen, Charlotte

    2016-01-01

    The paper presents an analytical method for quantification of low molecular weight (LMW) selenium compounds in human plasma based on liquid chromatography inductively coupled plasma mass spectrometry (LC-ICP-MS) and post column isotope dilution-based quantification. Prior to analysis, samples were...

  20. 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.

  1. Considerations of particle vaporization and analyte diffusion in single-particle inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Ho, Koon-Sing; Lui, Kwok-On; Lee, Kin-Ho; Chan, Wing-Tat

    2013-01-01

    The intensity of individual gold nanoparticles with nominal diameters of 80, 100, 150, and 200 nm was measured using single-particle inductively coupled plasma-mass spectrometry (ICP-MS). Since the particles are not perfectly monodisperse, a distribution of ICP-MS intensity was obtained for each nominal diameter. The distribution of particle mass was determined from the transmission electron microscopy (TEM) image of the particles. The distribution of ICP-MS intensity and the distribution of particle mass for each nominal diameter were correlated to give a calibration curve. The calibration curves are linear, but the slope decreases as the nominal diameter increases. The reduced slope is probably due to a smaller degree of vaporization of the large particles. In addition to the degree of particle vaporization, the rate of analyte diffusion in the ICP is an important factor that determines the measured ICP-MS intensity. Simulated ICP-MS intensity versus particle size was calculated using a simple computer program that accounts for the vaporization rate of the gold nanoparticles and the diffusion rate and degree of ionization of the gold atoms. The curvature of the simulated calibration curves changes with sampling depth because the effects of particle vaporization and analyte diffusion on the ICP-MS intensity are dependent on the residence time of the particle in the ICP. Calibration curves of four hypothetical particles representing the four combinations of high and low boiling points (2000 and 4000 K) and high and low analyte diffusion rates (atomic masses of 10 and 200 Da) were calculated to further illustrate the relative effects of particle vaporization and analyte diffusion. The simulated calibration curves show that the sensitivity of single-particle ICP-MS is smaller than that of the ICP-MS measurement of continuous flow of standard solutions by a factor of 2 or more. Calibration using continuous flow of standard solution is semi-quantitative at best. An

  2. The application of inductively coupled plasma mass spectrometry to the study of environmental radioactivity

    International Nuclear Information System (INIS)

    Igarashi, Yasuhito; Shiraishi, Kunio; Takaku, Yuichi.

    1991-01-01

    This paper discusses how far inductively coupled plasma mass spectrometry (ICP-MS) is applied in the field of environmental radioactivity. An outline of the apparatus for ICP-MS is given. Interferences associated with ICP-MS are explained in terms of spectrum interference, blocking phenomenon for sampling cone and other elements, and matrix effects. Detection efficiency of ICP-MS is discussed in view of sample induction efficiency, ionization efficiency, sampling efficiency or ion permeability efficiency, and double-focus ICP-MS. Finally, some problems of ICP-MS in measuring long-lived radionuclides are presented, which may be associated with extremely small ratio of radionuclides, measurement accuracy of radionuclide ratio, and extremely small almounts of radionuclides. A great contribution of ICP-MS to the study of environmental radioactivity is stressed. (N.K.) 112 refs

  3. Studies of selenium and xenon in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Bricker, T.

    1994-01-01

    Since its development, inductively coupled plasma mass spectrometry (ICP-MS) has been a widely used analytical technique. ICP-MS offers low detection limits, easy determination of isotope ratios, and simple mass spectra from analyte elements. ICP-MS has been successfully employed for many applications including geological, environmental, biological, metallurgical, food, medical, and industrial. One specific application important to many areas of study involves elemental speciation by using ICP-MS as an element specific detector interfaced to liquid chromatography. Elemental speciation information is important and cannot be obtained by atomic spectrometric methods alone which measure only the total concentration of the element present. Part 1 of this study describes the speciation of selenium in human serum by size exclusion chromatography (SEC) and detection by ICP-MS. Although ICP-MS has been widely sued, room for improvement still exists. Difficulties in ICP-MS include noise in the background, matrix effects, clogging of the sampling orifice with deposited solids, and spectral interference caused by polyatomic ions. Previous work has shown that the addition of xenon into the central channel of the ICP decreases polyatomic ion levels. In Part 2 of this work, a fundamental study involving the measurement of the excitation temperature is carried out to further understand xenon's role in the reduction of polyatomic ions. 155 refs

  4. Elemental labelling combined with liquid chromatography inductively coupled plasma mass spectrometry for quantification of biomolecules: A review

    International Nuclear Information System (INIS)

    Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

    2012-01-01

    Highlights: ► Survey of bio-analytical approaches utilizing biomolecule labelling. ► Detailed discussion of methodology and chemistry of elemental labelling. ► Biomedical and bio-analytical applications of elemental labelling. ► FI-ICP-MS and LC–ICP-MS for quantification of elemental labelled biomolecules. ► Review of selected applications. - Abstract: This article reviews novel quantification concepts where elemental labelling is combined with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) or liquid chromatography inductively coupled plasma mass spectrometry (LC–ICP-MS), and employed for quantification of biomolecules such as proteins, peptides and related molecules in challenging sample matrices. In the first sections an overview on general aspects of biomolecule quantification, as well as of labelling will be presented emphasizing the potential, which lies in such methodological approaches. In this context, ICP-MS as detector provides high sensitivity, selectivity and robustness in biological samples and offers the capability for multiplexing and isotope dilution mass spectrometry (IDMS). Fundamental methodology of elemental labelling will be highlighted and analytical, as well as biomedical applications will be presented. A special focus will lie on established applications underlining benefits and bottlenecks of such approaches for the implementation in real life analysis. Key research made in this field will be summarized and a perspective for future developments including sophisticated and innovative applications will given.

  5. Slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for steelmaking flue dust analysis

    Science.gov (United States)

    Coedo, A. G.; Dorado, T.; Padilla, I.; Maibusch, R.; Kuss, H.-M.

    2000-02-01

    A commercial atomic absorption graphite furnace (AAGF), with a self-made adapter and valve system, was used as a slurry sampling cell for electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). The system was applied to the determination of As, Sn, Sb, Se, Te, Bi, Cd, V, Ti and Mo in steelmaking flue dusts. Experimental conditions with respect to ETV and ICP-MS operating parameters were optimized. Compared to aqueous solutions, slurry samples were found to present better analyte transport. Microgram amounts of Rh were used to reduce the difference in analyte response in sensitivity for aqueous solutions of the tested analytes. No such increasing effect was observed for slurry samples and aqueous standards. An added quantity of Rh acting as modifier/carrier resulted in an increase for the same analytes in matrix-slurry solutions, even the addition of an extra Rh quantity has resulted in a decrease in the signals. The effect of Triton X-100 (used as a dispersant agent) on analyte intensity and precision was also studied. External calibration from aqueous standards spiked with 100 μg ml -1 Rh was performed to quantified 0.010 g/100 ml slurry samples. Results are presented for a certified reference electrical arc furnace flue dust (EAF): CRM-876-1 (Bureau of Analysis Samples Ltd., Cleveland, UK), a reference sample of coke ashes X-3705 (from AG der Dillinger Hüttenwerke, Germany), and a representative sample of EAF flue dust from a Spanish steelmaking company (CENIM-1). For the two reference materials an acceptable agreement with certificate values was achieved, and the results for the CENIM sample matched with those obtained from conventional nebulization solution.

  6. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    Energy Technology Data Exchange (ETDEWEB)

    Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J.M.; García Alonso, J.I., E-mail: jiga@uniovi.es

    2015-06-01

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC–ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review. - Highlights: • Emphasis placed on the sulfur-specific detection by chromatographic techniques coupled on-line to ICP-MS. • Different instrumental approaches available for sulfur measurements by ICP-MS. • Quantification of proteins and the analysis of metalloproteins via sulfur by LC-ICP-MS. • Labelling procedures for metabolic applications are also included. • The measurement of natural variations in S isotope composition with multicollector ICP-MS.

  7. Elemental labelling combined with liquid chromatography inductively coupled plasma mass spectrometry for quantification of biomolecules: A review

    Science.gov (United States)

    Kretschy, Daniela; Koellensperger, Gunda; Hann, Stephan

    2012-01-01

    This article reviews novel quantification concepts where elemental labelling is combined with flow injection inductively coupled plasma mass spectrometry (FI-ICP-MS) or liquid chromatography inductively coupled plasma mass spectrometry (LC–ICP-MS), and employed for quantification of biomolecules such as proteins, peptides and related molecules in challenging sample matrices. In the first sections an overview on general aspects of biomolecule quantification, as well as of labelling will be presented emphasizing the potential, which lies in such methodological approaches. In this context, ICP-MS as detector provides high sensitivity, selectivity and robustness in biological samples and offers the capability for multiplexing and isotope dilution mass spectrometry (IDMS). Fundamental methodology of elemental labelling will be highlighted and analytical, as well as biomedical applications will be presented. A special focus will lie on established applications underlining benefits and bottlenecks of such approaches for the implementation in real life analysis. Key research made in this field will be summarized and a perspective for future developments including sophisticated and innovative applications will given. PMID:23062431

  8. A radiotracer study on the volatilization and transport effects of thermochemical reagents used in the analysis of alumina powders by slurry electrothermal vaporization inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Peschel, Birgit U.; Herdering, Wilhelm; Broekaert, Jose A.C.

    2007-01-01

    A neutron-activated Al 2 O 3 powder SRM 699 (NIST) containing the γ-radiation emitting radionuclides 51 Cr, 59 Fe, 60 Co and 65 Zn has been used to study the influence of thermochemical reagents on the volatilization and transport efficiency for these trace elements in electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) of Al 2 O 3 powders. From the signals in the γ-spectra for the radiotracers it has been found that less than 2% of the elements Cr, Fe, Co and Zn is left back in a graphite furnace from Al 2 O 3 powders at 2200 deg. C even without addition of a thermochemical reagent and the latter even was found to decrease the volatilization efficiencies. The recovery for the radiotracers on filters at the end of the transport tube as measured from the signals in the γ-spectra, however, was found to increase in most cases (i.e. from about 10% to more than 20%) when Pd(NO 3 ) 2 , Pd(NO 3 ) 2 + Mg(NO 3 ) 2 , PdCl 2 , IrCl 3 , SnCl 2 , AgCl, NaF, NH 4 Cl and NH 4 F were added at amounts generally used in electrothermal vaporization inductively coupled plasma mass spectrometry. However, when adding higher amounts as stoichiometrically required for a complete halogenation of the sample matrix in the case of AgCl, C 8 F 15 O 2 Na, IrCl 3 or PdCl 2 the transport efficiencies considerably decrease again. As shown in the case of NH 4 Cl the amount of thermochemical reagent used has to be optimized so as to obtain maximum analyte transport efficiencies. A comparison of the influence of NH 4 Cl on the transport efficiencies with its influence on the ETV-ICP-MS signals for Fe demonstrates the importance of transport efficiency changes for the effects of thermochemical reagents in electrothermal vaporization inductively coupled plasma mass spectrometry

  9. 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

  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

    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

  11. 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

  12. Application of inductively coupled plasma mass spectrometry (ICP/MS) to detection of trace elements, heavy metals and radioisotopes in scalp hair

    International Nuclear Information System (INIS)

    Ozturk, Yildirim; Benderli, Cihan

    2010-01-01

    Trace element analysis of human hair has the potential to reveal retrospective information about an individual's nutritional status and exposure. As trace elements are incorporated into the hair during the growth process, longitudinal segments of the hair may reflect the body burden during the growth period. it was evaluated the potential of human hair to indicate exposure or nutritional status over time by analysing trace element profiles in single strands of human hair. By using inductively coupled plasma mass spectrometry (ICP-MS), it was achieved profiles of 43 elements in single strands of human hair. It was shown that trace element analysis along single strands of human hair can yield information about essential and toxic elements and for some elements, can be correlated with seasonal changes in diet and exposure. The information obtained from the trace element profiles of human hair in this study substantiates the potential of hair as a biomarker

  13. 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.

  14. Slurry sampling flow injection chemical vapor generation inductively coupled plasma mass spectrometry for the determination of trace Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Wei-Ni [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Jiang, Shiuh-Jen, E-mail: sjjiang@faculty.nsysu.edu.tw [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Department of Medical Laboratory Science and Biotechnology, Kaohsiung Medical University, Kaohsiung 80708, Taiwan (China); Chen, Yen-Ling [Department of Fragrance and Cosmetic Science, Kaohsiung Medical University, Kaohsiung 80708, Taiwan (China); Sahayam, A.C. [National Centre for Compositional Characterisation of Materials (CCCM), Hyderabad (India)

    2015-02-20

    Highlights: • Determination of Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions in a single run. • Accurate analysis using isotope dilution and standard addition methods. • Vapor generation ICP-MS yielded superior detection limits compared to ETV-ICP-MS. • No sample dissolution increased sample through put. • Analysis of GBW09305 Cosmetic (Cream) reference material for accuracy. - Abstract: A slurry sampling inductively coupled plasma mass spectrometry (ICP-MS) method has been developed for the determination of Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions using flow injection (FI) vapor generation (VG) as the sample introduction system. A slurry containing 2% m/v lotion, 2% m/v thiourea, 0.05% m/v L-cysteine, 0.5 μg mL{sup −1} Co(II), 0.1% m/v Triton X-100 and 1.2% v/v HCl was injected into a VG-ICP-MS system for the determination of Ge, As, Cd, Sb, Hg and Bi without dissolution and mineralization. Because the sensitivities of the analytes in the slurry and that of aqueous solution were quite different, an isotope dilution method and a standard addition method were used for the determination. This method has been validated by the determination of Ge, As, Cd, Sb, Hg and Bi in GBW09305 Cosmetic (Cream) reference material. The method was also applied for the determination of Ge, As, Cd, Sb, Hg and Bi in three cosmetic lotion samples obtained locally. The analysis results of the reference material agreed with the certified value and/or ETV-ICP-MS results. The detection limit estimated from the standard addition curve was 0.025, 0.1, 0.2, 0.1, 0.15, and 0.03 ng g{sup −1} for Ge, As, Cd, Sb, Hg and Bi, respectively, in original cosmetic lotion sample.

  15. Slurry sampling flow injection chemical vapor generation inductively coupled plasma mass spectrometry for the determination of trace Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions

    International Nuclear Information System (INIS)

    Chen, Wei-Ni; Jiang, Shiuh-Jen; Chen, Yen-Ling; Sahayam, A.C.

    2015-01-01

    Highlights: • Determination of Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions in a single run. • Accurate analysis using isotope dilution and standard addition methods. • Vapor generation ICP-MS yielded superior detection limits compared to ETV-ICP-MS. • No sample dissolution increased sample through put. • Analysis of GBW09305 Cosmetic (Cream) reference material for accuracy. - Abstract: A slurry sampling inductively coupled plasma mass spectrometry (ICP-MS) method has been developed for the determination of Ge, As, Cd, Sb, Hg and Bi in cosmetic lotions using flow injection (FI) vapor generation (VG) as the sample introduction system. A slurry containing 2% m/v lotion, 2% m/v thiourea, 0.05% m/v L-cysteine, 0.5 μg mL −1 Co(II), 0.1% m/v Triton X-100 and 1.2% v/v HCl was injected into a VG-ICP-MS system for the determination of Ge, As, Cd, Sb, Hg and Bi without dissolution and mineralization. Because the sensitivities of the analytes in the slurry and that of aqueous solution were quite different, an isotope dilution method and a standard addition method were used for the determination. This method has been validated by the determination of Ge, As, Cd, Sb, Hg and Bi in GBW09305 Cosmetic (Cream) reference material. The method was also applied for the determination of Ge, As, Cd, Sb, Hg and Bi in three cosmetic lotion samples obtained locally. The analysis results of the reference material agreed with the certified value and/or ETV-ICP-MS results. The detection limit estimated from the standard addition curve was 0.025, 0.1, 0.2, 0.1, 0.15, and 0.03 ng g −1 for Ge, As, Cd, Sb, Hg and Bi, respectively, in original cosmetic lotion sample

  16. Trace metal analysis of road dust by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Powell, M.J.; Liu, L.; Gnanalingham, N.; Peters, L.

    2000-01-01

    Dust from roads in an air impingement zone close to anthropogenic sources of air pollutants can be a concern for people living in the immediate vicinity. The Ministry of the Environment (MOE) has conducted a case study to monitor the concentration of uranium, strontium, thorium and arsenic in road dust from one such area. A method for the analysis of road dust by inductively coupled plasma mass spectrometry (ICP-MS) has been developed with detection limits in the ng/1 range. A digestion technique has been developed by conducting experiments using single and combinations of acids in open-vessel wet digestions. Accuracy has been determined by the use of matrix representative certified reference materials (CRMs). Digestion precision was determined by elemental concentration measurements of the most representative CRM through replicates. Spike recovery data were from 95% to 110% for all elements, and inter-method comparison studies between hydride generation atomic absorption spectrometry (AAS) inductively coupled plasma atomic emission spectrometry (ICP-AES) and ICP-MS for arsenic and strontium show good agreement. (author)

  17. Recent Developments in Trace, Ultratrace and Isotope Ratio Measurements in Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Zahran, N. F.

    2004-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) and Laser Ablation (LA-ICP-MS) are recent techniques for trace, ultratrace and isotope ratio measurements. Main features of these techniques and their figure of merit and capabilities are discussed. An overview of ICP-MS instrument is presented in addition to its precision, accuracy and detection limits. Uses of ICP-MS in environmental monitoring in some cases for detection of some radio nuclides are presented. Two geological applications namely, zircon grains analysis and age dating of Rb-Sr method are presented. Zn elemental and isotopic analyses in blood and serum as a biological application is shown. (Author)

  18. Matrix digestion of soil and sediment samples for extraction of lead, cadmium and antimony and their direct determination by inductively coupled plasma-mass spectrometry and atomic emission spectrometry

    International Nuclear Information System (INIS)

    Chattopadhyay, P.; Fisher, A.S.; Henon, D.N.; Hill, S.J.

    2004-01-01

    An environmentally friendly and simple method has been developed for complete digestion of lead, cadmium and antimony from soil samples using a magnesium nitrate assisted dry ashing procedure. Statistical data for a series of experiments with standard reference materials are presented, and precision values are found to be comparable for inductively coupled plasma-mass spectrometry and for inductively coupled plasma-atomic emission spectrometry. From a single digest solution all analytes are quantified without involving any preconcentration routes. Inter-method comparison of inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) shows that the probability of the results being different is less than 99 %. (author)

  19. 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)

  20. 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).

  1. Applications of inductively coupled plasma-mass spectrometry to radionuclide determinations: Second volume

    International Nuclear Information System (INIS)

    Morrow, R.W.; Crain, J.S.

    1998-01-01

    Even from its early conception, inductively coupled plasma-mass spectrometry (ICP-MS) was thought to be well-suited to the unique measurement problems facing the nuclear industry. These thoughts were well-founded; indeed, one might consider it unusual if a modern nuclear research center did not have access to one or more ICP mass spectrometers (quadrupole or otherwise). However, as ICP-MS has matured, improvements in sensitivity and precision have made possible measurements that were inconceivable to the founding fathers of the technology. Therefore, there is a periodic need to gather information and obtain a snapshot in time of the technology and its applications in nuclear energy. This second symposium was an international event in which speakers from the US, Europe, and the Middle East described new developments in ICP-MS relevant to the nuclear energy community. The papers presented at the 1998 symposium are published herein. Several papers have been processed separately for inclusion on the data base

  2. 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....

  3. 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...

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

    DEFF Research Database (Denmark)

    Qiao, Jixin; Lagerkvist, Petra; Rodushkin, Ilia

    2018-01-01

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

  5. Application of femtosecond laser ablation inductively coupled plasma mass spectrometry for quantitative analysis of thin Cu(In,Ga)Se{sub 2} solar cell films

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Seokhee [School of Mechatronics, Gwangju Institute of Science and Technology, 1 Oryong-dong, Buk-gu, Gwangju 500-712 (Korea, Republic of); Gonzalez, Jhanis J. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Yoo, Jong H. [Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Chirinos, Jose R. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Facultad de Ciencias, Universidad Central de Venezuela, Caracas 1041A (Venezuela, Bolivarian Republic of); Russo, Richard E. [Lawrence Berkeley National Laboratory, 1 Cyclotron Road, Berkeley, CA 94720 (United States); Applied Spectra Inc., 46665 Fremont Boulevard, Fremont, CA 94538 (United States); Jeong, Sungho, E-mail: shjeong@gist.ac.kr [School of Mechatronics, Gwangju Institute of Science and Technology, 1 Oryong-dong, Buk-gu, Gwangju 500-712 (Korea, Republic of)

    2015-02-27

    This work reports that the composition of Cu(In,Ga)Se{sub 2} (CIGS) thin solar cell films can be quantitatively predicted with high accuracy and precision by femtosecond laser ablation-inductively coupled plasma-mass spectrometry (fs-LA-ICP-MS). It is demonstrated that the results are strongly influenced by sampling conditions during fs-laser beam (λ = 1030 nm, τ = 450 fs) scanning on the CIGS surface. The fs-LA-ICP-MS signals measured at optimal sampling conditions generally provide a straight line calibration with respect to the reference concentrations measured by inductively coupled plasma optical emission spectroscopy (ICP-OES). The concentration ratios predicted by fs-LA-ICP-MS showed high accuracy, to 95–97% of the values measured with ICP-OES, for Cu, In, Ga, and Se elements. - Highlights: • Laser ablation inductively coupled plasma mass spectrometry of thin film is reported. • Concentration ratio prediction with a confidence level of 95–97% is achieved. • Quantitative determination of composition is demonstrated.

  6. A critical review of inductively coupled plasma-mass spectrometry for geoanalysis, geochemistry and hydrology, Part 1. Analytical performance

    Science.gov (United States)

    Brenner, I.B.; Taylor, Howard E.

    1992-01-01

    Present-day inductively coupled plasma-mass spectrometry (ICP-MS) instrumentation is described briefly. Emphasis is placed on performance characteristics for geoanalysis, geochemistry, and hydrology. Applications where ICP-MS would be indispensable are indicated. Determination of geochemically diagnostic trace elements (such as the rare earth elements [REE], U and Th), of isotope ratios for fingerprinting, tracer and other geo-isotope applications, and benchmark isotope dilution determinations are considered to be typical priority applications for ICP-MS. It is concluded that ICP-MS furnishes unique geoanalytical and environmental data that are not readily provided by conventional spectroscopic (emission and absorption) techniques.

  7. Measurement of isotopic composition of lanthanides in reprocessing process solutions by high-performance liquid chromatography with inductively coupled plasma mass spectrometry (HPLC/ICP-MS)

    International Nuclear Information System (INIS)

    Okano, Masanori; Jitsukata, Shu; Kuno, Takehiko; Yamada, Keiji

    2011-01-01

    Isotopic compositions of fission products in process solutions and wastes in a reprocessing plant are valuable to proceed safety study of the solutions and research/development concerning treatment/disposal of the wastes. The amount of neodymium-148 is a reliable indication to evaluate irradiation history. The isotopic compositions of samarium and gadolinium in high radioactive wastes are referred to as essential data to evaluate environmental impact in geological repositories. However, pretreatment of analysis must be done with complicated chemical separation such as solvent extraction and ion exchange. The actual measurement data of isotopic compositions of lanthanides comparable to the one of actinides in spent fuel reprocessing process has not been obtained enough. Rapid and high sensitive analytical technique based on high-performance liquid chromatography (HPLC) with an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the measurement of isotopic compositions of lanthanides in spent fuel reprocessing solutions. HPLC/ICP-MS measurement system was customized for a glove-box to be applied to the radioactive solutions. The cation exchange chromatographic columns (Shim-pack IC-C1) and injection valve (20μL) were located inside of the glove-box except the chromatographic pump. The elements of lanthanide group were separated by a gradient program of HPLC with α-hydroxyisobutyric acid. Isotopic compositions of lanthanides in eluate was sequentially analyzed by a quadruple ICP-MS. Optimization of parameter of HPLC and ICP-MS measurement system was examined with standard solutions containing 14 lanthanide elements. The elements of lanthanides were separated by HPLC and detected by ICP-MS within 25 minutes. The detection limits of Nd-146, Sm-147 and Gd-157 were 0.37 μg L -1 , 0.69 μg L -1 and 0.47 μg L -1 , respectively. The analytical precision of the above three isotopes was better than 10% for standard solutions of 100 μg L -1 with

  8. 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...

  9. Critical evaluation of analytical performance of atomic absorption spectrometry and inductively coupled plasma mass spectrometry for mercury determination

    International Nuclear Information System (INIS)

    Krata, A.; Bulska, E.

    2005-01-01

    The analytical performance of cold vapor atomic absorption spectrometry (CV AAS), graphite furnace atomic absorption spectrometry (GF AAS) and inductively coupled plasma mass spectrometry (ICP-MS) for mercury determination have been investigated with the use of two reference materials SRM 2710 Montana I Soil and BCR-144R (sewage sludge from domestic origin). The digestion conditions and their influence on determination of mercury have been studied. Samples were decomposed by microwave digestion in closed vessels with the use of HCl alone or mixture of HCl+HNO 3 +HF. The digestion solutions were analyzed by CV AAS using NaBH 4 as a reducing agent, by GF AAS with Pd or mixture of Pd/Rh as modifiers and by ICP-MS with Rh as internal standard. In the case of CV AAS, results were not dependent on digestion conditions. In the case of GF AAS and ICP-MS, results depended significantly on digestion conditions; in both cases, the use of the mixture of acids as defined above suppressed the signal of mercury. Therefore, in those cases, the microwave digestion with HCl is recommended. Detection limits of 0.003, 0.01 and 0.2 μg g -1 were achieved by ICP-MS, CV AAS and GF AAS, respectively

  10. Quantification of methionine and selenomethionine in biological samples using multiple reaction monitoring high performance liquid chromatography tandem mass spectrometry (MRM-HPLC-MS/MS).

    Science.gov (United States)

    Vu, Dai Long; Ranglová, Karolína; Hájek, Jan; Hrouzek, Pavel

    2018-05-01

    Quantification of selenated amino-acids currently relies on methods employing inductively coupled plasma mass spectrometry (ICP-MS). Although very accurate, these methods do not allow the simultaneous determination of standard amino-acids, hampering the comparison of the content of selenated versus non-selenated species such as methionine (Met) and selenomethionine (SeMet). This paper reports two approaches for the simultaneous quantification of Met and SeMet. In the first approach, standard enzymatic hydrolysis employing Protease XIV was applied for the preparation of samples. The second approach utilized methanesulfonic acid (MA) for the hydrolysis of samples, either in a reflux system or in a microwave oven, followed by derivatization with diethyl ethoxymethylenemalonate. The prepared samples were then analyzed by multiple reaction monitoring high performance liquid chromatography tandem mass spectrometry (MRM-HPLC-MS/MS). Both approaches provided platforms for the accurate determination of selenium/sulfur substitution rate in Met. Moreover the second approach also provided accurate simultaneous quantification of Met and SeMet with a low limit of detection, low limit of quantification and wide linearity range, comparable to the commonly used gas chromatography mass spectrometry (GC-MS) method or ICP-MS. The novel method was validated using certified reference material in conjunction with the GC-MS reference method. Copyright © 2018. Published by Elsevier B.V.

  11. Determination of hafnium at the 10−4% level (relative to zirconium content) using neutron activation analysis, inductively coupled plasma mass spectrometry and inductively coupled plasma atomic emission spectrometry

    International Nuclear Information System (INIS)

    Smolik, Marek; Polkowska-Motrenko, Halina; Hubicki, Zbigniew; Jakóbik-Kolon, Agata; Danko, Bożena

    2014-01-01

    Graphical abstract: -- Highlights: •We worked out ICP-MS method of Hf determination in Zr and Zr compounds. •We used NAA method as reference one. •We obtained pure zirconium matrix by ion exchange (Diphonix ® resin). •These permit to determine ≥1 × 10 −4 % Hf in Zr sample by ICP MS with good precision and accuracy. -- Abstract: Hafnium at the very low level of 1–8 ppm (in relation to zirconium) was determined in zirconium sulfate solutions (originating from investigations of the separation of ca. 44 ppm Hf from zirconium by means of the ion exchange method) by using three independent methods: inductively coupled plasma mass spectrometry (ICP MS), neutron activation analysis (NAA) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results of NAA and ICP MS determinations were consistent with each other across the entire investigated range (the RSD of both methods did not exceed 38%). The results of ICP-AES determination were more diverse, particularly at less than 5 ppm Hf (RSD was significantly higher: 29–253%). The ion exchange method exploiting Diphonix ® resin proved sufficient efficiency in Zr–Hf separation when the initial concentration ratio of the elements ([Zr] 0 /[Hf] 0 ) ranged from 1200 to ca. 143,000

  12. Establishment of methodology for determination of 93Zr in radioactive wastes by Liquid Scintillation Counting (LSC) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Oliveira, Thiago Cesar de

    2014-01-01

    The zirconium-93 is a long-lived pure β-particle-emitting radionuclide produced from 235 U fission and from neutron activation of the stable isotope 92 Zr and thus occurring as one of the radionuclides found in nuclear reactors. Due to its long half life, 93 Zr is one of the radionuclides of interest for the performance of assessment studies of waste storage or disposal. Measurement of 93 Zr is difficult owing to its trace level concentration and its low activity in nuclear wastes and further because its certified standards are not frequently available. The aim of this work was to develop a selective radiochemical separation methodology for the determination of 93 Zr in nuclear waste and analyze it by Liquid Scintillation Counting (LSC) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). To set up the radiochemical separation procedure for zirconium, a tracer solution of 95 Zr and its 724 keV γ-ray measurements by γ- spectrometry were used in order to follow the behavior of zirconium during the radiochemical separation. For the LSC technique a 55 Fe solution, which is one of the major interfering measures zirconium, was used to verify the decontamination factor during the separation process. The efficiency detection for 63 Ni was used to determination of 93 Zr activity in the matrices analyzed. The limit of detection of the 0.05 Bq 1 −1 was obtained for 63 Ni standard solutions by using a sample:cocktail ratio of 3:17 mL for Optiphase Hisafe 3 cocktail. For the ICP-MS technique a zirconium stable solution was used to verify the zirconium behavior and recovery during radiochemical separation and a solution of Ba, Co, Eu, Fe, Mn, Nb, Sr and Y was used to verify the decontamination factor during the separation process. A standard solution 93 Nb as isotope for determining the 93 Zr by ICP-MS was used for calibration and analysis. The detection limit of 0.039 ppb was obtained for the standard solution of zirconium. Then, the protocol was applied to low level

  13. 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.

  14. Results of an interlaboratory method performance study for the size determination and quantification of silver nanoparticles in chicken meat by single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS).

    Science.gov (United States)

    Weigel, Stefan; Peters, Ruud; Loeschner, Katrin; Grombe, Ringo; Linsinger, Thomas P J

    2017-08-01

    Single-particle inductively coupled plasma mass spectrometry (sp-ICP-MS) promises fast and selective determination of nanoparticle size and number concentrations. While several studies on practical applications have been published, data on formal, especially interlaboratory validation of sp-ICP-MS, is sparse. An international interlaboratory study was organized to determine repeatability and reproducibility of the determination of the median particle size and particle number concentration of Ag nanoparticles (AgNPs) in chicken meat. Ten laboratories from the European Union, the USA, and Canada determined particle size and particle number concentration of two chicken meat homogenates spiked with polyvinylpyrrolidone (PVP)-stabilized AgNPs. For the determination of the median particle diameter, repeatability standard deviations of 2 and 5% were determined, and reproducibility standard deviations were 15 and 25%, respectively. The equivalent median diameter itself was approximately 60% larger than the diameter of the particles in the spiking solution. Determination of the particle number concentration was significantly less precise, with repeatability standard deviations of 7 and 18% and reproducibility standard deviations of 70 and 90%.

  15. 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.

  16. Interfacing capillary electrophoresis with inductively coupled plasma mass spectrometry by direct injection nebulization for selenium speciation

    DEFF Research Database (Denmark)

    Bendahl, Lars; Gammelgaard, Bente; Jons, O.

    2001-01-01

    A demountable direct injection high efficiency nebulizer operating at low sample uptake rates was developed and used for coupling of capillary electrophoresis (CE) with inductively coupled plasma mass spectrometry (ICP-MS). When the nebulizer was used for continuous sample introduction, detection...

  17. 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)

  18. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Shih-Yi [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Jiang, Shiuh-Jen, E-mail: sjjiang@faculty.nsysu.edu.tw [Department of Chemistry, National Sun Yat-sen University, Kaohsiung 80424, Taiwan (China); Department of Medical Laboratory Science and Biotechnology, Kaohsiung Medical University, Kaohsiung 80708, Taiwan (China); Sahayam, A.C. [National Centre for Compositional Characterisation of Materials (CCCM), Hyderabad (India)

    2014-11-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min{sup −1} methane (CH{sub 4}) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g{sup −1} for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g{sup −1} (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions. - Highlights: • Determination of Cr, Fe, Cu, Zn and Se in cereal samples • Ultrasonic slurry sampling in combination with DRC-ICP-MS • Better sensitivity with thioacetamide modifier in ETV • Decreased sample preparation time with solid sampling • Validation with NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour.

  19. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    International Nuclear Information System (INIS)

    Huang, Shih-Yi; Jiang, Shiuh-Jen; Sahayam, A.C.

    2014-01-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min −1 methane (CH 4 ) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g −1 for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g −1 (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions. - Highlights: • Determination of Cr, Fe, Cu, Zn and Se in cereal samples • Ultrasonic slurry sampling in combination with DRC-ICP-MS • Better sensitivity with thioacetamide modifier in ETV • Decreased sample preparation time with solid sampling • Validation with NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour

  20. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young

    2005-01-01

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties

  1. Determination of Dibutyltin in Sediments Using Isotope Dilution Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Yim, Yong Hyeon; Park, Ji Youn; Han, Myung Sub; Park, Mi Kyung; Kim, Byung Joo; Lim, Young Ran; Hwang, Eui Jin; So, Hun Young [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

    2005-03-15

    A method is described for the determination of dibutyltin (DBT) in sediment by isotope dilution using liquid chromatography inductively-coupled plasma/mass spectrometry (LC-ICP/MS). To achieve the highest accuracy and precision, special attentions are paid in optimization and evaluation of overall processes of the analysis including extraction of analytes, characterization of the standards used for calibration and LC-ICP/MS conditions. An approach for characterization of natural abundance DBT standard has been developed by combining inductively-coupled plasma/optical emission spectrometry (ICP/OES) and LC-ICP/MS for the total Sn assay and the analysis of Sn species present as impurities, respectively. An excellent LC condition for separation of organotin species was found, which is suitable for simultaneous DBT and tributyltin (TBT) analysis as well as impurity analysis of DBT standards. Microwave extraction condition was also optimized for high efficiency while preventing species transformation. The present method determines the amount contents of DBT in sediments with expanded uncertainty of less than 5% and its result shows high degree of equivalence with reference values of an international inter-comparison and a certified reference material (CRM) within stated uncertainties.

  2. 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.

  3. 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.

  4. Multielemental analyses of tree rings by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Hall, G.S.

    1990-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) was evaluated for major, minor, trace, and ultra-trace elemental analyses of individual tree rings. The samples were obtained from an old-growth Douglas fir growing near Mount St. Helens volcano, and from trees at various other North American sites. Eightly percent of elements from Li to U had detection limits in the solid (wood) below 8.0 ng g -1 . Two anomalous peaks occur in Mount St. Helens samples at A.D. 1478 and 1490 that closely correlate with past eruptions of the volcano. These results show that ICP-MS is a rapid and sensitive analytical method for multielemental analyses of individual tree rings. (author) 16 refs.; 2 figs.; 2 tabs

  5. Determination of uranium in urine - Measurement of isotope ratios and quantification by use of inductively coupled plasma mass spectrometry

    NARCIS (Netherlands)

    Krystek, Petra; Ritsema, R.

    2002-01-01

    For analysis of uranium in urine determination of the isotope ratio and quantification were investigated by high-resolution inductively coupled plasma mass spectrometry (HR ICP-MS). The instrument used (ThermoFinniganMAT ELEMENT2) is a single-collector MS and, therefore, a stable sample-introduction

  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. Precise determination of dissolved silica in seawater by ion-exclusion chromatography isotope dilution inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Nonose, Naoko; Cheong, Chikako; Ishizawa, Yukari; Miura, Tsutomu; Hioki, Akiharu

    2014-08-20

    Ion exclusion chromatograph (IEC) isotope dilution (ID) inductively coupled plasma mass spectrometry (ICP-MS) (IEC-ID-ICP-MS) was developed for measurement of dissolved silica in seawater, which was applied to production of certified reference materials (CRMs) of three concentration levels of nutrients (high, medium and low levels). IEC-ICP-MS has been employed to separate dissolved silica from seawater matrix. In the present study, in order to solve substantial problems due to spectral interference in ICP-MS and to improve the accuracy of IEC-ICP-MS beyond standard addition or conventional calibration methods, ID method was coupled with ICP-sector field mass spectrometry (operated under medium resolution,i.e., m/Δm=4000). In addition, effects of various operating parameters in ICP-MS on a silicon background level were also investigated to obtain lower background equivalent concentration (BEC). As a result, 3 ng g(-1) of the BEC and 0.5 % of relative standard uncertainties were achieved in the analyses of dissolved silica in seawater samples at concentration levels from 4.0 mg kg (-1) to 0.8 mg kg(-1) as silicon. The developed method was successfully validated by analyses of an artificial seawater containing a known amount of silicate and the seawater certified reference material MOOS-2 produced by the National Research Council Canada. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

    Fabien Pointurier; Amelie Hubert; Anne-Claire Pottin

    2013-01-01

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

  9. 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...

  10. Ion deposition by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Hu, K.; Houk, R.S.

    1996-01-01

    An atmospheric pressure inductively coupled plasma (ICP) is used with a quadrupole mass spectrometer (MS) for ion deposition. The deposited element is introduced as a nebulized aqueous solution. Modifications to the ICP-MS device allow generation and deposition of a mass-resolved beam of 165 Ho + at 5x10 12 ions s -1 . The ICP is a universal, multielement ion source that can potentially be used for applications such as deposition of mixtures of widely varying stoichiometry or of alternating layers of different elements. copyright 1996 American Vacuum Society

  11. Plutonium determination in urine by techniques of mass spectrometry

    International Nuclear Information System (INIS)

    Hernandez M, H.; Yllera de Ll, A.

    2013-10-01

    The objective of this study was to develop an analytic method for quantification and plutonium reappraisal in plane tables of alpha spectrometry be means of the mass spectrometry technique of high resolution with plasma source inductively coupled and desolvator Aridus (Aridus-Hr-Icp-Ms) and mass spectrometry with accelerator (AMS). The obtained results were, the recovery percentage of Pu in the plane table was of ∼ 90% and activity minimum detectable obtained with Aridus-Hr-Icp-Ms and AMS was of ∼ 3 and ∼ 0.4 f g of 239 Pu, respectively. Conclusion, the results demonstrate the aptitude of the Aridus-Hr-Icp-Ms and AMS techniques in the Pu reappraisal in plane tables with bigger speed and precision, improving the values notably of the activity minimum detectable that can be obtained with the alpha spectrometry (∼ 50 f g of 239 Pu). (author)

  12. Quantitation of iothalamate in urine and plasma using liquid chromatography electrospray tandem mass spectrometry (HPLC-ESI-MS/MS).

    Science.gov (United States)

    Molinaro, Ross J; Ritchie, James C

    2010-01-01

    The following chapter describes a method to measure iothalamate in plasma and urine samples using high performance liquid chromatography combined with electrospray positive ionization tandem mass spectrometry (HPLC-ESI-MS/MS). Methanol and water are spiked with the internal standard (IS) iohexol. Iothalamate is isolated from plasma after IS spiked methanol extraction and from urine by IS spiked water addition and quick-spin filtration. The plasma extractions are dried under a stream of nitrogen. The residue is reconstituted in ammonium acetate-formic acid-water. The reconstituted plasma and filtered urine are injected into the HPLC-ESI-MS/MS. Iothalamate and iohexol show similar retention times in plasma and urine. Quantification of iothalamate in the samples is made by multiple reaction monitoring using the hydrogen adduct mass transitions, from a five-point calibration curve.

  13. Environmental application of elemental speciation analysis based on liquid or gas chromatography hyphenated to inductively coupled plasma mass spectrometry-A review

    International Nuclear Information System (INIS)

    Popp, Maximilian; Hann, Stephan; Koellensperger, Gunda

    2010-01-01

    In recent years the number of environmental applications of elemental speciation analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. The analytical characteristics, such as extremely low detection limits (LOD) for almost all elements, the wide linear range, the possibility for multi-elemental analysis and the possibility to apply isotope dilution mass spectrometry (IDMS) make ICP-MS an attractive tool for elemental speciation analysis. Two methodological approaches, i.e. the combination of ICP-MS with high performance liquid chromatography (HPLC) and gas chromatography (GC), dominate the field. Besides the investigation of metals and metalloids and their species (e.g. Sn, Hg, As), representing 'classic' elements in environmental science, more recently other elements (e.g. P, S, Br, I) amenable to ICP-MS determination were addressed. In addition, the introduction of isotope dilution analysis and the development of isotopically labeled species-specific standards have contributed to the success of ICP-MS in the field. The aim of this review is to summarize these developments and to highlight recent trends in the environmental application of ICP-MS coupled to GC and HPLC.

  14. A method for studies on interactions between a gold-based drug and plasma proteins based on capillary electrophoresis with inductively coupled plasma mass spectrometry detection

    DEFF Research Database (Denmark)

    Nguyen, Tam T T N; Østergaard, Jesper; Gammelgaard, Bente

    2015-01-01

    An analytical method based on capillary electrophoresis (CE) and inductively coupled plasma mass spectrometry (ICP-MS) detection was developed for studies on the interaction of gold-containing drugs and plasma proteins using auranofin as example. A detection limit of 18 ng/mL of auranofin corresp...

  15. 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)

  16. Total and species-specific quantitative analyses of trace elements in sediment by isotope dilution inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Inagaki, Kazumi; Takatsu, Akiko; Yarita, Takashi; Okamoto, Kensaku; Chiba, Koichi

    2009-01-01

    Isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) is one of the reliable methods for total and species-specific quantitative analysis of trace elements. However, several technical problems (e.g. spectral interference caused from sample constituents) should be overcome to obtain reliable analytical results when environmental samples are analyzed by ID-ICP-MS. In our laboratory, various methods based on ID-ICP-MS have been investigated for reliable quantitative analyses of trace elements in environmental samples. In this paper, coprecipitate separation/ID-ICP-MS for the determination of trace elements in sediment, cation exchange disk filtration/ID-ICP-MS for the determination of selenium in sediment, species-specific ID-ICP-MS using 118 Sn/labeled organotin compounds for the determination of butyltins and phenyltins, and the application of the ID-ICP-MS methods to the certification of sediment reference materials are described. (author)

  17. [A comparative study of cadmium, lead, mercury, arsenic, selenium, manganese, copper and zinc in brown rice and fish by inductively coupled plasma-mass spectrometry (ICP-MS) and atomic absorption spectrometry].

    Science.gov (United States)

    Oshima, Harumi; Ueno, Eiji; Saito, Isao; Matsumoto, Hiroshi

    2004-10-01

    A study was conducted to evaluate the applicability of ICP-MS techniques for determination of metals in brown rice and fish. Cadmium, lead, mercury, arsenic, selenium, manganese, copper and zinc were determined by this method. An open digestion with nitric acid (Method A) and a rapid open digestion with nitric acid and hydrochloric acid (Method B) were used to solubilize analytes in samples, and these procedures were followed by ICP-MS analysis. Recovery of certified elements from standard reference materials by Method A and Method B ranged from 92 to 110% except for mercury (70 to 100%). Analytical results of brown rice and fish samples obtained by this ICP-MS agreed with those obtained by atomic absorption spectrometry (AAS). The results of this study demonstrate that quadrupole ICP-MS provides precise and accurate measurements of the elements tested in brown rice and fish samples.

  18. Matrix separation by chelation to prepare biological materials for isotopic zinc analysis by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Durrant, S.F.; Krushevska, A.; Amarasiriwardena, D.; Argentine, M.D.; Romon-Guesnier, S.; Barnes, R.M.

    1994-01-01

    Following an evaluation of three chelating resins [Chelex-100, poly(dithiocarbamate) (PDTC) and carboxymethylated poly(ethyleneimine)-poly(methylenepolyphenylene) isocyanate (CPPI)], a procedure was established with the last of these for the separation of Zn from biological matrix elements prior to 70 Zn: 68 Zn isotopic analysis by inductively coupled plasma mass spectrometry (ICP-MS). The method was verified by establishing Zn recoveries and by determining its effectiveness in removing Cl and Na from buffered test solutions. Calcium, Na, and Zn concentration data were determined by inductively coupled plasma atomic emission spectrometry. Chlorine was measured by electrothermal vaporization ICP-MS. The efficacy of the technique was demonstrated by the determination of zinc isotope ratios in bovine milk and human urine. (Author)

  19. 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

  20. Rare earth elements determined in Antarctic ice by inductively coupled plasma-Time of flight, quadrupole and sector field-mass spectrometry: An inter-comparison study

    International Nuclear Information System (INIS)

    Dick, D.; Wegner, A.; Gabrielli, P.; Ruth, U.; Barbante, C.; Kriews, M.

    2008-01-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is a suitable tool for multi-element analysis at low concentration levels. Rare earth element (REE) determinations in standard reference materials and small volumes of molten ice core samples from Antarctica have been performed with an ICP-time of flight-MS (ICP-TOF-MS) system. Recovery rates for REE in e.g. SPS-SW1 amounted to ∼103%, and the relative standard deviations were 3.4% for replicate analysis at REE concentrations in the lower ng L -1 range. Analyses of REE concentrations in Antarctic ice core samples showed that the ICP-TOF-MS technique meets the demands of restricted sample mass. The data obtained are in good agreement with ICP-Quadrupole-MS (ICP-Q-MS) and ICP-Sector Field-MS (ICP-SF-MS) results. The ICP-TOF-MS system determines accurately and precisely REE concentrations exceeding 5 ng L -1 while between 0.5 and 5 ng L -1 accuracy and precision are element dependent

  1. Accurate determination of non-metallic impurities in high purity tetramethylammonium hydroxide using inductively coupled plasma tandem mass spectrometry

    Science.gov (United States)

    Fu, Liang; Xie, Hualin; Shi, Shuyun; Chen, Xiaoqing

    2018-06-01

    The content of non-metallic impurities in high-purity tetramethylammonium hydroxide (HPTMAH) aqueous solution has an important influence on the yield, electrical properties and reliability of the integrated circuit during the process of chip etching and cleaning. Therefore, an efficient analytical method to directly quantify the content of non-metallic impurities in HPTMAH aqueous solutions is necessary. The present study was aimed to develop a novel method that can accurately determine seven non-metallic impurities (B, Si, P, S, Cl, As, and Se) in an aqueous solution of HPTMAH by inductively coupled plasma tandem mass spectrometry (ICP-MS/MS). The samples were measured using a direct injection method. In the MS/MS mode, oxygen and hydrogen were used as reaction gases in the octopole reaction system (ORS) to eliminate mass spectral interferences during the analytical process. The detection limits of B, Si, P, S, Cl, As, and Se were 0.31, 0.48, 0.051, 0.27, 3.10, 0.008, and 0.005 μg L-1, respectively. The samples were analyzed by the developed method and the sector field inductively coupled plasma mass spectrometry (SF-ICP-MS) was used for contrastive analysis. The values of these seven elements measured using ICP-MS/MS were consistent with those measured by SF-ICP-MS. The proposed method can be utilized to analyze non-metallic impurities in HPTMAH aqueous solution. Table S2 Multiple potential interferences on the analytes. Table S3 Parameters of calibration curve and the detection limit (DL). Table S4 Results obtained for 25% concentration high-purity grade TMAH aqueous solution samples (μg L-1, mean ± standard deviation, n = 10).

  2. A novel quantification strategy of transferrin and albumin in human serum by species-unspecific isotope dilution laser ablation inductively coupled plasma mass spectrometry (ICP-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Feng, Liuxing, E-mail: fenglx@nim.ac.cn; Zhang, Dan; Wang, Jun; Shen, Dairui; Li, Hongmei

    2015-07-16

    Highlights: • Species-unspecific ID-PAGE-LA-ICP-MS was used to quantify Alb and Tf in human serum. • Addition methods of species-unspecific {sup 34}S spike were evaluated. • Isotope change conditions were investigated to reach satisfactory “isotope equilibration”. • Human serum CRM (ERM-DA470k/IFCC) was used to validate the new arrangements. • The developed method offers potential for accurate quantification of protein by ID-PAGE-LA-ICP-MS. - Abstract: Species-specific (SS) isotope dilution analysis with gel electrophoresis (GE)-laser ablation (LA)-ICP-MS is a promising technique for the quantification of particular metal-binding proteins in biological samples. However, unavailable isotopically enriched spike and metal losses in GE separation are main limitations for SS-isotope dilution PAGE-LA-ICP-MS. In this study, we report for the first time the absolute quantification of transferrin (Tf) and albumin (Alb) in human serum by non-denaturing (native) GE combined with species-unspecific isotope dilution mass spectrometry (IDMS). In order to achieve a homogeneous distribution of both protein and isotope-enriched spike (simulated isotope equilibration), immersing the protein strips with {sup 34}S spike solution after gel electrophoresis was demonstrated to be an effective way of spike addition. Furthermore, effects of immersion time and {sup 34}S spike concentration were investigated to obtain optimal conditions of the post-electrophoresis isotope dilution method. The relative mass of spike and ablated sample (m{sub sp}/m{sub sam}) in IDMS equation was calculated by standard Tf and Alb proteins, which could be applied to the quantification of Tf and Alb in ERM-DA470k/IFCC for method confirmation. The results were in agreement with the certified value with good precision and small uncertainty (1.5–3%). In this method, species-specific spike protein is not necessary and the integrity of the heteroatom-protein could be maintained in sample preparation

  3. A novel quantification strategy of transferrin and albumin in human serum by species-unspecific isotope dilution laser ablation inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Feng, Liuxing; Zhang, Dan; Wang, Jun; Shen, Dairui; Li, Hongmei

    2015-01-01

    Highlights: • Species-unspecific ID-PAGE-LA-ICP-MS was used to quantify Alb and Tf in human serum. • Addition methods of species-unspecific 34 S spike were evaluated. • Isotope change conditions were investigated to reach satisfactory “isotope equilibration”. • Human serum CRM (ERM-DA470k/IFCC) was used to validate the new arrangements. • The developed method offers potential for accurate quantification of protein by ID-PAGE-LA-ICP-MS. - Abstract: Species-specific (SS) isotope dilution analysis with gel electrophoresis (GE)-laser ablation (LA)-ICP-MS is a promising technique for the quantification of particular metal-binding proteins in biological samples. However, unavailable isotopically enriched spike and metal losses in GE separation are main limitations for SS-isotope dilution PAGE-LA-ICP-MS. In this study, we report for the first time the absolute quantification of transferrin (Tf) and albumin (Alb) in human serum by non-denaturing (native) GE combined with species-unspecific isotope dilution mass spectrometry (IDMS). In order to achieve a homogeneous distribution of both protein and isotope-enriched spike (simulated isotope equilibration), immersing the protein strips with 34 S spike solution after gel electrophoresis was demonstrated to be an effective way of spike addition. Furthermore, effects of immersion time and 34 S spike concentration were investigated to obtain optimal conditions of the post-electrophoresis isotope dilution method. The relative mass of spike and ablated sample (m sp /m sam ) in IDMS equation was calculated by standard Tf and Alb proteins, which could be applied to the quantification of Tf and Alb in ERM-DA470k/IFCC for method confirmation. The results were in agreement with the certified value with good precision and small uncertainty (1.5–3%). In this method, species-specific spike protein is not necessary and the integrity of the heteroatom-protein could be maintained in sample preparation process. Moreover, the

  4. Investigation of a measure of robustness in inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Makonnen, Yoseif; Beauchemin, Diane

    2015-01-01

    In industrial/commercial settings where operators often have minimal expertise in inductively coupled plasma (ICP) mass spectrometry (MS), there is a prevalent need for a response factor indicating robust plasma conditions, which is analogous to the Mg II/Mg I ratio in ICP optical emission spectrometry (OES), whereby a Mg II/Mg I ratio of 10 constitutes robust conditions. While minimizing the oxide ratio usually corresponds to robust conditions, there is no specific target value that is widely accepted as indicating robust conditions. Furthermore, tuning for low oxide ratios does not necessarily guarantee minimal matrix effects, as they really address polyatomic interferences. From experiments, conducted in parallel for both MS and OES, there were some element pairs of similar mass and very different ionization potential that were exploited for such a purpose, the rationale being that, if these elements were ionized to the same extent, then that could be indicative of a robust plasma. The Be II/Li I intensity ratio was directly related to the Mg II/Mg I ratio in OES. Moreover, the 9Be+/7Li+ ratio was inversely related to the CeO+/Ce+ and LaO+/La+ oxide ratios in MS. The effects of different matrices (i.e. 0.01-0.1 M Na) were also investigated and compared to a conventional argon plasma optimized for maximum sensitivity. The suppression effect of these matrices was significantly reduced, if not eliminated in the case of 0.01 M Na, when the 9Be+/7Li+ ratio was around 0.30 on the Varian 820 MS instrument. Moreover, a very similar ratio (0.28) increased robustness to the same extent on a completely different ICP-MS instrument (PerkinElmer NEXION). Much greater robustness was achieved using a mixed-gas plasma with nitrogen in the outer gas and either nitrogen or hydrogen as a sheathing gas, as the 9Be+/7Li+ ratio was then around 1.70. To the best of our knowledge, this is the first report on using a simple analyte intensity ratio, 9Be+/7Li+, to gauge plasma robustness.

  5. Laser ablation-inductively coupled plasma-mass spectrometry: Examinations of the origins of polyatomic ions and advances in the sampling of particulates

    Energy Technology Data Exchange (ETDEWEB)

    Witte, Travis [Iowa State Univ., Ames, IA (United States)

    2011-01-01

    This dissertation provides a general introduction to Inductively coupled plasma-mass spectrometry (ICP-MS) and laser ablation (LA) sampling, with an examination of analytical challenges in the employment of this technique. It discusses the origin of metal oxide ions (MO+) in LA-ICP-MS, as well as the effect of introducing helium and nitrogen to the aerosol gas flow on the formation of these polyatomic interferences. It extends the study of polyatomic ions in LA-ICP-MS to metal argide (MAr+) species, an additional source of possible significant interferences in the spectrum. It describes the application of fs-LA-ICP-MS to the determination of uranium isotope ratios in particulate samples.

  6. 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.

  7. 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.

  8. Progress in determination of long-lived radionuclides by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

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

    2000-01-01

    Mass spectrometric methods (such as inductively coupled plasma mass spectrometry - ICP-MS and laser ablation (LA)-ICP-MS) with their ability to provide a very sensitive multielemental and precise isotopic analysis have become established for the determination of radionuclides in quite different sample materials. The determination of long-lived radionuclides is of increasing interest for the characterization of radioactive waste materials and for the detection of radionuclide contamination in environmental materials in which several radioactive nuclides are present from fallout due to nuclear weapons testing, nuclear power plants or nuclear accidents. Due to its multielement capability, excellent sensitivity, low detection limits (up to sub pg I 1 range), very good precision, easy sample preparation and measurement procedures ICP-MS of aqueous solutions has been increasingly applied for the ultrasensitive determination of long-lived radionuclides such as 99 Tc, 129 I, 230 Th, 232 Th, 234 U, 235 U, 236 U, 239 Pu, 240 Pu and 241 Am and precise isotope ratio measurements of U,Th and Pu. The application especially of microanalytical methods (analysis of some MU by flow injection and on-line coupling techniques as capillary electrophoresis (CE-ICP-MS) or HPLC-ICP-MS) for the precise determination nuclide abundances and concentration of long-lived radionuclides at ultra trace concentration levels in radioactive waste and also for controlling contamination from radioactive waste in the environment is a challenging task

  9. Fourier Transform Infrared (FT-IR) and Laser Ablation Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS) Imaging of Cerebral Ischemia: Combined Analysis of Rat Brain Thin Cuts Toward Improved Tissue Classification.

    Science.gov (United States)

    Balbekova, Anna; Lohninger, Hans; van Tilborg, Geralda A F; Dijkhuizen, Rick M; Bonta, Maximilian; Limbeck, Andreas; Lendl, Bernhard; Al-Saad, Khalid A; Ali, Mohamed; Celikic, Minja; Ofner, Johannes

    2018-02-01

    Microspectroscopic techniques are widely used to complement histological studies. Due to recent developments in the field of chemical imaging, combined chemical analysis has become attractive. This technique facilitates a deepened analysis compared to single techniques or side-by-side analysis. In this study, rat brains harvested one week after induction of photothrombotic stroke were investigated. Adjacent thin cuts from rats' brains were imaged using Fourier transform infrared (FT-IR) microspectroscopy and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The LA-ICP-MS data were normalized using an internal standard (a thin gold layer). The acquired hyperspectral data cubes were fused and subjected to multivariate analysis. Brain regions affected by stroke as well as unaffected gray and white matter were identified and classified using a model based on either partial least squares discriminant analysis (PLS-DA) or random decision forest (RDF) algorithms. The RDF algorithm demonstrated the best results for classification. Improved classification was observed in the case of fused data in comparison to individual data sets (either FT-IR or LA-ICP-MS). Variable importance analysis demonstrated that both molecular and elemental content contribute to the improved RDF classification. Univariate spectral analysis identified biochemical properties of the assigned tissue types. Classification of multisensor hyperspectral data sets using an RDF algorithm allows access to a novel and in-depth understanding of biochemical processes and solid chemical allocation of different brain regions.

  10. Determination of Trace Iron in Red Wine by Isotope Dilution Mass Spectrometry Using Multiple-Collector Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Zhou Tao; Wang Jun; Lu Hai; Zhou Yuanjing; Li Haifeng

    2009-01-01

    This paper introduces determination of trace iron in red wine certified reference material by isotope dilution mass spectrometry (IDMS) method using a multiplecollector inductively coupled plasma mass spectrometry, equipped with a hexapole collision cell. The measurement procedure of iron isotopic abundance ratios was deeply researched. Reduced polyatomic ion interferences to iron isotopes ion by collision reaction using Ar and H 2 gas, high precise isotopic abundance ratios were achieved. Two relative measurement methods (ICP-MS and ICP-OES) were used to analyze trace iron in red wine. The results are compared with IDMS results, which indicate that they are accordant. The uncertainty analyses include each uncertainty factor in whole experiment and the uncertainty of used certified reference material and it shows that the procedure blank is not neglectable to detect limit and precision of the method. The establishment of IDMS method for analysis of trace iron in red wine supports the certification of certified reference materials. (authors)

  11. Standard test method for analysis of total and isotopic uranium and total thorium in soils by inductively coupled plasma-mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2008-01-01

    1.1 This test method covers the measurement of total uranium (U) and thorium (Th) concentrations in soils, as well as the determination of the isotopic weight percentages of 234U, 235U, 236U, and 238U, thereby allowing for the calculation of individual isotopic uranium activity or total uranium activity. This inductively coupled plasma-mass spectroscopy (ICP-MS) method is intended as an alternative analysis to methods such as alpha spectroscopy or thermal ionization mass spectroscopy (TIMS). Also, while this test method covers only those isotopes listed above, the instrumental technique may be expanded to cover other long-lived radioisotopes since the preparation technique includes the preconcentration of the actinide series of elements. The resultant sample volume can be further reduced for introduction into the ICP-MS via an electrothermal vaporization (ETV) unit or other sample introduction device, even though the standard peristaltic pump introduction is applied for this test method. The sample preparatio...

  12. 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)

  13. 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.

  14. 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.)

  15. Aerosol detection efficiency in inductively coupled plasma mass spectrometry

    Science.gov (United States)

    Hubbard, Joshua A.; Zigmond, Joseph A.

    2016-05-01

    An electrostatic size classification technique was used to segregate particles of known composition prior to being injected into an inductively coupled plasma mass spectrometer (ICP-MS). Size-segregated particles were counted with a condensation nuclei counter as well as sampled with an ICP-MS. By injecting particles of known size, composition, and aerosol concentration into the ICP-MS, efficiencies of the order of magnitude aerosol detection were calculated, and the particle size dependencies for volatile and refractory species were quantified. Similar to laser ablation ICP-MS, aerosol detection efficiency was defined as the rate at which atoms were detected in the ICP-MS normalized by the rate at which atoms were injected in the form of particles. This method adds valuable insight into the development of technologies like laser ablation ICP-MS where aerosol particles (of relatively unknown size and gas concentration) are generated during ablation and then transported into the plasma of an ICP-MS. In this study, we characterized aerosol detection efficiencies of volatile species gold and silver along with refractory species aluminum oxide, cerium oxide, and yttrium oxide. Aerosols were generated with electrical mobility diameters ranging from 100 to 1000 nm. In general, it was observed that refractory species had lower aerosol detection efficiencies than volatile species, and there were strong dependencies on particle size and plasma torch residence time. Volatile species showed a distinct transition point at which aerosol detection efficiency began decreasing with increasing particle size. This critical diameter indicated the largest particle size for which complete particle detection should be expected and agreed with theories published in other works. Aerosol detection efficiencies also displayed power law dependencies on particle size. Aerosol detection efficiencies ranged from 10- 5 to 10- 11. Free molecular heat and mass transfer theory was applied, but

  16. 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.

  17. Laser ablation inductively coupled plasma mass spectrometry for the determination of trace elements in soil

    International Nuclear Information System (INIS)

    Lee Yiling; Chang Chaochiang; Jiang Shiuhjen

    2003-01-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been applied to the determination of Cr, Cu, Zn, Cd and Pb in soil samples. The dried soil powder was pressed into a pellet for LA-ICP-MS analysis. Triton X-100 was added to work as the modifier to enhance the ion signals. The influences of instrument operating conditions (LA and ICP-MS) and pellet preparation on the ion signals were reported. For Cr determination, the ICP-MS was operated under the dynamic reaction cell mode which alleviated the mass overlap interference. Standard addition method and isotope dilution method were used for the quantitation work. The powder sample was spiked with suitable amounts of element standards and/or enriched isotopes, well-mixed, dried and then pressed into a pellet for LA-ICP-MS analysis. This method has been applied to determine Cr, Cu, Zn, Cd and Pb in NIST SRM 2711 Montana soil and NIST SRM 2709 San Joaquin soil reference materials. The analysis results were in agreement with the certified values. The precision between sample replicates was better than 5% with LA-ICP-MS method. Detection limits estimated from standard addition curves were approximately 0.9, 2, 9, 0.7 and 0.3 ng g -1 for Cr, Cu, Zn, Cd and Pb, respectively

  18. Characterisation of nuclear fuel samples by quadrupole and multi-collector inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Wernli, Beath; Guenther-Leopold, Ines; Kobler Waldis, Judith; Kopajtic, Zlatan

    2003-01-01

    The characterisation of nuclear fuel cycle materials for trace and minor metallic constituents is of great interest for the nuclear industry and safeguard officials. The main objective of various international programmes dealing with postirradiation examinations is to improve the knowledge of the inventories of actinides, fission and spallation products in spent nuclear fuels. The low detection limits for a large number of elements combined with the ability to analyse the isotopic composition of the elements have established inductively coupled plasma mass spectrometry (ICP-MS) as a powerful multi-element technique in diverse analytical applications for the characterisation of nuclear materials. Because numerous isobaric overlaps restrict the direct determination of many fission products by mass spectrometry, extensive chemical separations are required for these elements. In order to simplify this sample preparation procedure, a high performance liquid chromatography system (HPLC) was online coupled to the mass spectrometer. Since about 10 years a quadrupole based ICP-MS (Q-ICP-MS) combined with an HPLC is used within the Hot Laboratory of the Paul Scherrer Institut for different applications on nuclear fuel samples. Since May 2003 also a new multi-collector ICP-MS (MC-ICP-MS) is used for the mass spectrometric characterisation of nuclear fuel samples, especially for the precise determination of the isotopic vectors of fission products and actinides. Therefore, two complementary analytical systems are now available in the group of 'Isotope and Wet Analytical Chemistry'. A comparison of the analytical performance of both systems (with and without an online coupled HPLC system) for the determination of the isotopic composition and the elemental concentration of different nuclides in nuclear fuel samples, the advantages and limitations of both techniques, the accuracy and precision of the results and typical applications for both methods will be discussed in the

  19. 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.

  20. Molecules and elements for quantitative bioanalysis: The allure of using electrospray, MALDI, and ICP mass spectrometry side-by-side.

    Science.gov (United States)

    Linscheid, Michael W

    2018-03-30

    To understand biological processes, not only reliable identification, but quantification of constituents in biological processes play a pivotal role. This is especially true for the proteome: protein quantification must follow protein identification, since sometimes minute changes in abundance tell the real tale. To obtain quantitative data, many sophisticated strategies using electrospray and MALDI mass spectrometry (MS) have been developed in recent years. All of them have advantages and limitations. Several years ago, we started to work on strategies, which are principally capable to overcome some of these limits. The fundamental idea is to use elemental signals as a measure for quantities. We began by replacing the radioactive 32 P with the "cold" natural 31 P to quantify modified nucleotides and phosphorylated peptides and proteins and later used tagging strategies for quantification of proteins more generally. To do this, we introduced Inductively Coupled Plasma Mass Spectrometry (ICP-MS) into the bioanalytical workflows, allowing not only reliable and sensitive detection but also quantification based on isotope dilution absolute measurements using poly-isotopic elements. The detection capability of ICP-MS becomes particularly attractive with heavy metals. The covalently bound proteins tags developed in our group are based on the well-known DOTA chelate complex (1,4,7,10-tetraazacyclododecane-N,N',N″,N‴-tetraacetic acid) carrying ions of lanthanoides as metal core. In this review, I will outline the development of this mutual assistance between molecular and elemental mass spectrometry and discuss the scope and limitations particularly of peptide and protein quantification. The lanthanoide tags provide low detection limits, but offer multiplexing capabilities due to the number of very similar lanthanoides and their isotopes. With isotope dilution comes previously unknown accuracy. Separation techniques such as electrophoresis and HPLC were used and just

  1. Development of precise analytical methods for strontium and lanthanide isotopic ratios using multiple collector inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Ohno, Takeshi; Takaku, Yuichi; Hisamatsu, Shun'ichi

    2007-01-01

    We have developed precise analytical methods for strontium and lanthanide isotopic ratios using multiple collector-ICP-mass spectrometry (MC-ICP-MS) for experimental and environmental studies of their behavior. In order to obtain precise isotopic data using MC-ICP-MS, the mass discrimination effect was corrected by an exponential law correction method. The resulting isotopic data demonstrated that highly precise isotopic analyses (better than 0.1 per mille as 2SD) could be achieved. We also adopted a de-solvating nebulizer system to improve the sensitivity. This system could minimize the water load into the plasma and provided about five times larger intensity of analyte than a conventional nebulizer system did. (author)

  2. Detection efficiencies in nano- and femtosecond laser ablation inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Waelle, M.; Koch, J.; Flamigni, L.; Heiroth, S.; Lippert, T.; Hartung, W.; Guenther, D.

    2009-01-01

    Detection efficiencies of laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), defined as the ratio of ions reaching the detector and atoms released by LA were measured. For this purpose, LA of silicate glasses, zircon, and pure silicon was performed using nanosecond (ns) as well as femtosecond (fs) LA. For instance, ns-LA of silicate glass using helium as in-cell carrier gas resulted in detection efficiencies between approximately 1E-7 for low and 3E-5 for high mass range elements which were, in addition, almost independent on the laser wavelength and pulse duration chosen. In contrast, the application of argon as carrier gas was found to suppress the detection efficiencies systematically by a factor of up to 5 mainly due to a less efficient aerosol-to-ion conversion and ion transmission inside the ICP-MS

  3. Method-MS. Final report

    International Nuclear Information System (INIS)

    Skipperud, L.; Popic, J.M.; Roos, P.; Salminen, S.; Nygren, U.; Sigmarsson, O.; Palsson, S.E.

    2011-05-01

    Radiometric determination methods, such as alpha spectrometry require long counting times when low activities are to be determined. Mass spectrometric techniques as Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Thermal Ionisation Mass Spectrometry (TIMS) and Accelerator Mass Spectrometry (AMS) have shown several advantages compared to traditional methods when measuring long-lived radionuclides. Mass spectrometric methods for determination of very low concentrations of elemental isotopes, and thereby isotopic ratios, have been developed using a variety of ion sources. Although primarily applied to the determination of the lighter stable element isotopes and radioactive isotopes in geological studies, the techniques can equally well be applied to the measurement of activity concentrations of long-lived low-level radionuclides in various samples using 'isotope dilution' methods such as those applied in inductively coupled plasma mass spectrometry (ICP-MS). Due to the low specific activity of long-lived radionuclides, many of these are more conveniently detected using mass spectrometric techniques. Mass spectrometry also enables the individual determination of Pu-239 and Pu-240, which cannot be obtained by alpha spectrometry. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) are rapidly growing techniques for the ultra-trace analytical determination of stable and long-lived isotopes and have a wide potential within environmental science, including ecosystem tracers and radio ecological studies. Such instrumentation, of course needs good radiochemical separation, to give best performance. The objectives of the project is to identify current needs and problems within low-level determination of long-lived radioisotopes by ICP-MS, to perform intercalibration and development and improvement of ICP-MS methods for the measurement of radionuclides and isotope ratios and to develop new methods based on modified separation chemistry applied to new auxiliary

  4. Method-MS. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Skipperud, L.; Popic, J.M. (Norwegian Univ. of Life Science (UMB), Isotope Lab. (Norway)); Roos, P. (Technical Univ. of Denmark, Risoe National Lab. for Sustainable Energy, Roskilde (Denmark)); Salminen, S. (Univ. of Helsinki (UH) (Finland)); Nygren, U. (Swedish Defence Research Agency (FOI) (Sweden)); Sigmarsson, O.; Palsson, S.E. (Univ. of Iceland/Icelandic Radiation Protection Institute (Iceland))

    2011-05-15

    Radiometric determination methods, such as alpha spectrometry require long counting times when low activities are to be determined. Mass spectrometric techniques as Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Thermal Ionisation Mass Spectrometry (TIMS) and Accelerator Mass Spectrometry (AMS) have shown several advantages compared to traditional methods when measuring long-lived radionuclides. Mass spectrometric methods for determination of very low concentrations of elemental isotopes, and thereby isotopic ratios, have been developed using a variety of ion sources. Although primarily applied to the determination of the lighter stable element isotopes and radioactive isotopes in geological studies, the techniques can equally well be applied to the measurement of activity concentrations of long-lived low-level radionuclides in various samples using 'isotope dilution' methods such as those applied in inductively coupled plasma mass spectrometry (ICP-MS). Due to the low specific activity of long-lived radionuclides, many of these are more conveniently detected using mass spectrometric techniques. Mass spectrometry also enables the individual determination of Pu-239 and Pu-240, which cannot be obtained by alpha spectrometry. Inductively Coupled Plasma Mass Spectrometry (ICP-MS) are rapidly growing techniques for the ultra-trace analytical determination of stable and long-lived isotopes and have a wide potential within environmental science, including ecosystem tracers and radio ecological studies. Such instrumentation, of course needs good radiochemical separation, to give best performance. The objectives of the project is to identify current needs and problems within low-level determination of long-lived radioisotopes by ICP-MS, to perform intercalibration and development and improvement of ICP-MS methods for the measurement of radionuclides and isotope ratios and to develop new methods based on modified separation chemistry applied to new

  5. The Prestudy for Studying Inorganic Nutrient Metabolism in Humans : the Aplication of ICP-MS for Determination of Stable Isotope Ratio of Fe and Zn

    International Nuclear Information System (INIS)

    Rukihati; Sumadjo

    2001-01-01

    A method is described for the determination of isotope ratio of Fe and Zn by means of inductively coupled plasma-mass spectrometry (ICP-MS). The mass spectrometer was operated in low resolution mode to provide maximal sensitivity. Typical conditions for operations were: plasma power 0.85 k W, reflected power 56 Fe/ 54 Fe, 57 Fe/ 54 Fe, 58 Fe/ 54 Fe, dan 64 Zn/ 67 Zn, 66 Zn/ 67 Zn, 68 Zn/ 67 Zn, 70 Zn/ 67 Zn measured by ICP-MS showed a good level of agreement with TIMS (thermal ionization mass spectrometry). This method was prepared for studying the absorption and/or metabolism of inorganic nutrients in humans. (author)

  6. Determination of long-lived actinides in soil leachates by inductively coupled plasma: Mass spectrometry

    International Nuclear Information System (INIS)

    Crain, J.S.; Smith, L.L.; Yaeger, J.S.; Alvarado, J.A.

    1994-01-01

    Inductively coupled plasma -- mass spectrometry (ICP-MS) was used to concurrently determine multiple long-lived (t 1/2 > 10 4 y) actinide isotopes in soil samples. Ultrasonic nebulization was found to maximize instrument sensitivity. Instrument detection limits for actinides in solution ranged from 50 mBq L -1 ( 239 Pu) to 2 μBq L -1 ( 235 U) Hydride adducts of 232 Th and 238 U interfered with the determinations of 233 U and 239 Pu; thus, extraction chromatography was, used to eliminate the sample matrix, concentrate the analytes, and separate uranium from the other actinides. Alpha spectrometric determinations of 230 Th, 239 Pu, and the 234 U/ 238 U activity ratio in soil leachates compared well with ICP-MS determinations; however, there were some small systematic differences (ca. 10%) between ICP-MS and a-spectrometric determinations of 234 U and 238 U activities

  7. Forensic investigation of brick stones using instrumental neutron activation analysis (INAA), laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and X-ray fluorescence analysis (XRF)

    International Nuclear Information System (INIS)

    Scheid, Nicole; Becker, Stefan; Duecking, Marc; Hampel, Gabriele; Volker Kratz, Jens; Watzke, Peter; Weis, Peter; Zauner, Stephan

    2009-01-01

    Brick stones collected from different production facilities were studied for their elemental compositions under forensic aspects using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), instrumental neutron activation analysis (INAA) and X-ray fluorescence analysis (XRF). The aim of these examinations was to assess the potential of these methods in forensic comparison analyses of brick stones. The accuracy of the analysis methods was evaluated using NIST standard reference materials (679, 98b and 97b). In order to compare the stones to each other, multivariate data analysis was used. The evaluation of the INAA results (based on the concentrations of V, Na, K, Sm, U, Sc, Fe, Co, Rb and Cs) using principal component analysis (PCA) and cluster analysis is presented as an example. The results derived from the different analytical methods are consistent. It was shown that elemental analysis using the described methods is a valuable tool for forensic examinations of brick stones.

  8. 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)

  9. Measurements of total lead concentrations and of lead isotope ratios in whole blood by use of inductively coupled plasma source mass spectrometry

    International Nuclear Information System (INIS)

    Delves, H.T.; Campbell, M.J.

    1988-01-01

    Methods are described for the accurate and precise determination of total lead and its isotopic composition in whole blood using inductively coupled plasma source mass spectrometry (ICP-MS). Sensitivities of up to 3 x 10 6 counts s -1 for 208 Pb at a total lead concentration of 5 μmol l -1 (1 μg ml -1 ) enabled total blood lead levels to be measured in 4 min per sample, with a detection limit of 0.072 μmol l -1 (15 μg l -1 ). The agreement between ICP-MS and atomic absorption spectrometry (AAS) for this analysis was excellent: ICP-MS 0.996 x AAS -0.0165 μmol l -1 ; r 0.994. Isotope ratio measurements required 15 min to achieve the required accuracy and precision both of which were generally better than 0.5% for 206 Pb: 207 Pb and 208 Pb: 206 Pb isotopic lead ratios. The ICP-MS data for these ratios in ten quality control blood specimens has a mean bias relative to isotope dilution mass spectrometry of -0.412% for 206 Pb: 207 Pb ratios and of +0.055% for the 208 Pb: 206 Pb ratios. This level of accuracy and that of the total blood lead measurements is sufficient to permit application of these ICP-MS methods to environmental studies. (author)

  10. Determination of 20 trace elements and arsenic species for a realgar-containing traditional Chinese medicine Niuhuang Jiedu tablets by direct inductively coupled plasma-mass spectrometry and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Jin, Pengfei; Liang, Xiaoli; Xia, Lufeng; Jahouh, Farid; Wang, Rong; Kuang, Yongmei; Hu, Xin

    2016-01-01

    Niuhuang Jiedu tablet (NHJDT) is a realgar-containing traditional Chinese medicine. A direct inductively coupled plasma-mass spectrometry (ICP-MS) method for the simultaneous determination of 20 trace elements (Mg, K, Ca, Na, Fe, As, Zn, Sr, Ba, Cu, Mn, Ni, Pb, V, Cr, Se, Co, Mo, Cd, Hg) in NHJDT, as well as in water, gastric fluid and intestinal fluid was established. Meanwhile, a high performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) method was developed for the determination of arsenite (As(III)), arsenate (As(V)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and for the identification of arsenobetaine (AsB) and arsenocholine (AsC) in these extracts. Both methods were fully validated in the respect of linearity, sensitivity, precision, stability and accuracy. The reliability of the ICP-MS method was further evaluated using a certified standard reference material prepared from dried tomato leaves (NIST, SRM 1572a). The analysis showed that some manufacturers formulated lower amount of realgar than required in the Chinese Pharmacopoeia (ChP) in their preparations. In addition, almost same extraction profiles for total As and inorganic As were found in water and in gastrointestinal fluids, while higher extraction rates for other 19 elements were observed in gastrointestinal fluids. Our findings show that the toxicities of Hg, Cu, Cd and Pb in NHJDP are low, while the real As toxicity in NHJDT should be deeply investigated. Copyright © 2015 Elsevier GmbH. All rights reserved.

  11. Inductively Coupled Plasma: Fundamental Particle Investigations with Laser Ablation and Applications in Magnetic Sector Mass Spectrometry

    International Nuclear Information System (INIS)

    Nathan Joe Saetveit

    2008-01-01

    Particle size effects and elemental fractionation in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) are investigated with nanosecond and femtosecond laser ablation, differential mobility analysis, and magnetic sector ICP-MS. Laser pulse width was found to have a significant influence on the LA particle size distribution and the elemental composition of the aerosol and thus fractionation. Emission from individual particles from solution nebulization, glass, and a pressed powder pellet are observed with high speed digital photography. The presence of intact particles in an ICP is shown to be a likely source of fractionation. A technique for the online detection of stimulated elemental release from neural tissue using magnetic sector ICP-MS is described. Detection limits of 1 (micro)g L -1 or better were found for P, Mn, Fe, Cu, and Zn in a 60 (micro)L injection in a physiological saline matrix

  12. Fundamental studies of the plasma extraction and ion beam formation processes in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Niu, Hongsen.

    1995-01-01

    The fundamental and practical aspects are described for extracting ions from atmospheric pressure plasma sources into an analytical mass spectrometer. Methodologies and basic concepts of inductively coupled plasma mass spectrometry (ICP-MS) are emphasized in the discussion, including ion source, sampling interface, supersonic expansion, slumming process, ion optics and beam focusing, and vacuum considerations. Some new developments and innovative designs are introduced. The plasma extraction process in ICP-MS was investigated by Langmuir measurements in the region between the skimmer and first ion lens. Electron temperature (T e ) is in the range 2000--11000 K and changes with probe position inside an aerosol gas flow. Electron density (n e ) is in the range 10 8 --10 10 -cm at the skimmer tip and drops abruptly to 10 6 --10 8 cm -3 near the skimmer tip and drops abruptly to 10 6 --10 8 cm -3 downstream further behind the skimmer. Electron density in the beam leaving the skimmer also depends on water loading and on the presence and mass of matrix elements. Axially resolved distributions of electron number-density and electron temperature were obtained to characterize the ion beam at a variety of plasma operating conditions. The electron density dropped by a factor of 101 along the centerline between the sampler and skimmer cones in the first stage and continued to drop by factors of 10 4 --10 5 downstream of skimmer to the entrance of ion lens. The electron density in the beam expansion behind sampler cone exhibited a 1/z 2 intensity fall-off (z is the axial position). An second beam expansion originated from the skimmer entrance, and the beam flow underwent with another 1/z 2 fall-off behind the skimmer. Skimmer interactions play an important role in plasma extraction in the ICP-MS instrument

  13. 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...

  14. Sample introduction systems for the analysis of liquid microsamples by ICP-AES and ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Todoli, Jose L. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, 03080 Alicante (Spain)]. E-mail: jose.todoli@ua.es; Mermet, Jean M. [Spectroscopy Forever, 01390 Tramoyes (France)

    2006-03-15

    There are many fields in which the available sample volume is the limiting factor for an elemental analysis. Over the last ten years, sample introduction systems used in plasma spectrometry (i.e., Inductively Coupled Plasma Atomic Emission Spectrometry, ICP-AES, and Mass Spectrometry, ICP-MS) have evolved in order to expand the field of applicability of these techniques to the analysis of micro- and nanosamples. A full understanding of the basic processes occurring throughout the sample introduction system is absolutely necessary to improve analytical performance. The first part of the present review deals with fundamental studies concerning the different phenomena taking place from aerosol production to analyte excitation/ionization when the liquid consumption rate does not exceed 100 {mu}l/min. Existing sample introduction systems are currently far from the ideal and a significant effort has been made to develop new and efficient devices. Different approaches for continuously introducing small sample volumes (i.e., microsamples) have been reviewed and compared in the present work. Finally, applications as well as basic guidelines to select the best sample introduction system according to the sample particularities are given at the end of this review.

  15. 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

  16. Speciation of Selenium in Selenium-Enriched Sunflower Oil by High-Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry/Electrospray-Orbitrap Tandem Mass Spectrometry.

    Science.gov (United States)

    Bierla, Katarzyna; Flis-Borsuk, Anna; Suchocki, Piotr; Szpunar, Joanna; Lobinski, Ryszard

    2016-06-22

    The reaction of sunflower oil with selenite produces a complex mixture of selenitriglycerides with antioxidant and anticancer properties. To obtain insight into the identity and characteristics of the species formed, an analytical approach based on the combination of high-performance liquid chromatography (HPLC) with (78)Se-specific selenium detection by inductively coupled plasma mass spectrometry (ICP MS) and high-resolution (100 000), high mass accuracy (HPLC-ICP MS for the separation of a complex mixture of selenospecies and a mathematical correction of the background signal was developed. The identical chromatographic conditions served for the sample introduction into electrospray MS. Two types of samples were analyzed: sunflower oil dissolved in isopropanol and methanol extract of the oil containing 65% selenium. HPLC-ICP MS showed 14 peaks, 11 of which could also be detected in the methanol extract. Isotopic patterns corresponding to molecules with one or two selenium atoms could be attributed by Orbitrap MS at the retention times corresponding to the HPLC-ICP MS peak apexes. Structural data for these species were acquired by MS(2) and MS(3) fragmentation of protonated or sodiated ions using high-energy collisional dissociation (HCD). A total of 11 selenium-containing triglycerol derivatives resulting from the oxidation of one or two double bonds of linoleic acid and analogous derivatives of glycerol-mixed linoleate(s)/oleinate(s) have been identified for the first time. The presence of these species was confirmed by the targeted analysis in the total oil isopropanol solution. Their identification corroborated the predicted elution order in reversed-phase chromatography: LLL (glycerol trilinoleate), LLO (glycerol dilinoleate-oleinate), LOO (glycerol linoleate-dioleinate), OOO (glycerol trioleinate), of which the extrapolation allowed for the prediction of the identity [glycerol dioleinate-stearate (OOS) and glycerol oleinate-distearate (OSS)] of the

  17. Matrix effects in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Chen, Xiaoshan.

    1995-01-01

    The inductively coupled plasma is an electrodeless discharge in a gas (usually Ar) at atmospheric pressure. Radio frequency energy generated by a RF power source is inductively coupled to the plasma gas through a water cooled load coil. In ICP-MS the open-quotes Fasselclose quotes TAX quartz torch commonly used in emission is mounted horizontally. The sample aerosol is introduced into the central flow, where the gas kinetic temperature is about 5000 K. The aerosol is vaporized, atomized, excited and ionized in the plasma, and the ions are subsequently extracted through two metal apertures (sampler and skimmer) into the mass spectrometer. In ICP-MS, the matrix effects, or non-spectroscopic interferences, can be defined as the type of interferences caused by dissolved concomitant salt ions in the solution. Matrix effects can be divided into two categories: (1) signal drift due to the deposition of solids on the sampling apertures; and/or (2) signal suppression or enhancement by the presence of the dissolved salts. The first category is now reasonably understood. The dissolved salts, especially refractory oxides, tend to deposit on the cool tip of the sampling cone. The clogging of the orifices reduces the ion flow into the ICP-MS, lowers the pressure in the first stage of ICP-MS, and enhances the level of metal oxide ions. Because the extent of the clogging increases with the time, the signal drifts down. Even at the very early stage of the development of ICP-MS, matrix effects had been observed. Houk et al. found out that the ICP-MS was not tolerant to solutions containing significant amounts of dissolved solids

  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. Flow injection on-line dilution for multi-element determination in human urine with detection by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald; Gammelgaard, Bente

    2001-01-01

    A simple flow injection on-line dilution procedure with detection by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of copper, zinc, arsenic, lead, selenium, nickel and molybdenum in human urine. Matrix effects were minimized by employing a dilution factor...

  1. 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)

  2. 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)

  3. Thermal ionisation mass spectrometry (TIMS): what, how and why?

    International Nuclear Information System (INIS)

    Aggarwal, S.K.

    2002-01-01

    Thermal ionisation mass spectrometry (TIMS) is one of the oldest mass spectrometric techniques, which has been used for determining the isotopic composition and concentration of different elements using isotope dilution. In spite of the introduction of many other inorganic mass spectrometric techniques like spark source mass spectrometry (SSMS), glow discharge mass spectrometry (GDMS), inductively coupled plasma-mass spectrometry (ICP-MS), secondary ion mass spectrometry (SIMS), the TIMS technique plays the role of a definitive analytical methodology and still occupies a unique position in terms of its capabilities with respect to precision and accuracy as well as sensitivity

  4. The determination of long life radionuclides by means of sector field ICP mass spectrometry

    International Nuclear Information System (INIS)

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

    1996-01-01

    Different analytical processes for determining long life radionuclides by means of double-focussing sector field ICP mass spectrometry are described. In determining long life radionuclides by means of ICP-MS, on the one hand the analytical problem areas are in the interference of isobaric atom or molecule ions (eg: 151 Eu + - 151 Sm + , 79 Se + - 39 Ar 40 ArH + ) and on the other hand in the high detection limits when using commercial sample introduction systems (eg: For 129 I). An online coupling of HPLC and ICP-MS was built up for the separation of isobaric atom ions and was tested for the separation of isobaric atom ions and was tested for its efficiency in the separation of lanthanides. Special sample introduction systems for ICP-MS were developed for the analysis of 129 I, by which the sensitivity of detection can be appreciably improved compared to commercial sample introduction systems. (orig.) [de

  5. Mass Spectrometry Applications for Toxicology.

    Science.gov (United States)

    Mbughuni, Michael M; Jannetto, Paul J; Langman, Loralie J

    2016-12-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MS n ) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology.

  6. ICP Mass and Optical Emission Spectrometry of Ore Samples Containing Rare Earth Elements

    International Nuclear Information System (INIS)

    Mohammed, A.E.W.M.

    2013-01-01

    Inductively Coupled Plasma Optical Emission and Mass Spectrometry (ICP-OES and ICPMS) are widely accepted as a rapid and sensitive techniques for Rare Earth Elements (REEs) analysis of geological samples. However, the achievable accuracy of these techniques are seriously limited by the problem of matrix interferences. In this study, matrix effects in ICP-AES were addressed using two approaches. In the first approach, the mechanisms of matrix interferences and analyte excitation were elucidated fundamentally. First, matrix effects from a comprehensive list of thirty-nine elements were investigated. It was confirmed that matrix elements with low second (instead of the widely reported first) ionization potentials (IP) produce a stronger matrix effect in all cases. Another critical parameter defining the severity of the matrix effect was found to be the availability of low-lying energy levels in the doubly charged matrix ion. Penning ionization followed by ion electron recombination through successive cycles is proposed as the mechanism for the more severe matrix effects caused by low second-IP matrices. In the second approach ICP-OES and ICP-MS are applied in this study for the analysis of Rare Earth Elements of two selected standard reference samples namely AGV-2 and BCR-2 beside a fluorspar geological sample (G-9 sample). Effective procedures are developed to avoid the spectral interference from matrix elements by using ion exchange resin Amberlite IR-120 before determination of REEs using ICP-OES and ICPMS. The potential of the method is evaluated by analysis of Certified Reference Materials (AGV-2 and BCR-2). Results obtained by ICP-MS show that experimental data are in agreement with the certified values and their values could be used as a quantitative data. The results obtained using ICP-OES were compared and discussed.

  7. Isotopic analysis of calcium in blood plasma and bone from mouse samples by multiple collector-ICP-mass spectrometry

    International Nuclear Information System (INIS)

    Hirata, Takafumi; Tanoshima, Mina; Suga, Akinobu; Tanaka, Yu-ki; Nagata, Yuichi; Shinohara, Atsuko; Chiba, Momoko

    2008-01-01

    The biological processing of Ca produces significant stable isotope fractionation. The level of isotopic fractionation can provide key information about the variation in dietary consumption or Ca metabolism. To investigate this, we measured the 43 Ca/ 42 Ca and 44 Ca/ 42 Ca ratios for bone and blood plasma samples collected from mice of various ages using multiple collector-ICP-mass spectrometry (MC-ICP-MS). The 44 Ca/ 42 Ca ratio in bones was significantly (0.44 - 0.84 per mille) lower than the corresponding ratios in the diet, suggesting that Ca was isotopically fractionated during Ca metabolism for bone formation. The resulting 44 Ca/ 42 Ca ratios for blood plasma showed almost identical, or slightly higher, values (0.03 - 0.2 per mille) than found in a corresponding diet. This indicates that a significant amount of Ca in the blood plasma was from dietary sources. Unlike that discovered for Fe, there were not significant differences in the measured 44 Ca/ 42 Ca ratios between female and male specimens (for either bone or blood plasma samples). Similarity, the 44 Ca/ 42 Ca ratios suggests that there were no significant differences in Ca dietary consumption or Ca metabolism between female and male specimens. In contrast, the 44 Ca/ 42 Ca ratios of blood plasma from mother mice during the lactation period were significantly higher than those for all other adult specimens. This suggests that Ca supplied to infants through lactation was isotopically lighter, and the preferential supply of isotropically lighter Ca resulted in isotopically heavier Ca in blood plasma of mother mice during the lactation period. The data obtained here clearly demonstrate that the Ca isotopic ratio has a potential to become a new tool for evaluating changes in dietary consumption, or Ca metabolism of animals. (author)

  8. Mass Spectrometry Applications for Toxicology

    Science.gov (United States)

    Mbughuni, Michael M.; Jannetto, Paul J.

    2016-01-01

    Toxicology is a multidisciplinary study of poisons, aimed to correlate the quantitative and qualitative relationships between poisons and their physiological and behavioural effects in living systems. Other key aspects of toxicology focus on elucidation of the mechanisms of action of poisons and development of remedies and treatment plans for associated toxic effects. In these endeavours, Mass spectrometry (MS) has become a powerful analytical technique with a wide range of application used in the Toxicological analysis of drugs, poisons, and metabolites of both. To date, MS applications have permeated all fields of toxicology which include; environmental, clinical, and forensic toxicology. While many different analytical applications are used in these fields, MS and its hyphenated applications such as; gas chromatography MS (GC-MS), liquid chromatography MS (LC-MS), inductively coupled plasma ionization MS (ICP-MS), tandem mass spectrometry (MS/MS and MSn) have emerged as powerful tools used in toxicology laboratories. This review will focus on these hyphenated MS technologies and their applications for toxicology. PMID:28149262

  9. 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

  10. 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.)

  11. Method-MS, final report 2010

    DEFF Research Database (Denmark)

    Skipperud, Lindis; Popic, Jelena M.; Roos, Per

    Radiometric determination methods, such as alpha spectrometry require long counting times when low activities are to be determined. Mass spectrometric techniques as Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Thermal Ionisation Mass Spectrometry (TIMS) and Accelerator Mass Spectrometry...

  12. Determination of isotope ratios of metals (and metalloids) by means of inductively coupled plasma-mass spectrometry for provenancing purposes - A review

    International Nuclear Information System (INIS)

    Balcaen, L.; Moens, L.; Vanhaecke, F.

    2010-01-01

    Since considerable time, isotopic analysis of different elements present in a sample, material or object (such as the 'light' elements H, C, N, O and S and 'heavy' elements, such as Sr and Pb), has been used in provenancing studies, as several factors - defined by 'the environment' or origin of the sample - can lead to measurable differences in their isotopic composition. For the light elements, traditionally, (gas source) isotope ratio mass spectrometry (IR-MS) is used, while for a long period of time, thermal ionization mass spectrometry (TIMS) was considered as the only technique capable of detecting subtle variations in the isotopic composition of the 'heavier' elements. However, since the introduction of the first inductively coupled plasma mass spectrometers (ICP-MS), considerable attention has been devoted to the development of methodologies and strategies to perform isotopic analysis by means of ICP-MS. While the relatively modest isotope ratio precision offered by single-collector ICP-MS may already be fit-for-purpose under some circumstances, especially the introduction of multi-collector ICP-MS instruments, equipped with an array of Faraday detectors instead of a single electron multiplier, has lead to tremendous improvements in the field of isotopic analysis. As a result, MC-ICP-MS can be seen as a very strong competitor of TIMS nowadays, while it even provides information on the small isotopic variations shown by some elements, that are not or hardly accessible by means of TIMS (e.g., elements with a high ionization energy). Owing to these new instrumental developments, the application field of isotopic analysis by means of ICP-MS is continuously growing, also in the field of provenance determination. This paper is intended as a review of the developments in and the recent applications of isotopic analysis by means of ICP-MS in this specific research field.

  13. Analysis of Rare Earth Elements in Geologic Samples using Inductively Coupled Plasma Mass Spectrometry; US DOE Topical Report - DOE/NETL-2016/1794

    Energy Technology Data Exchange (ETDEWEB)

    Bank, Tracy L. [AECOM, Pittsburgh, PA (United States); Roth, Elliot A. [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States); Tinker, Phillip [AECOM, Pittsburgh, PA (United States); Granite, Evan [National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States)

    2016-04-17

    Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is used to measure the concentrations of rare earth elements (REE) in certified standard reference materials including shale and coal. The instrument used in this study is a Perkin Elmer Nexion 300D ICP-MS. The goal of the study is to identify sample preparation and operating conditions that optimized recovery of each element of concern. Additionally, the precision and accuracy of the technique are summarized and the drawbacks and limitations of the method are outlined.

  14. THE DEVELOPMENT OF IODINE BASED IMPINGER SOLUTIONS FOR THE EFFICIENT CAPTURE OF HG USING DIRECT INJECTION NEBULIZATION - INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY ANALYSIS

    Science.gov (United States)

    Inductively coupled plasma mass spectrometry (ICP/MS) with direct injection nebulization (DIN) was used to evaluate novel impinger solution compositions capable of capturing elemental mercury (Hgo) in EPA Method 5 type sampling. An iodine based impinger solutoin proved to be ver...

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

    Science.gov (United States)

    Hansen, Matthew N; Clogston, Jeffrey D

    2018-01-01

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

  16. 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)

  17. Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Fe, Cu, Zn and Se in cereals

    Science.gov (United States)

    Huang, Shih-Yi; Jiang, Shiuh-Jen; Sahayam, A. C.

    2014-11-01

    Ultrasonic slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry (USS-ETV-ICP-MS) has been applied to determine Cr, Fe, Cu, Zn and Se in several cereal samples. Thioacetamide was used as the modifier to enhance the ion signals. The background ions at the masses of interest were reduced in intensity significantly by using 1.0 mL min- 1 methane (CH4) as reaction cell gas in the dynamic reaction cell (DRC). Since the sensitivities of Cr, Fe, Cu, Zn and Se in different matrices were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Fe, Cu, Zn and Se in these cereal samples. The method detection limits estimated from standard addition curves were about 1, 10, 4, 12 and 2 ng g- 1 for Cr, Fe, Cu, Zn and Se, respectively, in original cereal samples. This procedure has been applied to the determination of Cr, Fe, Cu, Zn and Se whose concentrations are in μg g- 1 (except Cr and Se) in standard reference materials (SRM) of National institute of standards and technology (NIST), NIST SRM 1568a Rice Flour and NIST SRM 1567a Wheat Flour and two cereal samples purchased from a local market. The analysis results of reference materials agreed with certified values at 95% confidence level according to Student's T-test. The results for the real world cereal samples were also found to be in good agreement with the pneumatic nebulization DRC ICP-MS results of the sample solutions.

  18. 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).

  19. 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

  20. Development of new applications of inductively coupled plasma mass spectrometry (ICP-MS) hyphenated with different sample introduction systems

    OpenAIRE

    Ugarte Baztán, Ana

    2014-01-01

    225 p. : il. Texto en español con conclusiones en inglés Hoy en día, la espectrometría de masas con plasma de acoplamiento inductivo (ICP-MS) es una de las técnicas más potentes y versátiles para el análisis de elementos traza dada su robustez y bajos límites de detección. En el presente trabajo se pretende ampliar el abanico de aplicaciones de esta técnica desarrollando nuevas combinaciones de la misma a distintos sistemas de introducción de muestra. En primera lugar, se presenta el a...

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

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  2. Mapping of lead, magnesium and copper accumulation in plant tissues by laser-induced breakdown spectroscopy and laser-ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Kaiser, J. [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technicka 2896/2, 616 69 Brno (Czech Republic)], E-mail: kaiser@fme.vutbr.cz; Galiova, M.; Novotny, K.; Cervenka, R. [Department of Chemistry, Faculty of Science, Masaryk University, Kotlarska 2, 611 37 Brno (Czech Republic); Reale, L. [Faculty of Sciences, University of L' Aquila, Via Vetoio (Coppito 1), 67010 L' Aquila (Italy); Novotny, J.; Liska, M.; Samek, O. [Institute of Physical Engineering, Faculty of Mechanical Engineering, Brno University of Technology, Technicka 2896/2, 616 69 Brno (Czech Republic); Kanicky, V.; Hrdlicka, A. [Department of Chemistry, Faculty of Science, Masaryk University, Kotlarska 2, 611 37 Brno (Czech Republic); Stejskal, K.; Adam, V.; Kizek, R. [Department of Chemistry and Biochemistry, Faculty of Agronomy, Mendel University of Agriculture and Forestry, Zemedelska 1, 613 00 Brno (Czech Republic)

    2009-01-15

    Laser-Induced Breakdown Spectroscopy (LIBS) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) were utilized for mapping the accumulation of Pb, Mg and Cu with a resolution up to 200 {mu}m in a up to cm x cm area of sunflower (Helianthus annuus L.) leaves. The results obtained by LIBS and LA-ICP-MS are compared with the outcomes from Atomic Absorption Spectrometry (AAS) and Thin-Layer Chromatography (TLC). It is shown that laser-ablation based analytical methods can substitute or supplement these techniques mainly in the cases when a fast multi-elemental mapping of a large sample area is needed.

  3. Study of plasma parameters influencing fractionation in laser ablation-inductively coupled plasma-mass spectrometry

    Science.gov (United States)

    Gäckle, M.; Merten, D.

    2010-12-01

    Methods permitting to test the influence of the matrix as well as of its local and temporal distribution on the plasma conditions in laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) are developed. For this purpose, the MS interface is used as plasma probe allowing to investigate the average plasma condition within the ICP zone observed in terms of temporal and spatial distribution of the matrix. Inserted matrix particles, particularly when being atomized and ionized, can cause considerable changes in both electron density and plasma temperature thus influencing the ionization equilibrium of the individual analytes. In this context, the plasma probe covers a region of the plasma for which no local thermodynamic equilibrium can be assumed. The differences in temperature, identified within the region of the plasma observed, amounted up to 3000 K. While in the central region conditions were detected that would not allow efficient atomization and ionization of the matrix, these conditions improve considerably towards the margin of the area observed. Depending on the nature as well as on the temporally and locally variable density of the matrix, this can lead to varying intensity ratios of the analytes and explain fractionation effects. By means of a derived equation it is shown that the deviation of the intensity ratio from the concentration ratio turns out to be more serious the higher the difference of the ionization potential of the analytes observed, the lower the plasma temperature and the higher the matrix concentration within the area observed.

  4. 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

  5. Gas chromatography/plasma spectrometry - an important analytical tool for elemental speciation studies

    International Nuclear Information System (INIS)

    Wuilloud, Jorgelina C.A.; Wuilloud, Rodolfo G.; Vonderheide, Anne P.; Caruso, Joseph A.

    2004-01-01

    In this review, a full discussion and update of the state-of-the-art of gas chromatography (GC) coupled to all known plasma spectrometers is presented. A brief introductive discussion of the advantages and disadvantages of GC-plasma interfaces, as well as types of plasmas and mass spectrometers, is given. The plasma-based techniques covered include inductively coupled plasma mass spectrometry (ICP-MS) microwave-induced plasma optical emission spectrometry (MIP-OES), and inductively coupled plasma optical emission spectrometry (ICP-OES). Also, different variants of plasma sources, such as low power plasmas and glow discharge (GD) sources, are described and compared with respect to their capabilities in elemental speciation. Recent advances and alternative mass analyzers (collision/reaction cell; time-of-flight; double-focusing sector field) are also mentioned. Different aspects of the GC-plasma coupling are discussed with particular attention to the applications of these hyphenated techniques to the analysis of elemental species. Additionally, classical and modern sample preparation methods, including extraction and/or preconcentration and derivatization reactions, are presented and evaluated

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

    International Nuclear Information System (INIS)

    Ohno, Takeshi; Muramatsu, Yasuyuki

    2015-01-01

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

  7. Arsenic speciation in soil using high performance liquid chromatography/inductively coupled plasma/mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Bass, D.A.; Yaeger, J.S.; Parish, K.J.; Crain, J.S.; Kiely, J.T.; Gowdy, M.J. [Argonne National Lab., IL (United States); Mohrman, G.B.; Besmer, M.G. [Rocky Mountain Arsenal, Commerce City, CO (United States)

    1996-08-01

    A method has been developed to identify and quantify As(III), As(V), and organoarsenic compounds in soil samples from the Rocky Mountain Arsenal (RMA) by high performance liquid chromatography/inductively coupled plasma/mass spectrometry (HPLC/ICP/MS). The soils were extracted using tetrabutylammonium hydroxide (TBAH) and sonication. The percentages of As(III), As(V), and organoarsenic species extracted from soil samples were 30, 50, and 100 respectively. The arsenic species were not altered during the extraction process. They were separated by reversed-phase, ion-pairing, HPLC using a microbore Inertsil-ODS{trademark} column. The HPLC column effluent was introduced into an ICP/MS system using a direct injection nebulizer (DIN). Detection limits of less than 1 pg were readily obtained for each arsenic species. Internal standards are recommended to increase accuracy and precision. Soil samples spiked with arsenic oxide, sodium arsenate, dimethylarsinic acid (DMAA), and chlorovinyl arsenious acid (CVAA) were extracted, identified and quantified with the HPLC/ICP/MS system. The soil samples were analyzed in support of the analytical needs of a thermal desorption treatability study being conducted at the RMA.

  8. Establishment of methodology for determination of {sup 93}Zr in radioactive wastes by Liquid Scintillation Counting (LSC) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS); Estabelecimento de metodologia para determinacao de {sup 93}Zr em rejeitos radioativos por Espectrometria de Cintilacao Liquida (LSC) e Espectrometria de Massa com Plasma Indutivamente Acoplado (ICP-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Thiago Cesar de

    2014-06-01

    The zirconium-93 is a long-lived pure β-particle-emitting radionuclide produced from {sup 235}U fission and from neutron activation of the stable isotope {sup 92}Zr and thus occurring as one of the radionuclides found in nuclear reactors. Due to its long half life, {sup 93}Zr is one of the radionuclides of interest for the performance of assessment studies of waste storage or disposal. Measurement of {sup 93}Zr is difficult owing to its trace level concentration and its low activity in nuclear wastes and further because its certified standards are not frequently available. The aim of this work was to develop a selective radiochemical separation methodology for the determination of {sup 93}Zr in nuclear waste and analyze it by Liquid Scintillation Counting (LSC) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS). To set up the radiochemical separation procedure for zirconium, a tracer solution of {sup 95}Zr and its 724 keV γ-ray measurements by γ- spectrometry were used in order to follow the behavior of zirconium during the radiochemical separation. For the LSC technique a {sup 55}Fe solution, which is one of the major interfering measures zirconium, was used to verify the decontamination factor during the separation process. The efficiency detection for {sup 63}Ni was used to determination of {sup 93}Zr activity in the matrices analyzed. The limit of detection of the 0.05 Bq 1{sup −1} was obtained for {sup 63}Ni standard solutions by using a sample:cocktail ratio of 3:17 mL for Optiphase Hisafe 3 cocktail. For the ICP-MS technique a zirconium stable solution was used to verify the zirconium behavior and recovery during radiochemical separation and a solution of Ba, Co, Eu, Fe, Mn, Nb, Sr and Y was used to verify the decontamination factor during the separation process. A standard solution {sup 93}Nb as isotope for determining the {sup 93}Zr by ICP-MS was used for calibration and analysis. The detection limit of 0.039 ppb was obtained for the standard

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

    Science.gov (United States)

    Jantzi, Sarah C; Almirall, José R

    2014-01-01

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

  10. Comparison of inductively coupled plasma mass spectrometry with inductively coupled plasma atomic emission spectrometry and instrumental neutron activation analysis for the determination of rare earth elements in Greek bauxites

    International Nuclear Information System (INIS)

    Ochsenkuehn-Petropoulou, Maria; Luck, Joachim

    1991-01-01

    Fore the determination of rare earth elements (REE) in bauxitic materials the techniques of inductively coupled plasma mass spectrometry (ICP-MS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and instrumental neutron activation analysis (INAA) were compared. In the NIST (National Institute of Standards and Technology) bauxites SRM 697 Dominican, and SRM 69 b Arkansas, the concentration of some REEs were determined. With the reference bauxite BX-N of the ARNT (Association Nationale de la Recherche Technique) the precision and accuracy of ICP-AES for the determination of REEs in bauxites was tested. Furthermore, Greek bauxites of the Parnassos-Giona area were investigated. In a comparison of the three methods it was possible to calculate from the data series the precision of each method, which showed that the tendency found in the deviations for the different REEs is in accordance with published values. Also the limits of detection for REEs in bauxites were calculated and found to be in the same range as those in the literature. (author)

  11. 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.

  12. Determination of selenoprotein P in human plasma by solid phase extraction and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Bendahl, L.; Sidenius, U.; Gammelgaard, Bente

    2000-01-01

    measured by inductively coupled plasma mass spectrometry (ICP-MS) monitoring the Se-82 isotope. Linear response was observed in the concentration range 0.3-70.8 mu g/l selenium as selenoprotein P with a correlation coefficient of 0.9994. The precision expressed as relative standard deviation was better...... than 2% in this range. The estimated limit of detection was 2 mu g/l and the experimentally verified quantification limit was 5 mu g/l, giving a relative standard deviation less than 2%. (C) 2000 Elsevier Science B.V. All rights reserved...

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

    OpenAIRE

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

    2016-01-01

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

  14. Validation of methods to measure uranium isotopes using magnetic sector mass spectrometry with inductively coupled plasma source

    International Nuclear Information System (INIS)

    Hernandez M, H.; Rios L, M. J.; Romero G, E. T.

    2017-10-01

    The mass spectrometry technique with inductively coupled plasma source (Icp-Ms) has been widely used to measure isotopic ratios of elements toxic to human health. Reason for which, in this work several measurement methods for the analysis of uranium isotopes in different matrices were implemented using magnetic sector mass spectrometry with inductively coupled plasma source (Icp-SFMS). Groundwater, sediment, soil and urine were the matrices analyzed, which were supplied by intercomparison tests conducted by the IAEA and Association for the Promotion of Quality Control of Medical Biology Analysis in Radio-toxicology. The procedures used in the treatment of soil, sediment and water samples were based on US EPA methods. In the case of the urine sample, the preparation was rapid (1:20 dilution). The average of the results obtained in yield of each matrix was 94, 71, 72 and 78% for water, urine, soil and sediment respectively. In addition, the precision in terms of standard relative deviation was less than 5% and the accuracy was less than 4%. In conclusion, the Icp-SFMS is a very sensitive technique for measuring isotopes of U in different matrices. However, careful tuning is necessary, especially in the mass regions of interest 234, 235 and 238 if an external quantification is considered using natural U solutions. (Author)

  15. Laser ablation inductively coupled plasma mass spectrometry. An alternative technique for monitoring 90Sr

    International Nuclear Information System (INIS)

    TsingHai Wang; Yan-Chen Lai; Yi-Kong Hsieh; Chu-Fang Wang

    2017-01-01

    Developing a rapid detection method for monitoring released 90 Sr remains a challenge to analytical chemists, particularly considering its low concentration and significant interferences in environmental samples. We proposed a concept as an alternative to detect 90 Sr on the surface of fish scales using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The high affinity of fish scales to Sr is capable of preconcentrating 90 Sr that minimizes isobaric interferences from 90 Zr + or 89 YH + , while tailing effect by abundant 88 Sr can be effectively reduced by adjusting the forward power of ICP-MS component. Adopting dried droplets of internal standards further allows a semiquantification of 90 Sr content on the surface of fish scales, which also arises an opportunity to monitoring the bioaccumulation of 90 Sr after Fukushima Daiichi nuclear disaster. (author)

  16. 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.

  17. 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

  18. Application of laser ablation-ICP-MS to determine high-resolution elemental profiles across the Cretaceous/Paleogene boundary at Agost (Spain)

    NARCIS (Netherlands)

    Sosa-Montes de Oca, Claudia; de Lange, Gert J.|info:eu-repo/dai/nl/073930962; Martínez-Ruiz, Francisca; Rodríguez-Tovar, Francisco J.

    2018-01-01

    A high-resolution analysis of the distribution of major and trace elements across a Cretaceous/Paleogene boundary (KPgB) was done using Laser Ablation-Inductivity Coupled Plasma-Mass Spectrometry (LA-ICP-MS) and was compared with traditional distinct sampling and analysis. At the Agost site (SE

  19. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part I. Theoretical considerations

    Energy Technology Data Exchange (ETDEWEB)

    Leclercq, Amélie, E-mail: amelie.leclercq@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Nonell, Anthony, E-mail: anthony.nonell@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Todolí Torró, José Luis, E-mail: jose.todoli@ua.es [Universidad de Alicante, Departamento de Quimica Analitica, Nutricion y Bromatología, Ap. de Correos, 99, 03080 Alicante (Spain); Bresson, Carole, E-mail: carole.bresson@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vio, Laurent, E-mail: laurent.vio@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vercouter, Thomas, E-mail: thomas.vercouter@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Chartier, Frédéric, E-mail: frederic.chartier@cea.fr [CEA Saclay, DEN, DANS, DPC, 91191 Gif-sur-Yvette (France)

    2015-07-23

    Highlights: • Tutorial review addressed to beginners or more experienced analysts. • Theoretical background of effects caused by organic matrices on ICP techniques. • Spatial distribution of carbon species and analytes in plasma. • Carbon spectroscopic and non-spectroscopic interferences in ICP. - Abstract: Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical “matrix removal” approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the

  20. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part I. Theoretical considerations

    International Nuclear Information System (INIS)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-01-01

    Highlights: • Tutorial review addressed to beginners or more experienced analysts. • Theoretical background of effects caused by organic matrices on ICP techniques. • Spatial distribution of carbon species and analytes in plasma. • Carbon spectroscopic and non-spectroscopic interferences in ICP. - Abstract: Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical “matrix removal” approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the

  1. 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.

  2. 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

  3. Direct determination of cadmium in foods by solid sampling electrothermal vaporization inductively coupled plasma mass spectrometry using a tungsten coil trap

    Science.gov (United States)

    Zhang, Ying; Mao, Xuefei; Liu, Jixin; Wang, Min; Qian, Yongzhong; Gao, Chengling; Qi, Yuehan

    2016-04-01

    In this work, a solid sampling device consisting of a tungsten coil trap, porous carbon vaporizer and on-line ashing furnace of a Ni-Cr coil was interfaced with inductively coupled plasma mass spectrometry (ICP-MS). A modified double gas circuit system was employed that was composed of carrier and supplemental gas lines controlled by separate gas mass flow controllers. For Cd determination in food samples using the assembled solid sampling ICP-MS, the optimal ashing and vaporization conditions, flow rate of the argon-hydrogen (Ar/H2) (v:v = 24:1) carrier gas and supplemental gas, and minimum sampling mass were investigated. Under the optimized conditions, the limit of quantification was 0.5 pg and the relative standard deviation was within a 10.0% error range (n = 10). Furthermore, the mean spiked recoveries for various food samples were 99.4%-105.9% (n = 6). The Cd concentrations measured by the proposed method were all within the certified values of the reference materials or were not significantly different (P > 0.05) from those of the microwave digestion ICP-MS method, demonstrating the good accuracy and precision of the solid sampling ICP-MS method for Cd determination in food samples.

  4. Exploration of robust operating conditions in inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Tromp, John W.; Pomares, Mario; Alvarez-Prieto, Manuel; Cole, Amanda; Ying Hai; Salin, Eric D.

    2003-01-01

    'Robust' conditions, as defined by Mermet and co-workers for inductively coupled plasma (ICP)-atomic emission spectrometry, minimize matrix effects on analyte signals, and are obtained by increasing power and reducing nebulizer gas flow. In ICP-mass spectrometry (MS), it is known that reduced nebulizer gas flow usually leads to more robust conditions such that matrix effects are reduced. In this work, robust conditions for ICP-MS have been determined by optimizing for accuracy in the determination of analytes in a multi-element solution with various interferents (Al, Ba, Cs, K, Na), by varying power, nebulizer gas flow, sample introduction rate and ion lens voltage. The goal of the work was to determine which operating parameters were the most important in reducing matrix effects, and whether different interferents yielded the same robust conditions. Reduction in nebulizer gas flow and in sample input rate led to a significantly decreased interference, while an increase in power seemed to have a lesser effect. Once the other parameters had been adjusted to their robust values, there was no additional improvement in accuracy attainable by adjusting the ion lens voltage. The robust conditions were universal, since, for all the interferents and analytes studied, the optimum was found at the same operating conditions. One drawback to the use of robust conditions was the slightly reduced sensitivity; however, in the context of 'intelligent' instruments, the concept of 'robust conditions' is useful in many cases

  5. 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)

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

    International Nuclear Information System (INIS)

    Pedreira Filho, Walter dos Reis

    2000-01-01

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

  7. 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

  8. Speciation of arsenic in marine food (Anemonia sulcata) by liquid chromatography coupled to inductively coupled plasma mass spectrometry and organic mass spectrometry.

    Science.gov (United States)

    Contreras-Acuña, M; García-Barrera, T; García-Sevillano, M A; Gómez-Ariza, J L

    2013-03-22

    Arsenic species have been investigated in Anemonia sulcata, which is frequently consumed food staple in Spain battered in wheat flour and fried with olive oil. Speciation in tissue extracts was carried out by anion/cation exchange chromatography with inductively coupled plasma mass spectrometry (HPLC-(AEC/CEC)-ICP-MS). Three methods for the extraction of arsenic species were investigated (ultrasonic bath, ultrasonic probe and focused microwave) and the optimal one was applied. Arsenic speciation was carried out in raw and cooked anemone and the dominant species are dimethylarsinic acid (DMA(V)) followed by arsenobetaine (AB), As(V), monomethylarsonic acid (MA(V)), tetramethylarsonium ion (TETRA) and trimethylarsine oxide (TMAO). In addition, arsenocholine (AsC), glyceryl phosphorylarsenocholine (GPAsC) and dimethylarsinothioic acid (DMAS) were identified by liquid chromatography coupled to triple quadrupole mass spectrometry (HPLC-MS). These results are interesting since GPAsC has been previously reported in marine organisms after experimental exposure to AsC, but not in natural samples. In addition, this paper reports for the first time the identification of DMAS in marine food. Copyright © 2013 Elsevier B.V. All rights reserved.

  9. Ultra-Sensitive Elemental Analysis Using Plasmas 4.Application of Inductively Coupled Plasma Mass Spectrometry to the Study of Environmental Radioactivity

    Science.gov (United States)

    Yoshida, Satoshi

    Applications of inductively coupled plasma mass spectrometry (ICP-MS) to the determination of long-lived radionuclides in environmental samples were summarized. In order to predict the long-term behavior of the radionuclides, related stable elements were also determined. Compared with radioactivity measurements, the ICP-MS method has advantages in terms of its simple analytical procedures, prompt measurement time, and capability of determining the isotope ratio such as240Pu/239Pu, which can not be separated by radiation. Concentration of U and Th in Japanese surface soils were determined in order to determine the background level of the natural radionuclides. The 235U/238U ratio was successfully used to detect the release of enriched U from reconversion facilities to the environment and to understand the source term. The 240Pu/239Pu ratios in environmental samples varied widely depending on the Pu sources. Applications of ICP-MS to the measurement of I and Tc isotopes were also described. The ratio between radiocesium and stable Cs is useful for judging the equilibrium of deposited radiocesium in a forest ecosystem.

  10. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part I. Theoretical considerations.

    Science.gov (United States)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-07-23

    Due to their outstanding analytical performances, inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are widely used for multi-elemental measurements and also for isotopic characterization in the case of ICP-MS. While most studies are carried out in aqueous matrices, applications involving organic/hydro-organic matrices become increasingly widespread. This kind of matrices is introduced in ICP based instruments when classical "matrix removal" approaches such as acid digestion or extraction procedures cannot be implemented. Due to the physico-chemical properties of organic/hydro-organic matrices and their associated effects on instrumentation and analytical performances, their introduction into ICP sources is particularly challenging and has become a full topic. In this framework, numerous theoretical and phenomenological studies of these effects have been performed in the past, mainly by ICP-OES, while recent literature is more focused on applications and associated instrumental developments. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP-OES and ICP-MS. The present Part I, provides theoretical considerations in connection with the physico-chemical properties of organic/hydro-organic matrices, in order to better understand the induced phenomena. This focal point is divided in four chapters highlighting: (i) the impact of organic/hydro-organic matrices from aerosol generation to atomization/excitation/ionization processes; (ii) the production of carbon molecular constituents and their spatial distribution in the plasma with respect to analytes repartition; (iii) the subsequent modifications of plasma fundamental properties; and (iv) the resulting spectroscopic and non spectroscopic interferences. This first part of this tutorial review is addressed either to beginners or to more experienced scientists who are interested in the

  11. 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.

  12. The potential of using laser ablation inductively coupled plasma time of flight mass spectrometry (LA-ICP-TOF-MS) in the forensic analysis of micro debris.

    Science.gov (United States)

    Scadding, Cameron J; Watling, R John; Thomas, Allen G

    2005-08-15

    The majority of crimes result in the generation of some form of physical evidence, which is available for collection by crime scene investigators or police. However, this debris is often limited in amount as modern criminals become more aware of its potential value to forensic scientists. The requirement to obtain robust evidence from increasingly smaller sized samples has required refinement and modification of old analytical techniques and the development of new ones. This paper describes a new method for the analysis of oxy-acetylene debris, left behind at a crime scene, and the establishment of its co-provenance with single particles of equivalent debris found on the clothing of persons of interest (POI). The ability to rapidly determine and match the elemental distribution patterns of debris collected from crime scenes to those recovered from persons of interest is essential in ensuring successful prosecution. Traditionally, relatively large amounts of sample (up to several milligrams) have been required to obtain a reliable elemental fingerprint of this type of material [R.J. Walting , B.F. Lynch, D. Herring, J. Anal. At. Spectrom. 12 (1997) 195]. However, this quantity of material is unlikely to be recovered from a POI. This paper describes the development and application of laser ablation inductively coupled plasma time of flight mass spectrometry (LA-ICP-TOF-MS), as an analytical protocol, which can be applied more appropriately to the analysis of micro-debris than conventional quadrupole based mass spectrometry. The resulting data, for debris as small as 70mum in diameter, was unambiguously matched between a single spherule recovered from a POI and a spherule recovered from the scene of crime, in an analytical procedure taking less than 5min.

  13. Study of the matrix specific mass discrimination effects during inductively coupled plasma mass spectrometry isotope ratio measurements

    International Nuclear Information System (INIS)

    Vassileva, E.; Quetel, Ch.R.

    2004-01-01

    Sample matrix related effects on mass discrimination during inductively coupled plasma mass spectrometry (ICP-MS) isotope ratio measurements have only been rarely reported. However, they can lead to errors larger than the uncertainty claimed on the ratio results when not properly taken into account or corrected for. These matrix specific affects were experienced during an Isotope Dilution Mass Spectrometry (IDMS) campaign we carried out for the certification of the Cd amount content in some food digest samples (7% acidity and salts content around 450μg g -1 ). Dilution was not possible for Cd only present at the low ng g -1 level. Up to 1% difference was observed on Cd isotope ratio results between measurements performed directly or after matrix separation. This was a significant difference considering that less than 1.5% relative combined uncertainty was eventually estimated for these IDMS measurements. Similar results could be obtained either way after the implementation of necessary corrections. The direct measurement approach associated to a correction for mass discrimination effects using the food digest sample itself (and the IUPAC table values as reference for the natural Cd isotopic composition) was preferred as it was the easiest. Consequently, the impact of matrix effects on mass discrimination during isotope ratio measurements with two types of ICP- MS (quadrupole and magnetic sector instruments) was studied for 4 elements (Li, Cu, Cd and Tl). Samples of varying salinity (up to 0.25%) and acidity (up to 7%) characteristics were prepared using isotopic certified reference materials of these elements. The long term and short-term stability, respectively reproducibility and repeatability, of the results, as well as the evolution of the difference to certified ratio values were monitored. As expected the 13 investigated isotopic ratios were all sensitive to variations in salt and acid concentrations. Our experiments also showed that simultaneous variation

  14. 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.

  15. Validation of the determination of the B isotopic composition in Roman glasses with laser ablation multi-collector inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Devulder, Veerle [Department of Analytical Chemistry, Ghent University, Krijgslaan 281-S12, 9000 Ghent (Belgium); Department of Earth and Environmental Sciences, Katholieke Universiteit Leuven, Celestijnenlaan 200 E-box 2408, 3001 Leuven (Belgium); Gerdes, Axel [Institute of Geoscience, Goethe Universität, Altenhoeferallee 1, 60438 Frankfurt am Main (Germany); Vanhaecke, Frank, E-mail: Frank.Vanhaecke@UGent.be [Department of Analytical Chemistry, Ghent University, Krijgslaan 281-S12, 9000 Ghent (Belgium); Degryse, Patrick [Department of Earth and Environmental Sciences, Katholieke Universiteit Leuven, Celestijnenlaan 200 E-box 2408, 3001 Leuven (Belgium)

    2015-03-01

    The applicability of laser ablation multi-collector inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS) for the determination of the B isotopic composition in Roman glasses was investigated. The δ{sup 11}B values thus obtained provide information on the natron flux used during the glass-making process. The glass samples used for this purpose were previously characterized using pneumatic nebulization (PN) MC-ICP-MS. Unfortunately, this method is time-consuming and labor-intensive and consumes some 100 mg of sample, which is a rather high amount for ancient materials. Therefore, the use of the less invasive and faster LA-MC-ICP-MS approach was explored. In this work, the results for 29 Roman glasses and 4 home-made glasses obtained using both techniques were compared to assess the suitability of LA-MC-ICP-MS in this context. The results are in excellent agreement within experimental uncertainty. No difference in overall mass discrimination was observed between the Roman glasses, NIST SRM 610 reference glass and B6 obsidian. The expanded uncertainty of the LA-MC-ICP-MS approach was estimated to be < 2‰, which is similar to that obtained upon sample digestion and PN-MC-ICP-MS measurement. - Highlights: • First use of LA-MC-ICP-MS for B isotopic analysis of ancient glass • Careful validation of LA-MC-ICP-MS approach • Similar precision & accuracy via solution MC-ICP-MS after isolation of B • Enhancement of sample throughput & reduction of sample consumption • Improved conditions for archeometric research on (pre-)Roman glass.

  16. Validation of the determination of the B isotopic composition in Roman glasses with laser ablation multi-collector inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Devulder, Veerle; Gerdes, Axel; Vanhaecke, Frank; Degryse, Patrick

    2015-01-01

    The applicability of laser ablation multi-collector inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS) for the determination of the B isotopic composition in Roman glasses was investigated. The δ 11 B values thus obtained provide information on the natron flux used during the glass-making process. The glass samples used for this purpose were previously characterized using pneumatic nebulization (PN) MC-ICP-MS. Unfortunately, this method is time-consuming and labor-intensive and consumes some 100 mg of sample, which is a rather high amount for ancient materials. Therefore, the use of the less invasive and faster LA-MC-ICP-MS approach was explored. In this work, the results for 29 Roman glasses and 4 home-made glasses obtained using both techniques were compared to assess the suitability of LA-MC-ICP-MS in this context. The results are in excellent agreement within experimental uncertainty. No difference in overall mass discrimination was observed between the Roman glasses, NIST SRM 610 reference glass and B6 obsidian. The expanded uncertainty of the LA-MC-ICP-MS approach was estimated to be < 2‰, which is similar to that obtained upon sample digestion and PN-MC-ICP-MS measurement. - Highlights: • First use of LA-MC-ICP-MS for B isotopic analysis of ancient glass • Careful validation of LA-MC-ICP-MS approach • Similar precision & accuracy via solution MC-ICP-MS after isolation of B • Enhancement of sample throughput & reduction of sample consumption • Improved conditions for archeometric research on (pre-)Roman glass

  17. Detection of counterfeit antiviral drug Heptodin and classification of counterfeits using isotope amount ratio measurements by multicollector inductively coupled plasma mass spectrometry (MC-ICPMS) and isotope ratio mass spectrometry (IRMS).

    Science.gov (United States)

    Santamaria-Fernandez, Rebeca; Hearn, Ruth; Wolff, Jean-Claude

    2009-06-01

    Isotope ratio mass spectrometry (IRMS) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) are highly important techniques that can provide forensic evidence that otherwise would not be available. MC-ICP-MS has proved to be a very powerful tool for measuring high precision and accuracy isotope amount ratios. In this work, the potential of combining isotope amount ratio measurements performed by MC-ICP-MS and IRMS for the detection of counterfeit pharmaceutical tablets has been investigated. An extensive study for the antiviral drug Heptodin has been performed for several isotopic ratios combining MC-ICP-MS and an elemental analyser EA-IRMS for stable isotope amount ratio measurements. The study has been carried out for 139 batches of the antiviral drug and analyses have been performed for C, S, N and Mg isotope ratios. Authenticity ranges have been obtained for each isotopic system and combined to generate a unique multi-isotopic pattern only present in the genuine tablets. Counterfeit tablets have then been identified as those tablets with an isotopic fingerprint outside the genuine isotopic range. The combination of those two techniques has therefore great potential for pharmaceutical counterfeit detection. A much greater power of discrimination is obtained when at least three isotopic systems are combined. The data from these studies could be presented as evidence in court and therefore methods need to be validated to support their credibility. It is also crucial to be able to produce uncertainty values associated to the isotope amount ratio measurements so that significant differences can be identified and the genuineness of a sample can be assessed.

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

    Science.gov (United States)

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

    2017-12-18

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

  19. Plutonium determination in seawater by inductively coupled plasma mass spectrometry: A review.

    Science.gov (United States)

    Cao, Liguo; Bu, Wenting; Zheng, Jian; Pan, Shaoming; Wang, Zhongtang; Uchida, Shigeo

    2016-05-01

    Knowing the concentration and isotopic ratio of Pu in seawater is of critical importance for assessing Pu contamination and investigating oceanic processes. In recent decades, the concentration of (239+240)Pu in seawater, particularly for surface seawater, has presented an exponential decreasing trend with time; thus determination of Pu in seawater has become a challenge nowadays. Here, we have summarized and critically discussed a variety of reported analytical methods for Pu determination in seawater sample based on inductively coupled plasma mass spectrometry (ICP-MS) analytical technique for rapid ultra-trace detection of Pu. Generally, pretreatments for seawater sample include co-precipitation, valence adjustment and chemical separation and purification procedures, all of which are comprehensively reviewed. Overall, the selected anion-exchange, extraction resins and operation condition are important for decontamination of interference from matrix elements and achieving satisfactory chemical yields. In addition, other mass spectrometric and radiometric detections are briefly addressed and compared with the focus on assessing ICP-MS. Finally, we discuss some issues and prospects in determination and application of Pu isotopes in seawater samples for future research. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2018-01-01

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

  1. Trace and surface analysis of ceramic layers of solid oxide fuel cells by mass spectrometry.

    Science.gov (United States)

    Becker, J S; Breuer, U; Westheide, J; Saprykin, A I; Holzbrecher, H; Nickel, H; Dietze, H J

    1996-06-01

    For the trace analysis of impurities in thick ceramic layers of a solid oxide fuel cell (SOFC) sensitive solid-state mass spectrometric methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and radiofrequency glow discharge mass spectrometry (rf-GDMS) have been developed and used. In order to quantify the analytical results of LA-ICP-MS, the relative sensitivity coefficients of elements in a La(0.6)Sr(0.35)MnO(3) matrix have been determined using synthetic standards. Secondary ion mass spectrometry (SIMS) - as a surface analytical method - has been used to characterize the element distribution and diffusion profiles of matrix elements on the interface of a perovskite/Y-stabilized ZrO(2) layer. The application of different mass spectrometric methods for process control in the preparation of ceramic layers for the SOFC is described.

  2. Contribution to the development of new analytical methods by the coupling between capillary electrophoresis and mass spectrometry (ICP-MS and ESI-MS): applications to the nuclear and biological fields; Contribution au developpement de nouvelles methodes analytiques par le couplage entre l'electrophorese capillaire et la spectrometrie de masse (ICP-MS et ESI-MS): applications dans les domaines nucleaires et biologiques

    Energy Technology Data Exchange (ETDEWEB)

    Pitois, A

    2006-04-15

    The coupling between chromatographic and electrophoretic separation techniques and mass spectrometry is used to combine the efficiency of the separation technique to the selectivity and sensitivity of the detectors. In this work, the number of applications of the CE-MS couplings has been increased. New analytical methods have been set up in the nuclear and biological fields. New analytical methods for the determination of fission products (cesium and lanthanides) have been developed by CE-ICP-MS. They enable to determine both concentration and isotopic composition of the fission products for very low detection limits (ng/mL by CE-Q-ICPMS, pg/mL by CE-HR-ICP-MS), since all the isobaric interferences are resolved. Moreover, only some nano-liters of sample are necessary to perform the analysis. These method have been applied with success to a simulated sample of spent fuel, to a nuclear sample from PUREX process and to a leaching of MOX fuel. Then, lanthanides have been analysed by CE-ESI-MS and the capability of ESI-MS to provide structural information has been studied. Elementary information has been obtained for strong potentials. Structural information has been obtained for low potentials. Finally, a new analytical method by CE-ESI-MS for the determination of 10B-boronophenylalanine (10B-BPA) has been developed for Boron Neutron Capture Therapy (BNCT). It has been applied to the cellular lines F98 and HUVEC. This CE-ESI-MS method has been validated by HR-ICP-MS. It enables a direct quantification of the chemical form 10B-BPA in samples of limited size (some nano-liters) and for low concentrations (ng/mL). As a consequence, this CE-ESI-MS method has enabled the study of the kinetics of 10B-BPA release and uptake for the F98 cells. (author)

  3. Quantitative images of metals in plant tissues measured by laser ablation inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Becker, J.S.; Dietrich, R.C.; Matusch, A.; Pozebon, D.; Dressler, V.L.

    2008-01-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was used for quantitative imaging of toxic and essential elements in thin sections (thickness of 30 or 40 μm) of tobacco plant tissues. Two-dimensional images of Mg, Fe, Mn, Zn, Cu, Cd, Rh, Pt and Pb in leaves, shoots and roots of tobacco were produced. Sections of the plant tissues (fixed onto glass slides) were scanned by a focused beam of a Nd:YAG laser in a laser ablation chamber. The ablated material was transported with argon as carrier gas to the ICP ion source at a quadrupole ICP-MS instrument. Ion intensities of the investigated elements were measured together with 13 C + , 33 S + and 34 S + within the entire plant tissue section. Matrix matching standards (prepared using powder of dried tobacco leaves) were used to constitute calibration curves, whereas the regression coefficient of the attained calibration curves was typically 0.99. The variability of LA-ICP-MS process, sample heterogeneity and water content in the sample were corrected by using 13 C + as internal standard. Quantitative imaging of the selected elements revealed their inhomogeneous distribution in leaves, shoots and roots

  4. Trace Analysis of Irradiated Granite Samples from Hiroshima by Laser Ablation Inductively Coupled Plasma Mass Spectrometry

    International Nuclear Information System (INIS)

    Amr, M.A.; Helal, N.F.; Zahran, N.F.; Becker, J.S.; Pickhardt, C.; Dietze, H.J.

    1999-01-01

    Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is widely accepted as a rapid and sensitive technique for trace elemental analysis of solid materials and for local analysis of inhomogeneous materials (such as geological samples). Due to its direct solid sample analysis capability, LA-ICP-MS (using a quadrupole based ICP-MS and at the Research Center Juelich developed laser ablation system: Nd-YAG-laser, 226 nm, 10 Hz and 5 ns) is applied for the analysis of geological (granite) samples from Hiroshima. In order to prepare homogeneous targets, these samples were melted together with a lithium-borate mixture in a muffle furnace at 1050 degree c. Furthermore, for investigating of matrix effects the powder of these samples is mixed with graphite and pressed as targets for laser ablation. The quantification of the analysis results was carried out using granite (GM) as standard reference material. The relative sensitivity coefficients (RSCs) for most elements, which were determined for correction of the measured values, varied between 0.3 and 3

  5. Determination of the platinum - group elements (PGE) and gold (Au) in the manganese nodule reference samples by nickel sulfide fire-assay and Te coprecipitation with ICP-MS

    Digital Repository Service at National Institute of Oceanography (India)

    Balaram, V.; Mathur, R.; Banakar, V.K.; Hein, J.R.; Rao, C.R.M.; Rao, T.G.; Dasaram, B.

    Platinum group elements (PGE) and Au data in polymetallic oceanic ferromanganese nodule reference samples and crust samples obtained by inductively coupled plasma mass spectrometry (ICP-MS), after separation and pre-concentration by nickel sulfide...

  6. Determination of chromium, iron and selenium in foodstuffs of animal origin by collision cell technology, inductively coupled plasma mass spectrometry (ICP-MS), after closed vessel microwave digestion

    International Nuclear Information System (INIS)

    Dufailly, Vincent; Noel, Laurent; Guerin, Thierry

    2006-01-01

    The determination of chromium ( 52 Cr), iron ( 56 Fe) and selenium ( 80 Se) isotopes in foodstuffs of animal origin has been performed by collision cell technology (CCT) mode using an inductively coupled plasma mass spectrometry (ICP-MS) as detector after closed vessel microwave digestion. To significantly decrease the argon-based interferences at mass to charge ratios (m/z): 52 ( 40 Ar 12 C), 56 ( 40 Ar 16 O) and 80 ( 40 Ar 40 Ar), the gas-flow rates of a helium and hydrogen mixture used in the hexapole collision cell were optimised to 1.5 ml min -1 H 2 and 0.5 ml min -1 He and the quadrupole bias was adjusted daily between -2 and -15 mV. Limits of quantification (LOQ) of 0.025, 0.086 and 0.041 mg kg -1 for Cr, Fe and Se, respectively, in 6% HNO 3 were estimated under optimized CCT conditions. These LOQ were improved by a factor of approximately 10 for each element compared to standard mode. Precision under repeatability, intermediate precision reproducibility and trueness have been tested on nine different certified reference materials in foodstuffs of animal origin and on an external proficiency testing scheme. The results obtained for chromium, iron and selenium were in all cases in good agreement with the certified values and trueness was improved, compared to those obtained in standard mode

  7. Contribution of bulk mass spectrometry isotopic analysis to characterization of materials in the framework of CMX-4

    International Nuclear Information System (INIS)

    Kuchkin, A.; Stebelkov, V.; Zhizhin, K.; Lierse von Gostomski, Ch.; Kardinal, Ch.; Loi, E.; Keegan, E.; Kristo, M.J.

    2018-01-01

    Seven laboratories used the results of bulk uranium isotopic analysis by either inductively coupled plasma mass spectrometry (ICP-MS) or thermal ionization mass spectrometry (TIMS) for characterization of the samples in the Nuclear Forensic International Technical Working Group fourth international collaborative material exercise, CMX-4. Comparison of the measured isotopic compositions of uranium in three exercise samples is implemented for identifying any differences or similarities between the samples. The role of isotopic analyses in the context of a real nuclear forensic investigation is discussed. Several limitations in carrying out ICP-MS or TIMS analysis in CMX-4 are noted. (author)

  8. 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}.

  9. 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

  10. 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.

  11. 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)

  12. 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.)

  13. Visualizing fossilization using laser ablation-inductively coupled plasma-mass spectrometry maps of trace elements in Late Cretaceous bones

    Science.gov (United States)

    Koenig, A.E.; Rogers, R.R.; Trueman, C.N.

    2009-01-01

    Elemental maps generated by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) provide a previously unavailable high-resolution visualization of the complex physicochemical conditions operating within individual bones during the early stages of diagenesis and fossilization. A selection of LA-ICP-MS maps of bones collected from the Late Cretaceous of Montana (United States) and Madagascar graphically illustrate diverse paths to recrystallization, and reveal unique insights into geochemical aspects of taphonomic history. Some bones show distinct gradients in concentrations of rare earth elements and uranium, with highest concentrations at external bone margins. Others exhibit more intricate patterns of trace element uptake related to bone histology and its control on the flow paths of pore waters. Patterns of element uptake as revealed by LA-ICP-MS maps can be used to guide sampling strategies, and call into question previous studies that hinge upon localized bulk samples of fossilized bone tissue. LA-ICP-MS maps also allow for comparison of recrystallization rates among fossil bones, and afford a novel approach to identifying bones or regions of bones potentially suitable for extracting intact biogeochemical signals. ?? 2009 Geological Society of America.

  14. Determination of Total Arsenic and Speciation in Apple Juice by Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry: An Experiment for the Analytical Chemistry Laboratory

    Science.gov (United States)

    He, Ping; Colon, Luis A.; Aga, Diana S.

    2016-01-01

    A two-part laboratory experiment was designed for upper-level analytical chemistry students to provide hands-on experience in the use of high performance liquid chromatography (HPLC) for separation and inductively coupled plasma mass spectrometry (ICP-MS) for detection. In the first part of the experiment, the students analyze total arsenic in…

  15. 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.

  16. Ultra-sensitive radionuclide spectrometry. Radiometrics and mass spectrometry synergy

    International Nuclear Information System (INIS)

    Povinec, P.P.

    2005-01-01

    Recent developments in radiometrics and mass spectrometry techniques for ultra-sensitive analysis of radionuclides in the marine environment are reviewed. In the radiometrics sector the dominant development has been the utilization of large HPGe detectors in underground laboratories with anti-cosmic or anti-Compton shielding for the analysis of short and medium-lived radionuclides in the environment. In the mass spectrometry sector, applications of inductively coupled plasma mass spectrometry (ICP-MS) and accelerator mass spectrometry (AMS) for the analysis of long-lived radionuclides in the environment are the most important recent achievements. The recent developments do not only considerably decrease the detection limits for several radionuclides (up to several orders of magnitude), but they also enable to decrease sample volumes so that sampling, e.g., of the water column can be much easier and more effective. A comparison of radiometrics and mass spectrometry results for the analysis of radionuclides in the marine environment shows a reasonable agreement - within quoted uncertainties, for wide range of activities and different sample matrices analyzed. (author)

  17. 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.

  18. Plutonium determination in urine by techniques of mass spectrometry; Determinacion de plutonio en orina por tecnicas de espectrometria de masas

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez M, H. [ININ, Departamento de Quimica, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Yllera de Ll, A., E-mail: hector.hernandez520@gmail.com [Centro de Investigaciones Energeticas, Medioambientales y Tecnologicas, Departamento de Medio Ambiente, Av. Complutense 22, 28040 Madrid (Spain)

    2013-10-15

    The objective of this study was to develop an analytic method for quantification and plutonium reappraisal in plane tables of alpha spectrometry be means of the mass spectrometry technique of high resolution with plasma source inductively coupled and desolvator Aridus (Aridus-Hr-Icp-Ms) and mass spectrometry with accelerator (AMS). The obtained results were, the recovery percentage of Pu in the plane table was of ∼ 90% and activity minimum detectable obtained with Aridus-Hr-Icp-Ms and AMS was of ∼ 3 and ∼ 0.4 f g of {sup 239}Pu, respectively. Conclusion, the results demonstrate the aptitude of the Aridus-Hr-Icp-Ms and AMS techniques in the Pu reappraisal in plane tables with bigger speed and precision, improving the values notably of the activity minimum detectable that can be obtained with the alpha spectrometry (∼ 50 f g of {sup 239}Pu). (author)

  19. Determination of aluminium in groundwater samples by GF-AAS, ICP-AES, ICP-MS and modelling of inorganic aluminium complexes.

    Science.gov (United States)

    Frankowski, Marcin; Zioła-Frankowska, Anetta; Kurzyca, Iwona; Novotný, Karel; Vaculovič, Tomas; Kanický, Viktor; Siepak, Marcin; Siepak, Jerzy

    2011-11-01

    The paper presents the results of aluminium determinations in ground water samples of the Miocene aquifer from the area of the city of Poznań (Poland). The determined aluminium content amounted from aluminium determinations were performed using three analytical techniques: graphite furnace atomic absorption spectrometry (GF-AAS), inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The results of aluminium determinations in groundwater samples for particular analytical techniques were compared. The results were used to identify the ascent of ground water from the Mesozoic aquifer to the Miocene aquifer in the area of the fault graben. Using the Mineql+ program, the modelling of the occurrence of aluminium and the following aluminium complexes: hydroxy, with fluorides and sulphates was performed. The paper presents the results of aluminium determinations in ground water using different analytical techniques as well as the chemical modelling in the Mineql+ program, which was performed for the first time and which enabled the identification of aluminium complexes in the investigated samples. The study confirms the occurrence of aluminium hydroxy complexes and aluminium fluoride complexes in the analysed groundwater samples. Despite the dominance of sulphates and organic matter in the sample, major participation of the complexes with these ligands was not stated based on the modelling.

  20. 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.

  1. 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

  2. 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

  3. A provenance study of iron archaeological artefacts by Inductively Coupled Plasma-Mass Spectrometry multi-elemental analysis

    International Nuclear Information System (INIS)

    Desaulty, Anne-Marie; Mariet, Clarisse; Dillmann, Philippe; Joron, Jean Louis; Fluzin, Philippe

    2008-01-01

    Raw materials and wastes (i.e. ore, slag and laitier) from ironmaking archaeological sites have been analyzed in order to understand the behavior of the trace elements in the ancient ironmaking processes and to find the significant-most elements to characterize an iron making region. The ICP-MS (Inductively Coupled Plasma Mass Spectrometry) appears to be an excellent technique for this type of studies. The comparison between the ICP-MS results obtained with the Standard Addition method and the INAA (Instrumental Neutron Activation Analyses) results proved that Sc, Co, (Ni), Rb, Cs, Ba, La, Ce, Sm, Eu, Yb, Hf, Th, U contents in the ores, slag and laitiers, and Co and Ni contents in the cast iron can be successfully determined by ICP-MS after wet acid digestion (low detection limits, good sensitivity and precision). By using significant trace element pairs (Yb/Ce, Ce/Th, La/Sc, U/Th, Nb/Y) present in the ores, laitiers and slag, it is possible to discriminate different French ironmaking regions as the Pays de Bray, Lorraine and Pays d'Ouche. These results open the way to further studies on the provenance of iron objects. The comparison between the ICP-MS results obtained with the Standard Calibration Curves method and the INAA results shows that matrices rich in iron, affect the ICP-MS analyses by suppressing the analytes signal. Further studies are necessary to improve understanding matrix effects

  4. Determination of mercury in hair: Comparison between gold amalgamation-atomic absorption spectrometry and mass spectrometry.

    Science.gov (United States)

    Domanico, Francesco; Forte, Giovanni; Majorani, Costanza; Senofonte, Oreste; Petrucci, Francesco; Pezzi, Vincenzo; Alimonti, Alessandro

    2017-09-01

    Mercury is a heavy metal that causes serious health problems in exposed subjects. The most toxic form, i.e., methylmercury (MeHg), is mostly excreted through human hair. Numerous analytical methods are available for total Hg analysis in human hair, including cold vapour atomic fluorescence spectrometry (CV-AFS), inductively coupled plasma mass spectrometry (ICP-MS) and thermal decomposition amalgamation atomic absorption spectrometry (TDA-AAS). The aim of the study was to compare the TDA-AAS with the ICP-MS in the Hg quantification in human hair. After the washing procedure to minimize the external contamination, from each hair sample two aliquots were taken; the first was used for direct analysis of Hg by TDA-AAS and the second was digested for Hg determination by the ICP-MS. Results indicated that the two data sets were fully comparable (median; TDA-AAS, 475ngg -1 ; ICP-MS, 437ngg -1 ) and were not statistically different (Mann-Whitney test; p=0.44). The two techniques presented results with a good coefficient of correlation (r=0.94) despite different operative ranges and method limits. Both techniques satisfied internal performance requirements and the parameters for method validation resulting sensitive, precise and reliable. Finally, the use of the TDA-AAS can be considered instead of the ICP-MS in hair analysis in order to reduce sample manipulation with minor risk of contamination, less time consuming due to the absence of the digestion step and cheaper analyses. Copyright © 2016 Elsevier GmbH. All rights reserved.

  5. Controlled dissolution of silicon dioxide layers for depth resolved multielement analysis by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Lorge, Susan E.; Houk, R.S.

    2009-01-01

    Dissolution procedures were developed to control the number of surface layers removed, in an attempt to achieve depth resolved analysis by inductively coupled plasma-mass spectrometry (ICP-MS). NIST 612 glass was chosen because it is a homogeneous material with many elements at interesting concentrations, ∼ 50 ppm. Varying dissolution time and HF concentration resulted in the reproducible removal of SiO 2 layers as thin as 70 A deep. Dissolved trace metals were determined after dilution by inductively coupled plasma-mass spectrometry (ICP-MS) with a magnetic sector instrument. The amount removed was determined from the concentration of a major element, Ca. With the exception of Zn, trace metal concentrations agreed reasonably well with their certified values for removal depths of 500, 300 and 150 A. Zinc concentration was significantly high in all dissolutions indicating either a contamination problem or that Zn is removed at a faster rate than Ca. For the dissolutions that removed 70 A of SiO 2 , Cr, Mn, Co, Sr, Cd, Ce, Dy, Er, Yb and U recovery results agreed with their certified values (∼ 50 ppm); Ti, As, Mo, Ba, and Th could not be determined because net intensities were below 3σ of the blank; and measured concentrations for Cu, Pb and Zn were well above the certified values.

  6. Multi-element analysis of urine using dynamic reaction cell inductively coupled plasma mass spectrometry (ICP-DRC-MS — A practical application

    Directory of Open Access Journals (Sweden)

    Renata Brodzka

    2013-04-01

    Full Text Available Objectives: The method for the determination of As, Al, Cd, Ni, Pb (toxic elements and Cr, Co, Cu, Fe, Mn, Zn (essential elements in human urine by the use of Inductively Coupled Plasma Mass Spectrometry (quadrupole ICP-MS DRCe Elan, Perkin Elmer with the dynamic reaction cell (DRC was developed. Materials and Methods: The method has been applied for multi-element analysis of the urine of 16 non-exposed healthy volunteers and 27 workers employed in a copper smelter. The analysis was conducted after initial 10-fold dilution of the urine samples with 0,1% nitric acid. Rhodium was used as an internal standard. The method validation parameters such as detection limit, sensitivity, precision were described for all elements. Accuracy of the method was checked by the regular use of certified reference materials ClinCheck®-Control Urine (Recipe as well as by participation of the laboratory in the German External Quality Assessment Scheme (G-EQUAS. Results: The detection limits (DL 3s of the applied method were 0.025, 0.007, 0.002, 0.004, 0.004, 0.086, 0.037, 0.009, 0.016, 0.008, 0.064 (μg/l for Al, As, Cd, Cr, Co, Cu, Fe, Mn, Ni, Pb, Zn in urine, respectively. For each element linearity with correlation coefficient of at least 0.999 was determined. Spectral interferences from some of the ions were removed using DRC-e with addition of alternative gas: methane for cobalt, copper, cadmium, chromium, iron, manganese, nickel and rhodium, and oxygen for arsenic. Conclusions: The developed method allows to determine simultaneously eleven elements in the urine with low detection limits, high sensitivity and good accuracy. Moreover, the method is appropriate for the assessment of both environmental and occupational exposure.

  7. [Determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry].

    Science.gov (United States)

    Lin, Li; Chen, Guang; Chen, Yuhong

    2011-07-01

    A method was established for the determination of iodine and its species in plant samples using ion chromatography-inductively coupled plasma mass spectrometry (IC-ICP/ MS). Alkaline extraction and IC-ICP/MS were applied as the sample pre-treatment method and the detection technique respectively, for iodate and iodide determination. Moreover, high-temperature pyrolysis absorption was adopted as the pre-treatment method for total iodine analysis, which finally converted all the iodine species into iodide and measured the iodide by IC-ICP/MS. The recoveries of iodine for alkaline extraction and high-temperature pyrolysis absorption were 89.6%-97.5% and 95.2%-111.2%, respectively. The results were satisfactory. The detection limit of iodine was 0.010 mg/kg. The iodine and its speciation contents in several kinds of plant samples such as seaweeds, kelp, cabbage, tea leaf and spinach were investigated. It was shown that the iodine in seaweeds mainly existed as organic iodine; while the ones in kelp, cabbage, tea leaf and spinach mainly existed as inorganic iodine.

  8. 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.

  9. 2D elemental mapping of sections of human kidney stones using laser ablation inductively-coupled plasma-mass spectrometry: Possibilities and limitations

    Energy Technology Data Exchange (ETDEWEB)

    Vašinová Galiová, Michaela [Department of Chemistry, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Central European Institute of Technology (CEITEC), Masaryk University, Kamenice 5, 625 00 Brno (Czech Republic); Čopjaková, Renata; Škoda, Radek [Department of Geological Sciences, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Štěpánková, Kateřina; Vaňková, Michaela [Department of Chemistry, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Kuta, Jan [Research Centre for Toxic Compounds in the Environment (RECETOX), Masaryk University, Kamenice 126/3, 625 00 Brno (Czech Republic); Prokeš, Lubomír [Department of Chemistry, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Department of Physical Electronics, Faculty of Science, Masaryk University, Kotlářská 2, 611 37 Brno (Czech Republic); Kynický, Jindřich [Department of Pedology and Geology, Faculty of Forestry and Wood Technology, Mendel University in Brno, Zemědělská 3, 613 00 Brno (Czech Republic); and others

    2014-10-01

    A 213 nm Nd:YAG-based laser ablation (LA) system coupled to quadrupole-based inductively coupled plasma-mass spectrometer and an ArF* excimer-based LA-system coupled to a double-focusing sector field inductively coupled plasma-mass spectrometer were employed to study the spatial distribution of various elements in kidney stones (uroliths). Sections of the surfaces of uroliths were ablated according to line patterns to investigate the elemental profiles for the different urolith growth zones. This exploratory study was mainly focused on the distinguishing of the main constituents of urinary calculus fragments by means of LA-ICP-mass spectrometry. Changes in the ablation rate for oxalate and phosphate phases related to matrix density and hardness are discussed. Elemental association was investigated on the basis of 2D mapping. The possibility of using NIST SRM 1486 Bone Meal as an external standard for calibration was tested. It is shown that LA-ICP-MS is helpful for determination of the mineralogical composition and size of all phases within the analyzed surface area, for tracing down elemental associations and for documenting the elemental content of urinary stones. LA-ICP-MS results (elemental contents and maps) are compared to those obtained with electron microprobe analysis and solution analysis ICP-MS. - Highlights: • Elements in phosphate and oxalate urolith phases were quantified by LA-ICP-MS. • SRM NIST 1486 Bone Meal was proved suitable for quantification in uroliths. • Different ablation rates in particular phases were included at quantification. • Oxalate and apatite phases show opposite hardness order to natural minerals. • Uroliths were classified according to elemental association to phases.

  10. Indigenous instrumentation for mass spectrometry: Part II - development of plasma source mass spectrometers. PD-5-3

    International Nuclear Information System (INIS)

    Nataraju, V.

    2007-01-01

    The growing demands from analytical community, for a precise isotope ratio and ultra trace concentration measurements, has lead to significant improvement in mass spectrometer instrumentation development with respect to sensitivity, detection limits, precision and accuracy. Among the many analytical techniques available, plasma source mass spectrometers like Inductively Coupled Plasma Mass Spectrometry (ICPMS), multi collector (MC) ICPMS and Glow Discharge Mass Spectrometry (GDMS), have matured into reliable tools for the above applications. Where as ICPMS is by far the most successful method for aqueous solutions, GDMS is being applied for bulk and impurity analysis of conducting as well non-conducting solids. VPID, BARC has been developing mass spectrometers for different inorganic applications of DAE users. Over the years expertise has been developed in all the aspects of mass spectrometry instrumentation. Part 1 of this indigenous instrumentation on mass spectrometry gives details of magnetic sector instruments with either EI or TI source for isotopic ratio analysis. The present paper is a continuation of that on plasma source and quadrupole mass spectrometers. This paper covers i) ICP-QMS, ii) MC-ICPMS, iii) GDMS and iv) QMS

  11. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: a tutorial review. Part II. Practical considerations.

    Science.gov (United States)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-07-23

    Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review, Electrothermal Vaporization and Laser Ablation will also be shortly described. The second issue is devoted to the analytical strategies for elemental quantification in such matrices, with particular insight into the isotope dilution technique, particularly used in speciation analysis by ICP-coupled separation techniques. Copyright © 2015 Elsevier B.V. All rights reserved.

  12. Contribution to the development of new analytical methods by the coupling between capillary electrophoresis and mass spectrometry (ICP-MS and ESI-MS): applications to the nuclear and biological fields

    International Nuclear Information System (INIS)

    Pitois, A.

    2006-04-01

    The coupling between chromatographic and electrophoretic separation techniques and mass spectrometry is used to combine the efficiency of the separation technique to the selectivity and sensitivity of the detectors. In this work, the number of applications of the CE-MS couplings has been increased. New analytical methods have been set up in the nuclear and biological fields. New analytical methods for the determination of fission products (cesium and lanthanides) have been developed by CE-ICP-MS. They enable to determine both concentration and isotopic composition of the fission products for very low detection limits (ng/mL by CE-Q-ICPMS, pg/mL by CE-HR-ICP-MS), since all the isobaric interferences are resolved. Moreover, only some nano-liters of sample are necessary to perform the analysis. These method have been applied with success to a simulated sample of spent fuel, to a nuclear sample from PUREX process and to a leaching of MOX fuel. Then, lanthanides have been analysed by CE-ESI-MS and the capability of ESI-MS to provide structural information has been studied. Elementary information has been obtained for strong potentials. Structural information has been obtained for low potentials. Finally, a new analytical method by CE-ESI-MS for the determination of 10B-boronophenylalanine (10B-BPA) has been developed for Boron Neutron Capture Therapy (BNCT). It has been applied to the cellular lines F98 and HUVEC. This CE-ESI-MS method has been validated by HR-ICP-MS. It enables a direct quantification of the chemical form 10B-BPA in samples of limited size (some nano-liters) and for low concentrations (ng/mL). As a consequence, this CE-ESI-MS method has enabled the study of the kinetics of 10B-BPA release and uptake for the F98 cells. (author)

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. Comparison of 4 analytical techniques based on atomic spectrometry for the determination of total tin in canned foodstuffs

    OpenAIRE

    2011-01-01

    Abstract Different techniques for the determination of total tin in beverage and canned food by atomic spectrometry were compared. The performance characteristics of Inductively Coupled Plasma Mass Spectrometry (ICP-MS), Hydride Generation Inductively Coupled Plasma Atomic Emission Spectrometry (HG-ICP-AES), Electrothermal Atomization Atomic Absorption Spectrometry (ETA-AAS) and Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) were determined in term of linearity, ...

  18. Determination of technetium-99, thorium-230 and uranium-234 in soils by inductively coupled plasma mass spectrometry using flow injection preconcentration

    International Nuclear Information System (INIS)

    Hollenbach, Mark; Grohs, James; Mamich, Stephen; Kroft, Marilyn; Denoyer, E.R.

    1994-01-01

    A new method is described for the determination of 99 Tc, 230 Th, and 234 U at ultra-trace levels in soils. The method used flow injection (FI) for on-line preconcentration of 99 Tc, 230 Th and 234 U prior to detection using inductively coupled plasma mass spectrometry (ICP-MS). The FI-ICP-MS method results in greater sensitivity and freedom from interferences compared with direct aspiration into an ICP mass spectrometer. Detection limits are improved by approximately a factor of 10. The FI-ICP-MS method is also faster, less labour intensive and generates less laboratory waste than traditional radiochemical methods. The accuracy of the method was tested for 99 Tc by comparison to liquid scintillation counting and for 230 Th and 234 U by analysis of a US Department of Energy reference soil. Detection limits in the soil for 99 Tc, 230 Th and 234 U were 11 mBq g -1 (0.02 ng g -1 ), 3.7 mBq g -1 (0.005 ng g -1 ) and 0.74 mBq g -1 (0.003 ng g -1 ), respectively. Sample preparation, analysis protocol, and method validation are described. (Author)

  19. 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)

  20. Multielement trace determination in SiC powders: assessment of interlaboratory comparisons aimed at the validation and standardization of analytical procedures with direct solid sampling based on ETV ICP OES and DC arc OES.

    Science.gov (United States)

    Matschat, Ralf; Hassler, Jürgen; Traub, Heike; Dette, Angelika

    2005-12-01

    The members of the committee NMP 264 "Chemical analysis of non-oxidic raw and basic materials" of the German Standards Institute (DIN) have organized two interlaboratory comparisons for multielement determination of trace elements in silicon carbide (SiC) powders via direct solid sampling methods. One of the interlaboratory comparisons was based on the application of inductively coupled plasma optical emission spectrometry with electrothermal vaporization (ETV ICP OES), and the other on the application of optical emission spectrometry with direct current arc (DC arc OES). The interlaboratory comparisons were organized and performed in the framework of the development of two standards related to "the determination of mass fractions of metallic impurities in powders and grain sizes of ceramic raw and basic materials" by both methods. SiC powders were used as typical examples of this category of material. The aim of the interlaboratory comparisons was to determine the repeatability and reproducibility of both analytical methods to be standardized. This was an important contribution to the practical applicability of both draft standards. Eight laboratories participated in the interlaboratory comparison with ETV ICP OES and nine in the interlaboratory comparison with DC arc OES. Ten analytes were investigated by ETV ICP OES and eleven by DC arc OES. Six different SiC powders were used for the calibration. The mass fractions of their relevant trace elements were determined after wet chemical digestion. All participants followed the analytical requirements described in the draft standards. In the calculation process, three of the calibration materials were used successively as analytical samples. This was managed in the following manner: the material that had just been used as the analytical sample was excluded from the calibration, so the five other materials were used to establish the calibration plot. The results from the interlaboratory comparisons were summarized and

  1. 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

  2. Determination of chromium, iron and selenium in foodstuffs of animal origin by collision cell technology, inductively coupled plasma mass spectrometry (ICP-MS), after closed vessel microwave digestion

    Energy Technology Data Exchange (ETDEWEB)

    Dufailly, Vincent [Agence Francaise de Securite Sanitaire des Aliments - Laboratoire d' Etudes et de Recherches sur la Qualite des Aliments et des procedees agroalimentaires - Unite des Contaminants Inorganiques et Mineraux de l' Environnement, 23, avenue du General de Gaulle, F-94706 Maisons-Alfort Cedex (France); Noel, Laurent [Agence Francaise de Securite Sanitaire des Aliments - Laboratoire d' Etudes et de Recherches sur la Qualite des Aliments et des procedees agroalimentaires - Unite des Contaminants Inorganiques et Mineraux de l' Environnement, 23, avenue du General de Gaulle, F-94706 Maisons-Alfort Cedex (France); Guerin, Thierry [Agence Francaise de Securite Sanitaire des Aliments - Laboratoire d' Etudes et de Recherches sur la Qualite des Aliments et des procedees agroalimentaires - Unite des Contaminants Inorganiques et Mineraux de l' Environnement, 23, avenue du General de Gaulle, F-94706 Maisons-Alfort Cedex (France)]. E-mail: t.guerin@afssa.fr

    2006-04-21

    The determination of chromium ({sup 52}Cr), iron ({sup 56}Fe) and selenium ({sup 80}Se) isotopes in foodstuffs of animal origin has been performed by collision cell technology (CCT) mode using an inductively coupled plasma mass spectrometry (ICP-MS) as detector after closed vessel microwave digestion. To significantly decrease the argon-based interferences at mass to charge ratios (m/z): 52 ({sup 40}Ar{sup 12}C), 56 ({sup 40}Ar{sup 16}O) and 80 ({sup 40}Ar{sup 40}Ar), the gas-flow rates of a helium and hydrogen mixture used in the hexapole collision cell were optimised to 1.5 ml min{sup -1} H{sub 2} and 0.5 ml min{sup -1} He and the quadrupole bias was adjusted daily between -2 and -15 mV. Limits of quantification (LOQ) of 0.025, 0.086 and 0.041 mg kg{sup -1} for Cr, Fe and Se, respectively, in 6% HNO{sub 3} were estimated under optimized CCT conditions. These LOQ were improved by a factor of approximately 10 for each element compared to standard mode. Precision under repeatability, intermediate precision reproducibility and trueness have been tested on nine different certified reference materials in foodstuffs of animal origin and on an external proficiency testing scheme. The results obtained for chromium, iron and selenium were in all cases in good agreement with the certified values and trueness was improved, compared to those obtained in standard mode.

  3. The Study of Titanium and Zirconium Ions in Water by MPT-LTQ Mass Spectrometry in Negative Mode.

    Science.gov (United States)

    Yang, Junqing; Zheng, Mei; Liu, Qiuju; Yang, Meiling Zhu Chushan; Zhang, Yan; Zhu, Zhiqiang

    2017-09-26

    Microwave plasma torches (MPTs) can be used as simple and low power-consumption ambient ion sources. When MPT-mass spectrometry (MPT-MS) is applied in the detection of some metal elements, the metallic ions exhibit some novel features which are significantly different with those obtained by the traditional inductively coupled plasma (ICP)-mass spectrometry (ICP-MS) and may be helpful for metal element analysis. As the representative elements of group IVA, titanium and zirconium are both of importance and value in modern industry, and they have impacts on human health. Here, we first provide a study on the complex anions of titanium and zirconium in water by using the MPT as ion source and a linear ion trap mass spectrometer (LTQ-MS). These complex anions were produced in the plasma flame by an aqueous solution flowing through the central tube of the MPT, and were introduced into the inlet of the mass spectrometry working in negative ion mode to get the feature mass spectrometric signals. Moreover, the feature fragment patterns of these ions in multi-step collision- induced dissociation processes have been explained. Under the optimized conditions, the limit of detection (LOD) using the MS² (the second tandem mass spectrometry) procedure was estimated to be at the level of 10μg/L for titanium and 20 μg/L for zirconium with linear dynamics ranges that cover at least two orders of magnitude, i.e., between 0-500 μg/L and 20-200 μg/L, respectively. These experimental data demonstrated that the MPT-MS is a promising and useful tool in field analysis of titanium and zirconium ions in water, and can be applied in many fields, such as environmental control, hydrogeology, and water quality inspection. In addition, MPT-MS could also be used as a supplement of ICP-MS for the rapid and on-site analysis of metal ions.

  4. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part II. Practical considerations

    Energy Technology Data Exchange (ETDEWEB)

    Leclercq, Amélie, E-mail: amelie.leclercq@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Nonell, Anthony, E-mail: anthony.nonell@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Todolí Torró, José Luis, E-mail: jose.todoli@ua.es [Universidad de Alicante, Departamento de Quimica Analitica, Nutricion y Bromatología, Ap. de Correos, 99, 03080 Alicante (Spain); Bresson, Carole, E-mail: carole.bresson@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vio, Laurent, E-mail: laurent.vio@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Vercouter, Thomas, E-mail: thomas.vercouter@cea.fr [CEA Saclay, DEN, DANS, DPC, SEARS, Laboratoire de développement Analytique Nucléaire Isotopique et Elémentaire, 91191 Gif-sur-Yvette (France); Chartier, Frédéric, E-mail: frederic.chartier@cea.fr [CEA Saclay, DEN, DANS, DPC, 91191 Gif-sur-Yvette (France)

    2015-07-23

    Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

  5. Introduction of organic/hydro-organic matrices in inductively coupled plasma optical emission spectrometry and mass spectrometry: A tutorial review. Part II. Practical considerations

    International Nuclear Information System (INIS)

    Leclercq, Amélie; Nonell, Anthony; Todolí Torró, José Luis; Bresson, Carole; Vio, Laurent; Vercouter, Thomas; Chartier, Frédéric

    2015-01-01

    Graphical abstract: This tutorial review is dedicated to the analysis of organic/hydro-organic matrices by ICP techniques. A state-of-the-art focusing on sample introduction, relevant operating parameters optimization and analytical strategies for elemental quantification is provided. - Highlights: • Practical considerations to perform analyses in organic/hydro-organic matrices. • Description, benefits and drawbacks of recent introduction devices. • Optimization to improve plasma tolerance towards organic/hydro-organic matrices. • Analytical strategies for elemental quantification in organic/hydro-organic matrices. - Abstract: Inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are increasingly used to carry out analyses in organic/hydro-organic matrices. The introduction of such matrices into ICP sources is particularly challenging and can be the cause of numerous drawbacks. This tutorial review, divided in two parts, explores the rich literature related to the introduction of organic/hydro-organic matrices in ICP sources. Part I provided theoretical considerations associated with the physico-chemical properties of such matrices, in an attempt to understand the induced phenomena. Part II of this tutorial review is dedicated to more practical considerations on instrumentation, instrumental and operating parameters, as well as analytical strategies for elemental quantification in such matrices. Two important issues are addressed in this part: the first concerns the instrumentation and optimization of instrumental and operating parameters, pointing out (i) the description, benefits and drawbacks of different kinds of nebulization and desolvation devices and the impact of more specific instrumental parameters such as the injector characteristics and the material used for the cone; and, (ii) the optimization of operating parameters, for both ICP-OES and ICP-MS. Even if it is at the margin of this tutorial review

  6. Determination of technetium-99 in soil samples by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Muto, Toshio; Shimokawa, Toshinari

    1997-01-01

    A new powerful analytical technique viz. high performance liquid chromatography(HPLC) coupled to inductively coupled plasma mass spectrometry(HPLC/ICP-MS) has been applied to the determination of technetium-99( 99 Tc) in soils as a typical environmental sample. Technetium was enriched in a solution from incinerated soil samples by leaching in HNO 3 and passed through 'TEVA resin' column. The solution was injected into HPLC/ICP-MS system to eliminate the interfering elements (i.e. Ru and Mo) and to determine the 99 Tc concentration at the same time. The concentrations of 99 Tc in the incinerated soils were found to be 0.49Bq/kg(0.77ng/kg)-1.4Bq/kg(2.2ng/kg) with the determination limit of 0.02Bq/kg(0.03ng/kg(0.03ppt)). The results indicate the following findings; 1) the determination of 99 Tc by ICP-MS after strict elimination of the interfering elements by HPLC brings about the improvement in their reliability; 2) the detection limits identified are much lower compared with those by conventional ICP-MS methods because of the concentration of 99 Tc to smaller volume, which is due to only 100μl of samples could be measured by HPLC/ICP-MS system; 3) sample preparation could be simplified because of strict elimination of the interfering elements by HPLC. This research showed that HPLC/ICP-MS system is very effective to determine 99 Tc in environmental samples. (author)

  7. 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.

  8. 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.

  9. Quantitative analysis of some important metals and metalloids in tobacco products by inductively coupled plasma-mass spectrometry (ICP-MS)

    Science.gov (United States)

    2012-01-01

    Background Large scale usage of tobacco causes a lot of health troubles in human. Various formulations of tobacco are extensively used by the people particularly in developing world. Besides several toxic tobacco constituents some metals and metalloids are also believed to pose health risks. This paper describes inductively coupled plasma-mass spectrometric (ICP-MS) quantification of some important metals and metalloids in various brands of smoked, sniffed, dipped and chewed tobacco products. Results A microwave-assisted digestion method was used for sample preparation. The method was validated by analyzing a certified reference material. Percentage relative standard deviation (% R.S.D.) between recovered and certified values was  r > 0.999. Improved limits of detection (LODs) were in range of ng/L for all elements. Fe, Al and Mn were found to be in the highest concentration in all types of tobacco products, while Zn, Cu, Ni and Cr were below the average concentration of 40 μg/g, and Pb, Co, As, Se and Cd were below 5 μg/g. All elements, apart from Pb, were high in concentration in dipping tobacco in comparison to other tobacco products. Generally, the order of all elemental concentration can be expressed in different tobacco products as chewing metalloids in a wide spectrum of tobacco formulations. The outcome of this study would be beneficial for health authorities and individuals. PMID:22709464

  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. 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.

  12. Investigating the adduct formation of organic mercury species with carbonic anhydrase and hemoglobin from human red blood cell hemolysate by means of LC/ESI-TOF-MS and LC/ICP-MS.

    Science.gov (United States)

    Hogeback, Jens; Schwarzer, Miriam; Wehe, Christoph A; Sperling, Michael; Karst, Uwe

    2016-01-01

    The interaction of mercury species with human erythrocytes is studied to investigate possible high molecular binding partners for mercury species. Human blood hemolysate was spiked with methylmercury and investigated by means of liquid chromatography (LC) coupled to electrospray ionization time of flight mass spectrometry (ESI-ToF-MS) and inductively coupled plasma mass spectrometry (ICP-MS). Beside adduct formation of mercury species with hemoglobin, the main compound of the erythrocytes, mercury binding to the enzyme carbonic anhydrase was revealed. Due to an enzymatic digest of the protein-mercury adduct, the binding site at the free thiol group of the protein was identified. These results indicate that carbonic anhydrase might play a role in mercury toxicity.

  13. Development of iodine based impinger solutions for the efficient capture of Hg{sup 0} using direct injection nebulization-inductively coupled plasma mass spectrometry analysis

    Energy Technology Data Exchange (ETDEWEB)

    Hedrick, E.; Lee, T.G.; Biswas, P.; Zhuang, Y. [US Environmental Protection Agency, Cincinnati, OH (USA). National Exposure Research Laboratory

    2001-09-15

    Inductively coupled plasma mass spectrometry (ICP/MS) with direct injection nebulization (DIN) was used to evaluate novel impinger solution compositions capable of capturing elemental mercury (Hg{sup 0}) in EPA Method 5 type sampling. An iodine based impinger solution proved to be very efficient for Hg{sup 0} capture and was amenable to direct analysis by DIN-ICP/MS. Hg{sup 0} capture efficiency using aqueous iodine (I{sub 3}{sup -}) was comparable to Hg{sup 0} capture using acidified potassium permanganate impinger solutions which were analyzed by cold vapor atomic absorption spectrometry (CVAAS) with greater than 98% capture of Hg{sup 0} in the oxidizing impinger. Using DIN-ICP/MS, it was demonstrated for the first time that iodine can be generated just prior to impinger sampling for efficiently oxidizing Hg{sup 0} and retailing it in solution as HgI{sub 4}{sup 2-}. Due to the increased interest in Hg speciation from combustion sources and the potential for using DIN-ICP/MS for multiple metals analyses, an impinger sampling train for gaseous Hg speciation and multiple metals analyses using DIN-ICP/MS analyses is presented. The unique feature of such a sampling train is that each impinger solution in the series is amenable to direct analysis by DIN-ICP/MS. A bituminous coal was combusted in a bench scale coal system, and gaseous Hg species (oxidized and elemental) were determined using the proposed impinger train. The DIN-ICP/Ms instrumental detection limit was 0.003 ppb, and MDLs ranged from 0.007 to 0.116 {mu}g/L (ppb) in a variety of impinger solutions used for Hg capture. 33 refs., 5 figs., 7 tabs.

  14. Recent trends in atomic spectrometry with microwave-induced plasmas

    International Nuclear Information System (INIS)

    Broekaert, Jose A.C.; Siemens, Volker

    2004-01-01

    The state-of-the-art and trends of development in atomic spectrometry with microwave-induced plasmas (MIPs) since the 1998s are presented and discussed. This includes developments in devices for producing microwave plasma discharges, with reference also to miniaturized systems as well as to progress in sample introduction for microwave-induced plasmas, such as pneumatic and ultrasonic nebulization using membrane desolvation, to the further development of gaseous analyte species generation systems and to both spark and laser ablation (LA). The features of microwave-induced plasma mass spectrometry (MIP-MS) as an alternative to inductively coupled plasma (ICP)-MS are discussed. Recent work on the use of microwave-induced plasma atomic spectrometry for trace element determinations and monitoring, their use as tandem sources and for particle sizing are discussed. Recent applications of the coupling of gas chromatography and MIP atomic spectrometry for the determination of organometallic compounds of heavy metals such as Pb, Hg, Se and Sn are reviewed and the possibilities of trapping for sensitivity enhancement, as required for many applications especially in environmental work, are showed at the hand of citations from the recent literature

  15. 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.

  16. 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

  17. Comparison of femtosecond and nanosecond laser ablation inductively coupled plasma mass spectrometry for uranium isotopic measurements

    Energy Technology Data Exchange (ETDEWEB)

    Havrilla, George Joseph [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); McIntosh, Kathryn Gallagher [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Judge, Elizabeth [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Dirmyer, Matthew R. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Campbell, Keri [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Gonzalez, Jhanis J. [Applied Spectra Inc., Fremont, CA (United States)

    2016-10-20

    Feasibility tests were conducted using femtosecond and nanosecond laser ablation inductively coupled plasma mass spectrometry for rapid uranium isotopic measurements. The samples used in this study consisted of a range of pg quantities of known 235/238 U solutions as dried spot residues of 300 pL drops on silicon substrates. The samples spanned the following enrichments of 235U: 0.5, 1.5, 2, 3, and 15.1%. In this direct comparison using these particular samples both pulse durations demonstrated near equivalent data can be produced on either system with respect to accuracy and precision. There is no question that either LA-ICP-MS method offers the potential for rapid, accurate and precise isotopic measurements of U10Mo materials whether DU, LEU or HEU. The LA-ICP-MS equipment used for this work is commercially available. The program is in the process of validating this work for large samples using center samples strips from Y-12 MP-1 LEU-Mo Casting #1.

  18. Comparison of femtosecond and nanosecond laser ablation inductively coupled plasma mass spectrometry for uranium isotopic measurements

    International Nuclear Information System (INIS)

    Havrilla, George Joseph; McIntosh, Kathryn Gallagher; Judge, Elizabeth; Dirmyer, Matthew R.; Campbell, Keri; Gonzalez, Jhanis J.

    2016-01-01

    Feasibility tests were conducted using femtosecond and nanosecond laser ablation inductively coupled plasma mass spectrometry for rapid uranium isotopic measurements. The samples used in this study consisted of a range of pg quantities of known 235/238 U solutions as dried spot residues of 300 pL drops on silicon substrates. The samples spanned the following enrichments of 235 U: 0.5, 1.5, 2, 3, and 15.1%. In this direct comparison using these particular samples both pulse durations demonstrated near equivalent data can be produced on either system with respect to accuracy and precision. There is no question that either LA-ICP-MS method offers the potential for rapid, accurate and precise isotopic measurements of U10Mo materials whether DU, LEU or HEU. The LA-ICP-MS equipment used for this work is commercially available. The program is in the process of validating this work for large samples using center samples strips from Y-12 MP-1 LEU-Mo Casting #1.

  19. Standard practice for alternate actinide calibration for inductively coupled plasma-mass spectrometry

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2004-01-01

    1.1 This practice provides guidance for an alternate linear calibration for the determination of selected actinide isotopes in appropriately prepared aqueous solutions by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). This alternate calibration is mass bias adjusted using thorium-232 (232Th) and uranium-238 (238U) standards. One of the benefits of this standard practice is the ability to calibrate for the analysis of highly radioactive actinides using calibration standards at much lower specific activities. Environmental laboratories may find this standard practice useful if facilities are not available to handle the highly radioactive standards of the individual actinides of interest. 1.2 The instrument response for a series of determinations of known concentration of 232Th and 238U defines the mass versus response relationship. For each standard concentration, the slope of the line defined by 232Th and 238U is used to derive linear calibration curves for each mass of interest using interference equ...

  20. 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

  1. 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

  2. A novel strategy to evaluate the degradation of quantum dots: identification and quantification of CdTe quantum dots and corresponding ionic species by CZE-ICP-MS.

    Science.gov (United States)

    Meng, Peijun; Xiong, Yamin; Wu, Yingting; Hu, Yue; Wang, Hui; Pang, Yuanfeng; Jiang, Shuqing; Han, Sihai; Huang, Peili

    2018-05-09

    In view of the significance and urgency of the speciation analysis of quantum dots (QDs) and their degradation products for clarifying their degradation rules and toxicity mechanisms, a method for the identification and quantification of CdTe QDs and corresponding ionic species in complex matrices was developed using capillary zone electrophoresis (CZE) coupled to inductively coupled plasma-mass spectrometry (ICP-MS). The quality assessment of commercial CdTe QDs and serum pharmacokinetics of synthesized CdTe QDs in rats were successfully undertaken using the developed CZE-ICP-MS method.

  3. The Means: Cytometry and Mass Spectrometry Converge in a Single Cell Deep Profiling Platform

    Science.gov (United States)

    Weis-Garcia, Frances; Bandura, Dmitry; Baranov, Vladimir; Ornatsky, Olga; Tanner, Scott

    2013-01-01

    Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is a distinct flavor of mass spectrometry that has had little association with cell biology: it remains the state of the art for the determination of the atomic composition of materials. Unrelatedly, flow cytometry is the superior method for distinguishing the heterogeneity of cells through the determination of antigen signatures using tagged antibodies. Simply replacing fluorophore tags with stable isotopes of the heavy metals, and measuring these cell-by-cell with ICP-MS, dramatically increases the number of probes that can be simultaneously measured in cytometry and enables a transformative increase in the resolution of rare cell populations in complex biological samples. While this can be thought of as a novel incarnation of single-cell targeted proteomics, the metal-labeling reagents, ICP-MS of single cells, and accompanying informatics comprise a new field of technology termed Mass Cytometry. While the conception of mass cytometry is simple the embodiment to address the issues of multi-parameter flow cytometry has been far more challenging. There are many elements, and many more stable isotopes of those elements, that might be used as distinct reporter tags. Still, there are many approaches to conjugating metals to antibodies (or other affinity reagents) and work in this area along with developing new applications is ongoing. The mass resolution and linear (quantitative) dynamic range of ICP-MS allows those many stable isotopes to be measured simultaneously and without the spectral overlap issues that limit fluorescence assay. However, the adaptation of ICP-MS to allow high-speed simultaneous measurement with single cell distinction at high throughput required innovation of the cell introduction system, ion optics (sampling, transmission and beam-shaping), mass analysis, and signal handling and processing. An overview of “the nuts and bolts” of Mass Cytometry is presented.

  4. CHAPTER 7. BERYLLIUM ANALYSIS BY NON-PLASMA BASED METHODS

    Energy Technology Data Exchange (ETDEWEB)

    Ekechukwu, A

    2009-04-20

    The most common method of analysis for beryllium is inductively coupled plasma atomic emission spectrometry (ICP-AES). This method, along with inductively coupled plasma mass spectrometry (ICP-MS), is discussed in Chapter 6. However, other methods exist and have been used for different applications. These methods include spectroscopic, chromatographic, colorimetric, and electrochemical. This chapter provides an overview of beryllium analysis methods other than plasma spectrometry (inductively coupled plasma atomic emission spectrometry or mass spectrometry). The basic methods, detection limits and interferences are described. Specific applications from the literature are also presented.

  5. New approach to the determination phosphorothioate oligonucleotides by ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Studzińska, Sylwia; Mounicou, Sandra; Szpunar, Joanna; Łobiński, Ryszard; Buszewski, Bogusław

    2015-01-15

    This text presents a novel method for the separation and detection of phosphorothioate oligonucleotides with the use of ion pair ultra high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry The research showed that hexafluoroisopropanol/triethylamine based mobile phases may be successfully used when liquid chromatography is coupled with such elemental detection. However, the concentration of both HFIP and TEA influences the final result. The lower concentration of HFIP, the lower the background in ICP-MS and the greater the sensitivity. The method applied for the analysis of serum samples was based on high resolution inductively coupled plasma mass spectrometry. Utilization of this method allows determination of fifty times lower quantity of phosphorothioate oligonucleotides than in the case of quadrupole mass analyzer. Monitoring of (31)P may be used to quantify these compounds at the level of 80 μg L(-1), while simultaneous determination of sulfur is very useful for qualitative analysis. Moreover, the results presented in this paper demonstrate the practical applicability of coupling LC with ICP-MS in determining phosphorothioate oligonucleotides and their metabolites in serum within 7 min with a very good sensitivity. The method was linear in the concentration range between 0.2 and 3 mg L(-1). The limit of detection was in the range of 0.07 and 0.13 mg L(-1). Accuracy varied with concentration, but was in the range of 3%. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    Science.gov (United States)

    Duyck, Christiane Béatrice; Saint'Pierre, Tatiana Dillenburg; Miekeley, Norbert; da Fonseca, Teresa Cristina Oliveira; Szatmari, Peter

    2011-05-01

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L - 1 and 8 μg L - 1 . The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  7. 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.)

  8. Development of a novel low-flow ion source/sampling cone geometry for inductively coupled plasma mass spectrometry and application in hyphenated techniques

    Science.gov (United States)

    Pfeifer, Thorben; Janzen, Rasmus; Steingrobe, Tobias; Sperling, Michael; Franze, Bastian; Engelhard, Carsten; Buscher, Wolfgang

    2012-10-01

    A novel ion source/sampling cone device for inductively coupled plasma mass spectrometry (ICP-MS) especially operated in the hyphenated mode as a detection system coupled with different separation modules is presented. Its technical setup is described in detail. Its main feature is the very low total argon consumption of less than 1.5 L min- 1, leading to significant reduction of operational costs especially when time-consuming speciation analysis is performed. The figures of merit of the new system with respect to sensitivity, detection power, long-term stability and working range were explored. Despite the profound differences of argon consumption of the new system in comparison to the conventional ICP-MS system, many of the characteristic features of the conventional ICP-MS could be maintained to a great extent. To demonstrate the ion source's capabilities, it was used as an element-selective detector for gas (GC) and high performance liquid chromatography (HPLC) where organic compounds of mercury and cobalt, respectively, were separated and detected with the new low-flow ICP-MS detection system. The corresponding chromatograms are shown. The applicability for trace element analysis has been validated with the certified reference material NIST 1643e.

  9. Simultaneous measurement of {sup 239}Pu, {sup 240}Pu, {sup 241}Pu, and {sup 242}Pu by high resolution inductively coupled plasma mass spectrometer (HR ICP-MS) in marine sediments; Mesure des isotopes du plutonium des sediments marins par spectrometrie de masse a plasma couple inductivement haute resolution (HR ICP-MS)

    Energy Technology Data Exchange (ETDEWEB)

    Bruneau, F

    1999-07-01

    Transuranics elements are of particular interest in radioecological studies because of their radiotoxicity and their potential use to decipher source fingerprints and transport processes. The simultaneous measurement of {sup 239}Pu, {sup 240}Pu, {sup 241}Pu, and {sup 242}Pu in environmental samples requires a specific chemical procedure. This work deals with an analytical procedure which yields a very high grade of purification of Pu suitable for ultra low level detection by HR ICP-MS, from marine sediments. After the elimination of major elements (Fe, Al, Mg...) by a first chromatographic separation, a new device of purification by solvent extraction and concentration by a second chromatographic separation is used to obtain a concentrated and high purified solution of plutonium. The chemical procedure have been validated on IAEA certified sediment samples and on sediment samples collected in the roads of Cherbourg which had been previously analysed by other techniques (a spectrometry and thermo-ionisation mass spectrometer). (author)

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

    Science.gov (United States)

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

    2017-09-25

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

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

    Science.gov (United States)

    Qu, W; Du, A; Zhao, D

    2001-10-31

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

  12. Selection of mode for the measurement of lead isotope ratios by inductively coupled plasma mass spectrometry and its application to milk powder analysis

    International Nuclear Information System (INIS)

    Dean, J.R.; Ebdon, L.; Massey, R.

    1987-01-01

    An investigation into the selection of the optimum mode for the measurement of isotope ratios in inductively coupled plasma mass spectrometry (ICP-MS) is reported, with particular reference to lead isotope ratios. Variation in the accuracy and precision achievable using the measurement modes of scanning and peak jumping are discussed. It is concluded that if sufficient sample and time are available, scanning gives best accuracy and precision. Isotope dilution analysis (IDA) has been applied to the measurement of the lead content of two dried milk powders of Australian and European origin introduced as slurries into ICP-MS. Differences in the lead isotope ratios in the two milk powders were investigated and the total lead content determined by IDA. Isotope dilution analysis permitted accurate data to be obtained with an RSD of 4.2% or milk powder containing less than 30 ng g -1 of lead. The ICP-MS technique is confirmed as a useful tool for IDA. (author)

  13. Mass spectrometry in grape and wine chemistry. Part II: The consumer protection.

    Science.gov (United States)

    Flamini, Riccardo; Panighel, Annarita

    2006-01-01

    Controls in food industry are fundamental to protect the consumer health. For products of high quality, warranty of origin and identity is required and analytical control is very important to prevent frauds. In this article, the "state of art" of mass spectrometry in enological chemistry as a consumer safety contribute is reported. Gas chromatography-mass spectrometry (GC/MS) and liquid-chromatography-mass spectrometry (LC/MS) methods have been developed to determine pesticides, ethyl carbamate, and compounds from the yeast and bacterial metabolism in wine. The presence of pesticides in wine is mainly linked to the use of dicarboxyimide fungicides on vineyard shortly before the harvest to prevent the Botrytis cinerea attack of grape. Pesticide residues are regulated at maximum residue limits in grape of low ppm levels, but significantly lower levels in wine have to be detected, and mass spectrometry offers effective and sensitive methods. Moreover, mass spectrometry represent an advantageous alternative to the radioactive-source-containing electron capture detector commonly used in GC analysis of pesticides. Analysis of ochratoxin A (OTA) in wine by LC/MS and multiple mass spectrometry (MS/MS) permits to confirm the toxin presence without the use of expensive immunoaffinity columns, or time and solvent consuming sample derivatization procedures. Inductively coupled plasma-mass spectrometry (ICP/MS) is used to control heavy metals contamination in wine, and to verify the wine origin and authenticity. Isotopic ratio-mass spectrometry (IRMS) is applied to reveal wine watering and sugar additions, and to determine the product origin and traceability.

  14. 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)

  15. Determination of trace amounts of rare-earth elements in highly pure neodymium oxide by sector field inductively coupled plasma mass spectrometry (ICP-SFMS) and high-performance liquid chromatography (HPLC) techniques

    Science.gov (United States)

    Pedreira, W. R.; Sarkis, J. E. S.; da Silva Queiroz, C. A.; Rodrigues, C.; Tomiyoshi, I. A.; Abrão, A.

    2003-02-01

    Recently rare-earth elements (REE) have received much attention in fields of geochemistry and industry. Rapid and accurate determinations of them are increasingly required as industrial demands expand. Sector field inductively coupled plasma mass spectrometry (ICP-SFMS) with high-performance liquid chromatography (HPLC) has been applied to the determination of REE. HR ICP-MS was used as an element-selective detector for HPLC in highly pure materials. The separation of REE with HPLC helped to avoid erroneous analytical results due to spectral interferences. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the HPLC/ICP-SFMS system using a concentration gradient methods. The detection limits with the HPLC/ICP-SFMS system were about 0.5-10 pg mL-1. The percentage recovery ranged from 90% to 100% for different REE. The %RSD of the methods varying between 2.5% and 4.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two highly pure neodymium oxides samples (IPEN and Johnson Matthey Company) were performed. In short, the IPEN's materials which are highly pure (>99.9%) were successfully analyzed without spectral interferences.

  16. Determination of trace amounts of rare-earth elements in highly pure neodymium oxide by sector field inductively coupled plasma mass spectrometry (ICP-SFMS) and high-performance liquid chromatography (HPLC) techniques

    International Nuclear Information System (INIS)

    Pedreira, W.R.; Sarkis, J.E.S.; Silva Queiroz, C.A. da; Rodrigues, C.; Tomiyoshi, I.A.; Abrao, A.

    2003-01-01

    Recently rare-earth elements (REE) have received much attention in fields of geochemistry and industry. Rapid and accurate determinations of them are increasingly required as industrial demands expand. Sector field inductively coupled plasma mass spectrometry (ICP-SFMS) with high-performance liquid chromatography (HPLC) has been applied to the determination of REE. HR ICP-MS was used as an element-selective detector for HPLC in highly pure materials. The separation of REE with HPLC helped to avoid erroneous analytical results due to spectral interferences. Sixteen elements (Sc, Y and 14 lanthanides) were determined selectively with the HPLC/ICP-SFMS system using a concentration gradient methods. The detection limits with the HPLC/ICP-SFMS system were about 0.5-10 pg mL -1 . The percentage recovery ranged from 90% to 100% for different REE. The %RSD of the methods varying between 2.5% and 4.5% for a set of five (n=5) replicates was found for the IPEN's material and for the certificate reference sample. Determination of trace REEs in two highly pure neodymium oxides samples (IPEN and Johnson Matthey Company) were performed. In short, the IPEN's materials which are highly pure (>99.9%) were successfully analyzed without spectral interferences

  17. Fundamental and methodological investigations for the improvement of elemental analysis by inductively coupled plasma mass soectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ebert, Christopher Hysjulien [Ames Lab., Ames, IA (United States)

    2012-01-01

    This dissertation describes a variety of studies meant to improve the analytical performance of inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation (LA) ICP-MS. The emission behavior of individual droplets and LA generated particles in an ICP is studied using a high-speed, high frame rate digital camera. Phenomena are observed during the ablation of silicate glass that would cause elemental fractionation during analysis by ICP-MS. Preliminary work for ICP torch developments specifically tailored for the improvement of LA sample introduction are presented. An abnormal scarcity of metal-argon polyatomic ions (MAr{sup +}) is observed during ICP-MS analysis. Evidence shows that MAr{sup +} ions are dissociated by collisions with background gas in a shockwave near the tip of the skimmer cone. Method development towards the improvement of LA-ICP-MS for environmental monitoring is described. A method is developed to trap small particles in a collodion matrix and analyze each particle individually by LA-ICP-MS.

  18. Microwave dissolution of plant tissue and the subsequent determination of trace lanthanide and actinide elements by inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Alvarado, J.S.; Neal, T.J.; Smith, L.L.; Erickson, M.D.

    1997-01-01

    Recently there has been much concern with the ability of plants to uptake heavy metals from their surroundings. With the development of instrumental techniques with low detection limits such as inductively coupled plasma-mass spectrometry (ICP-MS), attention is shifting toward achieving faster and more elegant ways of oxidizing the organic material inherent in environmental samples. Closed-vessel microwave dissolution was compared with conventional methods for the determination of concentrations of cerium, samarium, europium, terbium, uranium and thorium in a series of samples from the National Institute of Standards and Technology and from fields in Idaho. The ICP-MS technique exhibited detection limits in parts-per-trillion and linear calibration plots over three orders of magnitude for the elements under study. The results obtained by using nitric acid and hydrogen peroxide in a microwave digestion system for the analysis of reference materials showed close agreement with the accepted values. These values were compared with results obtained from dry- and wet-ashing procedures. The findings from an experiment comparing radiometric techniques for the determination of actinide elements to ICP-MS are reported

  19. Fast Determination of Toxic Arsenic Species in Food Samples Using Narrow-bore High-Performance Liquid-Chromatography Inductively Coupled Plasma Mass Spectrometry.

    Science.gov (United States)

    Terol, Amanda; Marcinkowska, Monika; Ardini, Francisco; Grotti, Marco

    2016-01-01

    A new method for the speciation analysis of arsenic in food using narrow-bore high-performance liquid-chromatography inductively coupled plasma mass spectrometry (HPLC-ICP-MS) has been developed. Fast separation of arsenite, arsenate, monomethylarsonic acid and dimethylarsinic acid was carried out in 7 min using an anion-exchange narrow-bore Nucleosil 100 SB column and 12 mM ammonium dihydrogen phosphate of pH 5.2 as the mobile phase, at a flow rate of 0.3 mL min(-1). A PFA-ST micronebulizer jointed to a cyclonic spray chamber was used for HPLC-ICP-MS coupling. Compared with standard-bore HPLC-ICP-MS, the new method has provided higher sensitivity, reduced mobile-phase consumption, a lower matrix plasma load and a shorter analysis time. The achieved instrumental limits of detection were in the 0.3 - 0.4 ng As mL(-1) range, and the precision was better than 3%. The arsenic compounds were efficiently (>80%) extracted from various food samples using a 1:5 methanol/water solution, with additional ultrasonic treatment for rice products. The applicability of this method was demonstrated by the analysis of several samples, such as seafood (fish, mussels, shrimps, edible algae) and rice-based products (Jasmine and Arborio rice, spaghetti, flour, crackers), including three certified reference materials.

  20. 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.

  1. Development of routines for simultaneous in situ chemical composition and stable Si isotope ratio analysis by femtosecond laser ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Frick, Daniel A., E-mail: dfrick@gfz-potsdam.de [GFZ German Research Centre for Geosciences, 14473 Potsdam (Germany); Schuessler, Jan A. [GFZ German Research Centre for Geosciences, 14473 Potsdam (Germany); Blanckenburg, Friedhelm von [GFZ German Research Centre for Geosciences, 14473 Potsdam (Germany); Institute of Geological Science, Freie Universität Berlin, 12249 Berlin (Germany)

    2016-09-28

    Stable metal (e.g. Li, Mg, Ca, Fe, Cu, Zn, and Mo) and metalloid (B, Si, Ge) isotope ratio systems have emerged as geochemical tracers to fingerprint distinct physicochemical reactions. These systems are relevant to many Earth Science questions. The benefit of in situ microscale analysis using laser ablation (LA) over bulk sample analysis is to use the spatial context of different phases in the solid sample to disclose the processes that govern their chemical and isotopic compositions. However, there is a lack of in situ analytical routines to obtain a samples' stable isotope ratio together with its chemical composition. Here, we evaluate two novel analytical routines for the simultaneous determination of the chemical and Si stable isotope composition (δ{sup 30}Si) on the micrometre scale in geological samples. In both routines, multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is combined with femtosecond-LA, where stable isotope ratios are corrected for mass bias using standard-sample-bracketing with matrix-independent calibration. The first method is based on laser ablation split stream (LASS), where the laser aerosol is split and introduced simultaneously into both the MC-ICP-MS and a quadrupole ICP-MS. The second method is based on optical emission spectroscopy using direct observation of the MC-ICP-MS plasma (LA-MC-ICP-MS|OES). Both methods are evaluated using international geological reference materials. Accurate and precise Si isotope ratios were obtained with an uncertainty typically better than 0.23‰, 2SD, δ{sup 30}Si. With both methods major element concentrations (e.g., Na, Al, Si, Mg, Ca) can be simultaneously determined. However, LASS-ICP-MS is superior over LA-MC-ICP-MS|OES, which is limited by its lower sensitivity. Moreover, LASS-ICP-MS offers trace element analysis down to the μg g{sup −1}-range for more than 28 elements due to lower limits of detection, and with typical uncertainties better than 15%. For in situ

  2. Development of routines for simultaneous in situ chemical composition and stable Si isotope ratio analysis by femtosecond laser ablation inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Frick, Daniel A.; Schuessler, Jan A.; Blanckenburg, Friedhelm von

    2016-01-01

    Stable metal (e.g. Li, Mg, Ca, Fe, Cu, Zn, and Mo) and metalloid (B, Si, Ge) isotope ratio systems have emerged as geochemical tracers to fingerprint distinct physicochemical reactions. These systems are relevant to many Earth Science questions. The benefit of in situ microscale analysis using laser ablation (LA) over bulk sample analysis is to use the spatial context of different phases in the solid sample to disclose the processes that govern their chemical and isotopic compositions. However, there is a lack of in situ analytical routines to obtain a samples' stable isotope ratio together with its chemical composition. Here, we evaluate two novel analytical routines for the simultaneous determination of the chemical and Si stable isotope composition (δ 30 Si) on the micrometre scale in geological samples. In both routines, multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is combined with femtosecond-LA, where stable isotope ratios are corrected for mass bias using standard-sample-bracketing with matrix-independent calibration. The first method is based on laser ablation split stream (LASS), where the laser aerosol is split and introduced simultaneously into both the MC-ICP-MS and a quadrupole ICP-MS. The second method is based on optical emission spectroscopy using direct observation of the MC-ICP-MS plasma (LA-MC-ICP-MS|OES). Both methods are evaluated using international geological reference materials. Accurate and precise Si isotope ratios were obtained with an uncertainty typically better than 0.23‰, 2SD, δ 30 Si. With both methods major element concentrations (e.g., Na, Al, Si, Mg, Ca) can be simultaneously determined. However, LASS-ICP-MS is superior over LA-MC-ICP-MS|OES, which is limited by its lower sensitivity. Moreover, LASS-ICP-MS offers trace element analysis down to the μg g −1 -range for more than 28 elements due to lower limits of detection, and with typical uncertainties better than 15%. For in situ

  3. Applications of plasma spectrometry and high performance liquid chromatography in environmental and food science

    International Nuclear Information System (INIS)

    Iordache, Andreea-Maria; Biraruti, Elisabeta-Irina; Ionete, Roxana-Elena

    2008-01-01

    Full text: Plasma spectrometry has many applications in food science in analysis of a wide range of samples in the food chain. Food science in the broadest sense can be extended to include soil chemistry, plant uptake and, at the other end of the food chain, studies into the metabolic fate of particular elements or elemental species when the foods are consumed by humans or animals. Inductively Coupled Plasma Mass Spectrometry allows multi-element measurements of most elements in the periodic table. A very sensitive analytical technique for trace analysis of samples can be performed by inductively plasma mass spectrometer with quadrupolar detector using ultrasonic nebulization. High Performance Liquid Chromatography (HPLC) is an analytical technique for the separation and determination of organic and inorganic solutes in any samples especially biological, pharmaceutical, food, environmental. The present paper emphasizes that the future tendencies HPLC-ICP-MS is often the preferred analytical technique for these applications due to the simplicity of the coupling between the HPLC and ICP-MS Varian 820 using ultrasonic nebulization, potential for on-line separations with high species specificity and the capability for optimum limits of detection without the necessity of using complex hydride generation mechanisms. (authors)

  4. 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.

  5. Controlled Dissolution of Surface Layers for Elemental Analysis by Inductively Coupled Plasma-Mass Spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lorge, Susan Elizabeth [Iowa State Univ., Ames, IA (United States)

    2007-01-01

    Determining the composition of thin layers is increasingly important for a variety of industrial materials such as adhesives, coatings and microelectronics. Secondary ion mass spectrometry (SIMS), Auger electron spectroscopy (AES), X-ray photoelectron spectroscopy (XPS), glow discharge optical emission spectroscopy (GDOES), glow discharge mass spectrometry (GDMS), and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) are some of the techniques that are currently employed for the direct analysis of the sample surface. Although these techniques do not suffer from the contamination problems that often plague sample dissolution studies, they do require matrix matched standards for quantification. Often, these standards are not readily available. Despite the costs of clean hoods, Teflon pipette tips and bottles, and pure acids, partial sample dissolution is the primary method used in the semiconductor industry to quantify surface impurities. Specifically, vapor phase decomposition (VPD) coupled to ICP-MS or total reflection x-ray fluorescence (TXRF) provides elemental information from the top most surface layers at detection sensitivities in the 107-1010atoms/cm2 range. The ability to quantify with standard solutions is a main advantage of these techniques. Li and Houk applied a VPD-like technique to steel. The signal ratio of trace element to matrix element was used for quantification. Although controlled dissolution concentrations determined for some of the dissolved elements agreed with the certified values, concentrations determined for refractory elements (Ti, Nb and Ta) were too low. LA-ICP-MS and scanning electron microscopy (SEM) measurements indicated that carbide grains distributed throughout the matrix were high in these refractory elements. These elements dissolved at a slower rate than the matrix element, Fe. If the analyte element is not removed at a rate similar to the matrix element a true

  6. 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.

  7. Determination of reduced homocysteine in human serum by elemental labelling and liquid chromatography with ICP-MS and ESI-MS detection.

    Science.gov (United States)

    Espina, Juan Gómez; Montes-Bayón, Maria; Blanco-González, Elisa; Sanz-Medel, Alfredo

    2015-10-01

    Analytical methods allowing sensitive determination of reduced homocysteine (rHcy), one of the so-called biothiols, in human serum is a topic of growing interest due to its close relation to several human disorders, mainly cardiovascular diseases. Although most widely used analytical strategies to determine total Hcy involve derivatization by means of fluorescent labels, this work proposes the use of ebselen, a Se-containing labelling agent to derivatize the reactive sulfhydryl group of the Hcy molecule in its "free" reduced form, which is more likely to play different roles in disease pathogenesis. Optimization of the derivatization and separation conditions by high-performance liquid chromatography (HPLC) to isolate the excess of derivatizing reagent is carried out here using UV/VIS detection. Further, the study of the Se labelling reaction by electrospray ionization tandem mass spectrometry (ESI-MS/MS) provides a stoichiometry of the derivative of 1:1. The main advantage of using ebselen as a labelling agent is the presence of the Se atom in the molecule that allows the use of inductively coupled plasma mass spectrometry (ICP-MS) as a sensitive and selective Se detector. The coupling of HPLC with ICP-MS provided excellent features for the determination of Se-derivatized rHcy (detection limit of 9.6 nM) in real samples. Quantification was accomplished by using post-column isotope dilution (ID) of Se in serum samples, after precipitation of the main serum proteins. Quantitative results for "free" rHcy turned out to be around 0.18-0.22 μM in serum samples from healthy individuals that could be directly analyzed without sample preconcentration.

  8. Hybrid Imaging Labels: Providing the Link Between Mass Spectrometry-Based Molecular Pathology and Theranostics

    Science.gov (United States)

    Buckle, Tessa; van der Wal, Steffen; van Malderen, Stijn J.M.; Müller, Larissa; Kuil, Joeri; van Unen, Vincent; Peters, Ruud J.B.; van Bemmel, Margaretha E.M.; McDonnell, Liam A.; Velders, Aldrik H.; Koning, Frits; Vanhaeke, Frank; van Leeuwen, Fijs W. B.

    2017-01-01

    Background: Development of theranostic concepts that include inductively coupled plasma mass spectrometry (ICP-MS) and laser ablation ICP-MS (LA-ICP-MS) imaging can be hindered by the lack of a direct comparison to more standardly used methods for in vitro and in vivo evaluation; e.g. fluorescence or nuclear medicine. In this study a bimodal (or rather, hybrid) tracer that contains both a fluorescent dye and a chelate was used to evaluate the existence of a direct link between mass spectrometry (MS) and in vitro and in vivo molecular imaging findings using fluorescence and radioisotopes. At the same time, the hybrid label was used to determine whether the use of a single isotope label would allow for MS-based diagnostics. Methods: A hybrid label that contained both a DTPA chelate (that was coordinated with either 165Ho or 111In) and a Cy5 fluorescent dye was coupled to the chemokine receptor 4 (CXCR4) targeting peptide Ac-TZ14011 (hybrid-Cy5-Ac-TZ4011). This receptor targeting tracer was used to 1) validate the efficacy of (165Ho-based) mass-cytometry in determining the receptor affinity via comparison with fluorescence-based flow cytometry (Cy5), 2) evaluate the microscopic binding pattern of the tracer in tumor cells using both fluorescence confocal imaging (Cy5) and LA-ICP-MS-imaging (165Ho), 3) compare in vivo biodistribution patterns obtained with ICP-MS (165Ho) and radiodetection (111In) after intravenous administration of hybrid-Cy5-Ac-TZ4011 in tumor-bearing mice. Finally, LA-ICP-MS-imaging (165Ho) was linked to fluorescence-based analysis of excised tissue samples (Cy5). Results: Analysis with both mass-cytometry and flow cytometry revealed a similar receptor affinity, respectively 352 ± 141 nM and 245 ± 65 nM (p = 0.08), but with a much lower detection sensitivity for the first modality. In vitro LA-ICP-MS imaging (165Ho) enabled clear discrimination between CXCR4 positive and negative cells, but fluorescence microscopy was required to determine the

  9. 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

  10. 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)

  11. 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.

  12. Determination of serum calcium levels by 42Ca isotope dilution inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Han, Bingqing; Ge, Menglei; Zhao, Haijian; Yan, Ying; Zeng, Jie; Zhang, Tianjiao; Zhou, Weiyan; Zhang, Jiangtao; Wang, Jing; Zhang, Chuanbao

    2017-11-27

    Serum calcium level is an important clinical index that reflects pathophysiological states. However, detection accuracy in laboratory tests is not ideal; as such, a high accuracy method is needed. We developed a reference method for measuring serum calcium levels by isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS), using 42Ca as the enriched isotope. Serum was digested with 69% ultrapure nitric acid and diluted to a suitable concentration. The 44Ca/42Ca ratio was detected in H2 mode; spike concentration was calibrated by reverse IDMS using standard reference material (SRM) 3109a, and sample concentration was measured by a bracketing procedure. We compared the performance of ID ICP-MS with those of three other reference methods in China using the same serum and aqueous samples. The relative expanded uncertainty of the sample concentration was 0.414% (k=2). The range of repeatability (within-run imprecision), intermediate imprecision (between-run imprecision), and intra-laboratory imprecision were 0.12%-0.19%, 0.07%-0.09%, and 0.16%-0.17%, respectively, for two of the serum samples. SRM909bI, SRM909bII, SRM909c, and GBW09152 were found to be within the certified value interval, with mean relative bias values of 0.29%, -0.02%, 0.10%, and -0.19%, respectively. The range of recovery was 99.87%-100.37%. Results obtained by ID ICP-MS showed a better accuracy than and were highly correlated with those of other reference methods. ID ICP-MS is a simple and accurate candidate reference method for serum calcium measurement and can be used to establish and improve serum calcium reference system in China.

  13. 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.

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

    International Nuclear Information System (INIS)

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

    1997-01-01

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

  15. New high temperature plasmas and sample introduction systems for analytical atomic emission and mass spectrometry

    International Nuclear Information System (INIS)

    Montaser, A.

    1993-01-01

    In this research, new high-temperature plasmas and new sample introduction systems are explored for rapid elemental and isotopic analysis of gases, solutions, and solids using mass spectrometry and atomic emission spectrometry. During the period January 1993--December 1993, emphasis was placed on (a) analytical investigations of atmospheric-pressure helium inductively coupled plasma (He ICP) that are suitable for atomization, excitation, and ionization of elements possessing high excitation and ionization energies; (b) simulation and computer modeling of plasma sources to predict their structure and fundamental and analytical properties without incurring the enormous cost of experimental studies; (c) spectrosopic imaging and diagnostic studies of high-temperature plasmas; (d) fundamental studies of He ICP discharges and argon-nitrogen plasma by high-resolution Fourier transform spectrometry; and (e) fundamental and analytical investigation of new, low-cost devices as sample introduction systems for atomic spectrometry and examination of new diagnostic techniques for probing aerosols. Only the most important achievements are included in this report to illustrate progress and obstacles. Detailed descriptions of the authors' investigations are outlined in the reprints and preprints that accompany this report. The technical progress expected next year is briefly described at the end of this report

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

    Science.gov (United States)

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

    2007-11-28

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

  17. Time-resolved studies of particle effects in laser ablation inductively coupled plasma-mass spectrometry. Part 2: Investigation of MO+ ions, effect of sample morphology, transport gas, and binding agents

    International Nuclear Information System (INIS)

    Perdian, D.; Bajic, S.; Baldwin, D.; Houk, R.

    2007-01-01

    Time resolved signals in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) are studied to determine the influence of experimental parameters on ICP-induced fractionation effects. Differences in sample composition and morphology, i.e., ablating brass, glass, or dust pellets, have a profound effect on the time resolved signal. Helium transport gas significantly decreases large positive signal spikes arising from large particles in the ICP. A binder for pellets also reduces the abundance and amplitude of spikes in the signal. MO + ions also yield signal spikes, but these MO + spikes generally occur at different times from their atomic ion counterparts.

  18. 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

  19. Determination of rare earth elements by liquid chromatographic separation using inductively coupled plasma mass spectrometric detection

    International Nuclear Information System (INIS)

    Braverman, D.S.

    1992-01-01

    High-performance liquid chromatography (HPLC) is used to separate the rare earth elements (REEs) prior to detection by inductively coupled plasma mass spectrometry (ICP-MS). The use of HPLC-ICP-MS in series combines the separation power and speed of HPLC with the sensitivity, isotopic selectivity and speed of ICP-MS. The detection limits for the REEs are in the sub-ng ml -1 range and the response is linear over four orders of magnitude. A preliminary comparison of isotope dilution and external standard results for the determination of REEs in National Institute of Standards and Technology (NIST) Standard Reference Material (SRM 1633a) Fly Ash is presented. (author)

  20. Method optimization and quality assurance in speciation analysis using high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt

    1998-01-01

    Achievement of optimum selectivity, sensitivity and robustness in speciation analysis using high performance liquid chromatography (HPLC) with inductively coupled mass spectrometry (ICP-MS) detection requires that each instrumental component is selected and optimized with a view to the ideal....... The optimized anion and cation exchange HPLC-ICP-MS systems were used for arsenic speciation in contaminated ground water and in an in-house shrimp reference sample. For the purpose of verification, HPLC coupled with tandem mass spectrometry with electrospray ionization was additionally used for arsenic...... a mass balance of the analytes in each fraction of the extraction procedure, by recovery of spikes and by employing and comparing independent techniques. The urgent need for reference materials certified for elemental species is stressed....

  1. Multielement determination of major-to-ultratrace elements in plant reference materials by ICP-AES/ICP-MS and evaluation of their enrichment factors

    International Nuclear Information System (INIS)

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

    2000-01-01

    The multielement determination of major-to-ultratrace elements in plant reference materials (SRM Pine Needles, SRM Tomato Leaves, and NIES Tea Leaves) was carried out by ICP-AES (inductively coupled plasma atomic emission spectrometry) and ICP-MS (inductively coupled plasma mass spectrometry). The plant sample was decomposed with nitric acid and hydrofluoric acid in a Teflon beaker on a hot plate. The digest was dissolved in 1 M HNO 3 solution, and then subjected to elemental analyses. As a consequence, the analytical data for about 40 elements including rare earth elements (REEs) were obtained over a wide concentration range, for example, from 49600 μg g -1 of Ca to 6.2 ng g -1 of Lu in Tomato Leaves. The enrichment factors, which were estimated by normalizing the observed concentrations of analyte elements in plant reference materials to their soil abundances, were evaluated in order to discuss the relative abundances of various elements between plants and soil. It was found that most of the elements, except for REEs in Pine Needles and Tea Leaves, were significantly accumulated in the plant reference materials. In particular, the essential elements (K, Mg, Ca, Mn, Cu, Zn, B and P) for plant growth provided large enrichment factors. (author)

  2. Trace Element Analysis of Minerals in Magmatic-Hydrothermal Ores by Laser Ablation Inductively-Coupled Plasma Mass Spectrometry: Approaches and Opportunities

    Directory of Open Access Journals (Sweden)

    Nigel Cook

    2016-10-01

    Full Text Available Laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS has rapidly established itself as the method of choice for generation of multi-element datasets for specific minerals, with broad applications in Earth science. Variation in absolute concentrations of different trace elements within common, widely distributed phases, such as pyrite, iron-oxides (magnetite and hematite, and key accessory minerals, such as apatite and titanite, can be particularly valuable for understanding processes of ore formation, and when trace element distributions vary systematically within a mineral system, for a vector approach in mineral exploration. LA-ICP-MS trace element data can assist in element deportment and geometallurgical studies, providing proof of which minerals host key elements of economic relevance, or elements that are deleterious to various metallurgical processes. This contribution reviews recent advances in LA-ICP-MS methodology, reference standards, the application of the method to new mineral matrices, outstanding analytical uncertainties that impact on the quality and usefulness of trace element data, and future applications of the technique. We illustrate how data interpretation is highly dependent on an adequate understanding of prevailing mineral textures, geological history, and in some cases, crystal structure.

  3. Determination of uranium isotopic composition and 236U content of soil samples and hot particles using inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Boulyga, S F; Becker, J S

    2001-07-01

    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The 236U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. Nuclear track radiography was applied for the identification and extraction of hot radioactive particles from soil samples. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on double-focusing inductively coupled plasma mass spectrometry (DF-ICP-MS) with a MicroMist nebulizer and a direct injection high-efficiency nebulizer (DIHEN). The performance of the DF-ICP-MS with a quartz DIHEN and plasma shielded torch was studied. Overall detection efficiencies of 4 x 10(-4) and 10(-3) counts per atom were achieved for 238U in DF-ICP-QMS with the MicroMist nebulizer and DIHEN, respectively. The rate of formation of uranium hydride ions UH+/U+ was 1.2 x 10(-4) and 1.4 x 10(-4), respectively. The precision of short-term measurements of uranium isotopic ratios (n = 5) in 1 microg L(-1) NBS U-020 standard solution was 0.11% (238U/235U) and 1.4% (236U/238U) using a MicroMist nebulizer and 0.25% (235U/238U) and 1.9% (236U/P38U) using a DIHEN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the 236U/238U ratio ranged from 10(-5) to 10(-3). Results obtained with ICP-MS, alpha- and gamma-spectrometry showed differences in the migration properties of spent uranium, plutonium, and americium. The isotopic ratio of uranium was also measured in hot particles extracted from soil samples.

  4. Determination of uranium isotopic composition and 236U content of soil samples and hot particles using inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Boulyga, S.F.; Becker, J.S.

    2001-01-01

    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The 236 U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. Nuclear track radiography was applied for the identification and extraction of hot radioactive particles from soil samples. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on double-focusing inductively coupled plasma mass spectrometry (DF-ICP-MS) with a MicroMist nebulizer and a direct injection high-efficiency nebulizer (DIHEN). The performance of the DF-ICP-MS with a quartz DIHEN and plasma shielded torch was studied. Overall detection efficiencies of 4 x 10 -4 and 10 -3 counts per atom were achieved for 238 U in DF-ICP-QMS with the MicroMist nebulizer and DIHEN, respectively. The rate of formation of uranium hydride ions UH + /U + was 1.2 x 10 -4 and 1.4 x 10 -4 , respectively. The precision of short-term measurements of uranium isotopic ratios (n = 5) in 1 μg L -1 NBS U-020 standard solution was 0.11% ( 238 U/ 235 U) and 1.4% ( 236 U/ 238 U) using a MicroMist nebulizer and 0.25% ( 235 U/ 238 U) and 1.9% ( 236 U/ 238 U) using a DIHEN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the 236 U/ 238 U ratio ranged from 10 -5 to 10 -3 . Results obtained with ICP-MS, α- and γ-spectrometry showed differences in the migration properties of spent uranium, plutonium, and americium. The isotopic ratio of uranium was also measured in hot particles extracted from soil samples. (orig.)

  5. Electrothermal vaporization inductively coupled plasma-mass spectrometry for the determination of Cr, Cu, Cd, Hg and Pb in rice flour

    International Nuclear Information System (INIS)

    Li, P.-C.; Jiang, S.-J.

    2003-01-01

    Ultrasonic slurry sampling (USS)-electrothermal vaporization (ETV) dynamic reaction cell TM (DRC) inductively coupled plasma-mass spectrometry (ICP-MS) has been applied to determine Cr, Cu, Cd, Hg and Pb in rice samples. The influences of instrument operating conditions and slurry preparation on the ion signals were reported. Ascorbic acid was used as a modifier to enhance the ion signals. The background ions at the chromium masses were reduced in intensity significantly by using 0.4 ml min -1 NH 3 as reaction cell gas in the dynamic reaction cell while a q value of 0.6 was used. Since the sensitivities of Cr, Cu, Cd, Hg and Pb in rice flour slurry and aqueous solution were quite different, standard addition and isotope dilution methods were used for the determination of Cr, Cu, Cd, Hg and Pb in these rice samples. This method has been applied to the determination of Cr, Cu, Cd, Hg and Pb in NIST SRM 1568a rice flour reference material and two rice samples purchased from the market. The analytical results for the reference material agreed with the certified values. The results for the rice samples for which no reference values were available were also found to be in good agreement between the isotope dilution and standard addition methods. The method's detection limits estimated from the standard addition plots were about 0.44, 1.7, 0.4, 0.53 and 0.69 ng g -1 for Cr, Cu, Cd, Hg and Pb, respectively, in the original rice flour

  6. Inductively coupled plasma mass spectrometry in the analysis of biological samples and pharmaceutical drugs

    Science.gov (United States)

    Ossipov, K.; Seregina, I. F.; Bolshov, M. A.

    2016-04-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is widely used in the analysis of biological samples (whole blood, serum, blood plasma, urine, tissues, etc.) and pharmaceutical drugs. The shortcomings of this method related to spectral and non-spectral interferences are manifested in full measure in determination of the target analytes in these complex samples strongly differing in composition. The spectral interferences are caused by similarity of masses of the target component and sample matrix components. Non-spectral interferences are related to the influence of sample matrix components on the physicochemical processes taking place during formation and transportation of liquid sample aerosols into the plasma, on the value and spatial distribution of plasma temperature and on the transmission of the ion beam from the interface to mass spectrometer detector. The review is devoted to analysis of different mechanisms of appearance of non-spectral interferences and to ways for their minimization or elimination. Special attention is paid to the techniques of biological sample preparation, which largely determine the mechanisms of the influence of sample composition on the results of element determination. The ways of lowering non-spectral interferences by instrumental parameter tuning and application of internal standards are considered. The bibliography includes 189 references.

  7. Inductively coupled plasma mass spectrometry with hexapole collision cell: figures of merit and applications

    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

    The use of gas-filled multipole collision cells represents important progress in ICP-MS instrumentation. It enables an increase in element sensitivity based on the improvement of ion transmission efficiency from near thermalization and collisional focusing of ions. In addition, gas-phase ion-molecule chemistry can be applied in order to reduce mass spectral interferences via charge transfer reaction of interfering ions with reaction gas or via fragmentation of interfering molecular ions by collision-induced dissociation. The application of a hexapole collision cell in quadrupole based ICP-MS (HEX-ICP-QMS) was studied systematically in order to characterize the analytical figures of merit of this approach. Additionally, the performance of different solution introduction systems as well as an inductively coupled plasma shielded torch was studied for use with HEX-ICP-QMS. (orig.)

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

    Science.gov (United States)

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

    2018-01-01

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

  9. 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.

  10. Analysis of liquid samples using dried-droplet laser ablation inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Do, Trong-Mui; Hsieh, Hui-Fang; Chang, Wei-Ciang [Department of Biomedical Engineering and Environmental Sciences, National Tsing Hua University, Hsinchu, 30013 Taiwan (China); Chang, E.-E. [Department of Biochemistry, Taipei Medical University, Taipei City, 11031 Taiwan (China); Wang, Chu-Fang, E-mail: cfwang@mx.nthu.edu.tw [Department of Biomedical Engineering and Environmental Sciences, National Tsing Hua University, Hsinchu, 30013 Taiwan (China); Institute of Nuclear Engineering and Science, National Tsing Hua University, Hsinchu 30013, Taiwan (China)

    2011-08-15

    In this study we developed a dried-droplet method for laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method provides accurate and precise results when building calibration curves and determining elements of interest in real liquid samples. After placing just 1 {mu}L of a liquid standard solution or a real sample onto the filter surface and then converting the solution into a very small, thin dry spot, the sample could be applied as an analytical subject for LA. To demonstrate the feasibility of this proposed method, we used LA-ICP-MS and conventional ICP-MS to determine the levels of 13 elements (Li, V, Mn, Co, Ni, Cu, Zn, As, Mo, Cd, Sb, Tl, and Pb) in five water samples. The correlation coefficients obtained from the various calibration curves ranged from 0.9920 ({sup 205}Tl) to 0.9998 ({sup 51}V), sufficient to allow the determination of a wide range of elements in the samples. We also investigated the effects of Methylene Blue (MB) and the NaCl concentration on the elemental analyses. MB could be used as an indicator during the ablation process; its presence in the samples only negligibly influenced the intensities of the signals of most of the tested elements. Notably, high NaCl contents led to signal suppression for some of the elements. In comparison with the established sample introduction by nebulization, our developed technique abrogates the need for time-consuming sample preparation and reduces the possibility of sample contamination.

  11. 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.

  12. 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)

  13. Flow injection analysis in inductively coupled plasma spectrometry

    International Nuclear Information System (INIS)

    Rosias, Maria F.G.G.

    1995-10-01

    The main features of flow injection analysis (FIA) as contribution to the inductively coupled plasma (Icp) spectrometry are described. A systematic review of researches using the combined FIA-Icp and the benefits of this association are presented. Flow systems were proposed to perform on-line Icp solution management for multielemental determination by atomic emission spectrometry (Icp-AES) or mass spectrometry. The inclusion of on-line ion exchangers in flow systems for matrix separation and/or analyte preconcentration are presented. Together with those applications the new advent of instruments with facilities for multielement detection on flow injection signals are described. (author). 75 refs., 19 figs

  14. 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

  15. Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

    Science.gov (United States)

    Kowalewska, Zofia; Ruszczyńska, Anna; Bulska, Ewa

    2005-03-01

    Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system, (ii) mineralization in a closed microwave system, (iii) combustion in hydrogen-oxygen flame in the Wickbold's apparatus, (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g - 1 in procedures i-v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g - 1 in procedures i-iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50-110 ng g - 1 in crude oil, oil, oil and 140-300 ng g - 1 in distillation residue.

  16. Heavy metals in aromatic spices by inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Bua, Daniel Giuseppe; Annuario, Giovanni; Albergamo, Ambrogina; Cicero, Nicola; Dugo, Giacomo

    2016-09-01

    Objective of this study was to determine the content of Cd, Hg, As and Pb in common spices traded in the Italian market, using inductively coupled plasma-mass spectrometry (ICP-MS). The results were compared with the maximum limits established by the national Legislative Decree (LD) no. 107 implementing the Council Directive 88/388/EEC and by international organisations, such as Food and Agriculture Organization (FAO) and World Health Organization (WHO). Food safety for spices was assessed considering the tolerable weekly intake (TWI) and the provisional tolerable weekly intake (PTWI), respectively, for Cd and Hg and the 95% lower confidence limit of the benchmark dose of 1% extra risk (BMDL01) for As and Pb. Investigated elements in all samples were within the maximum limits as set by the national and international normative institutions. Nevertheless, the heavy metal content of some spices exceeded the PTWI, TWI and BMDL01, which needs attention when considering consumer's health.

  17. Analysis of corrosions-products in tissue samples near surgical implants by means of LAMMA (Laser Microprobe Mass Analyzer) and ICP-MS (Inductively Coupled Plasma Mass Spectrometer)

    International Nuclear Information System (INIS)

    Schlagenhaufen, C.

    1996-08-01

    In this work corrosion products of surgical implants in tissue samples were identified. For the characterization of the corrosion products the LAMMA 500 (Laser Microprobe Mass Analyzer) was used. Additional analysis were made with the ICP-MS (Inductively Coupled Plasma Mass Spectrometer) to determine the concentration of chromium, cobalt, nickel, and molybdenum in the tissues. In the first part several synthetic chromium- and molybdenum compounds were investigated with LAMMA. With the anionic mass spectra of the chromium-compounds it is possible to the oxidation state of chromium. The mass spectra of the synthetic compounds were used to identify, the compounds in the corrosion products. In the second part thin sections prepared from the tissue samples from the surrounding of the implants were analyzed. Several embedding and cutting methods were tested. Histological staining methods and LAMMA spectra were used to characterize the deposits in the tissue. Three different deposits were found in the tissue. In all tissues metal splinters from the implant were found. In most of the tissues iron-rich deposits were found, that were identified as iron-phosphate. As definitive corrosion products of the implant mixtures of chromium(III)phosphate, calcium molybdate, calcium phosphate and chromium(III) molybdate were identified. The ICP-MS results show in comparison to normal values, very high concentrations for chromium, nickel, cobalt and molybdenum. These results support the conclusions based on LAMMA results. The results of these investigations clearly indicate, that stainless steel implants, are not corrosion-resistant in the body. Relatively high amounts of the constituents, of the implant dissolved, and are deposited as solid compounds in the tissue next to the implant. (author)

  18. Investigation into the behavior of metal-argon polyatomic ions (MAr+) in the extraction region of inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Ebert, Chris H.; Witte, Travis M.; Houk, R.S.

    2012-01-01

    The abundances of metal-argon polyatomic ions (MAr + ) are determined in inductively coupled plasma-mass spectrometry (ICP-MS). The ratios of MAr + abundance to that for M + ions are measured experimentally. These ratios are compared to expected values, calculated for typical plasma conditions using spectroscopic data. For all metals studied (Ti, V, Cr, Mn, Fe, Co, Ni, Cu, and Zn), the measured ratios are significantly lower than the calculated ratios. Increasing the plasma potential (and thereby increasing the ion kinetic energy) by means of a homemade guard electrode with a wide gap further reduces the MAr + /M + ratio. Implementing a skimmer cone designed for high transmission of light ions increases the MAr + abundance. Considering this evidence, the scarcity of MAr + ions is attributed to collision induced dissociation (CID), likely due to a shock wave at the tip of or in the throat of the skimmer cone. - Highlights: ► MAr + ions are less abundant in the mass spectrum than expected from the ICP. ► Increasing the plasma potential reduces their abundance further. ► The extraction lens voltage does not greatly affect the MAr + abundances. ► The weakly-bound MAr + ions are probably dissociated by collisions during extraction.

  19. 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.

  20. Validation of methods to measure uranium isotopes using magnetic sector mass spectrometry with inductively coupled plasma source; Validacion de metodos para medir isotopos de uranio usando espectrometria de masas de sector magnetico con fuente de plasma acoplado inductivamente

    Energy Technology Data Exchange (ETDEWEB)

    Hernandez M, H. [Universidad del Centro de Mexico, Capitan Caldera 75, Col. Tequixquiapan, 78250 San Luis Potosi, SLP (Mexico); Rios L, M. J. [Universidad Autonoma de San Luis Potosi, Facultad de Enfermeria y Nutricion, Unidad de Posgrado, Av. Nino Artillero 130, 78210 San Luis Potosi, SLP (Mexico); Romero G, E. T., E-mail: hector.hernandez520@gmail.com [ININ, Departamento de Quimica, Laboratorio Forense Nuclear, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico)

    2017-10-15

    The mass spectrometry technique with inductively coupled plasma source (Icp-Ms) has been widely used to measure isotopic ratios of elements toxic to human health. Reason for which, in this work several measurement methods for the analysis of uranium isotopes in different matrices were implemented using magnetic sector mass spectrometry with inductively coupled plasma source (Icp-SFMS). Groundwater, sediment, soil and urine were the matrices analyzed, which were supplied by intercomparison tests conducted by the IAEA and Association for the Promotion of Quality Control of Medical Biology Analysis in Radio-toxicology. The procedures used in the treatment of soil, sediment and water samples were based on US EPA methods. In the case of the urine sample, the preparation was rapid (1:20 dilution). The average of the results obtained in yield of each matrix was 94, 71, 72 and 78% for water, urine, soil and sediment respectively. In addition, the precision in terms of standard relative deviation was less than 5% and the accuracy was less than 4%. In conclusion, the Icp-SFMS is a very sensitive technique for measuring isotopes of U in different matrices. However, careful tuning is necessary, especially in the mass regions of interest 234, 235 and 238 if an external quantification is considered using natural U solutions. (Author)

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  2. [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.

  3. Elemental mapping in fossil tooth root section of Ursus arctos by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS)

    Czech Academy of Sciences Publication Activity Database

    Vašinová Galiová, M.; Nývltová Fišáková, Miriam; Kynický, J.; Prokeš, L.; Neff, H.; Mason, A. Z.; Gadas, P.; Košler, J.; Kanický, V.

    2013-01-01

    Roč. 105, 15 February 2013 (2013), s. 235-243 ISSN 0039-9140 Institutional research plan: CEZ:AV0Z80010507 Institutional support: RVO:68081758 Keywords : Diagenesis * Diet * Geochemical analysis * Laser ablation ICP-MS * Migration Subject RIV: AC - Archeology, Anthropology, Ethnology Impact factor: 3.511, year: 2013

  4. Metal-doped inorganic nanoparticles for multiplex detection of biomarkers by a sandwich-type ICP-MS immunoassay.

    Science.gov (United States)

    Ko, Jung Aa; Lim, H B

    2016-09-28

    Metal-doped inorganic nanoparticles were synthesized for the multiplex detection of biomarkers by a sandwich-type inductively coupled plasma mass spectrometry (ICP-MS) immunoassay. The synthesized Cs-doped multicore magnetic nanoparticles (MMNPs) were used not only for magnetic extraction of targets but also for ratiometric measurement in ICP-MS. In addition, three different metal/dye-doped silica nanoparticles (SNPs) were synthesized as probes for multiplex detection: Y/RhBITC (rhodamine B isothiocyanate)-doped SNPs for CRP (cardiovascular disease), Cd/RhBITC-doped SNPs for AFP (tumor), and Au/5(6)-XRITC (X-rhodamine-5-(and-6)-isothiocyanate)-doped SNPs for NSE (heart disease). For quantification, the doped metals of SNPs were measured by ICP-MS and then the signal ratio to Cs of MMNPs was plotted with respect to the concentration of targets by a ratiometry. Limits of detection (LOD) of 0.35 ng/mL to 77 ng mL(-1) and recoveries of 83%-125% were obtained for serum samples spiked with the biomarkers. Since no sample treatment was necessary prior to the extraction, the proposed method provided short analysis time and convenience for the multiplex determination of biomarkers, which will be valuable for clinical application. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Inductively coupled plasma as atomization, excitation and ionization sources in analytical atomic spectrometry

    International Nuclear Information System (INIS)

    Kawaguchi, Hiroshi

    1996-01-01

    Studies on inductively coupled plasma (ICP) for atomic emission and mass spectrometry accomplished in our laboratory since 1978 are reviewed. In emission spectrometry, the characteristics of the plasma are studied concerning the spatial profiles of spectral line intensity, axial profiles of gas and excitation temperatures, spectral line widths and matrix effect. The studies are particularly emphasized on the instrumentation such as developments of plasma generator, emission spectrometers, water-cooled torches and sample introduction methods. A slew-scan type spectrometer developed in these works represents a predecessor of the current commercial spectrometers. An ICP mass spectrometer was first developed in Japan in this laboratory in 1984. Non-spectroscopic interference of this method was found to have the correlation with the atomic weight of the matrix element. Plasma gases other than argon such as nitrogen and oxygen were used for the ICP to evaluate their performance in mass spectrometry as for the sensitivity and interferences. (author). 63 refs

  6. Determination of trace elements in petroleum products by inductively coupled plasma techniques: A critical review

    International Nuclear Information System (INIS)

    Sánchez, Raquel; Todolí, José Luis; Lienemann, Charles-Philippe; Mermet, Jean-Michel

    2013-01-01

    The fundamentals, applications and latter developments of petroleum products analysis through inductively coupled plasma optical emission spectrometry (ICP-OES) and mass spectrometry (ICP-MS) are revisited in the present bibliographic survey. Sample preparation procedures for the direct analysis of fuels by using liquid sample introduction systems are critically reviewed and compared. The most employed methods are sample dilution, emulsion or micro-emulsion preparation and sample decomposition. The first one is the most widely employed due to its simplicity. Once the sample has been prepared, an organic matrix is usually present. The performance of the sample introduction system (i.e., nebulizer and spray chamber) depends strongly upon the nature and properties of the solution finally obtained. Many different devices have been assayed and the obtained results are shown. Additionally, samples can be introduced into the plasma by using an electrothermal vaporization (ETV) device or a laser ablation system (LA). The recent results published in the literature showing the feasibility, advantages and drawbacks of latter alternatives are also described. Therefore, the main goal of the review is the discussion of the different approaches developed for the analysis of crude oil and its derivates by inductively coupled plasma (ICP) techniques. - Highlights: • Analysis of petroleum products by inductively coupled plasma techniques is revisited. • Fundamental studies are included together with reports dealing with applications. • Conventional and non-conventional sample introduction methods are considered. • Sample preparation methods are critically compared and described

  7. Sample Preprocessing For Atomic Spectrometry

    International Nuclear Information System (INIS)

    Kim, Sun Tae

    2004-08-01

    This book gives descriptions of atomic spectrometry, which deals with atomic absorption spectrometry such as Maxwell-Boltzmann equation and Beer-Lambert law, atomic absorption spectrometry for solvent extraction, HGAAS, ETASS, and CVAAS and inductively coupled plasma emission spectrometer, such as basic principle, generative principle of plasma and device and equipment, and interferences, and inductively coupled plasma mass spectrometry like device, pros and cons of ICP/MS, sample analysis, reagent, water, acid, flux, materials of experiments, sample and sampling and disassembling of sample and pollution and loss in open system and closed system.

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

    Science.gov (United States)

    Boulyga, Sergei F.; Heumann, Klaus G.

    2005-04-01

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

  9. Redox speciation of final repository relevant elements using separation methods in combination with ICP mass spectrometry

    International Nuclear Information System (INIS)

    Graser, Carl-Heinrich

    2015-01-01

    The long-term safety assessment for nuclear waste repositories requires a detailed understanding of the chemistry of actinide elements in the geosphere. The development of advanced analytical tools is required to gain detailed insights into actinide redox speciation in a given system. The mobility of radionuclides is mostly determined by the geochemical conditions which control the redox state of radionuclides. Besides the longlived radionuclides plutonium (Pu) and neptunium (Np), which are key elements in high level nuclear waste, iron (Fe) represents a main component in natural systems controlling redox related geochemical processes. Analytical techniques for determining oxidation state distribution for redox sensitive radionuclides and other metal ions often have a lack of sensitivity. The detection limits of these methods (i.e. UV/vis, TRLFS, XANES) are in general in the range of ≥ 10 -6 mol.L -1 . As a consequence ultrasensitive new analytical techniques are required. Capillary electrophoresis (CE) and ion chromatography (IC) are powerful separation methods for metal ions. In the course of this thesis different speciation method for iron, neptunium and plutonium were optimized. With the optimized setup redox speciation analysis of these elements in different samples were done. Furthermore CE hyphenated to inductively coupled plasma sector field mass spectrometry (CE - ICP - SF - MS) was used to measure the redox speciation of Pu (III, IV, V, VI), Np (IV, V, VI) and Fe (II, III) at concentrations lower than 10 -7 mol.L -1 . CE coupling and separation parameters such as sample gas pressure, make up flow rate, capillary position, auxiliary gas flow, as well as the electrolyte system were optimized to obtain the maximum sensitivity. The methodes detection limits are 10 -12 mol.L -1 for Np and Pu. The various oxidation state species of Pu and Np in different samples were separated by application of an acetate based electrolyte system. The separation of Fe (II

  10. Determination of ruthenium in photographic emulsions - Development and comparison of different sample treatments and mass spectrometric methods

    NARCIS (Netherlands)

    Krystek, Petra; Heumann, Klaus G.

    1999-01-01

    Different sample treatment procedures were combined with inductively coupled plasma mass spectrometry (ICP-MS) and negative thermal ionisation mass spectrometry (NTI-MS) for the determination of ruthenium traces in photographic emulsions. Dissolution of the samples in concentrated ammonia solution

  11. 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)

  12. Elemental bioimaging of nanosilver-coated prostheses using X-ray fluorescence spectroscopy and laser ablation-inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Blaske, Franziska; Reifschneider, Olga; Gosheger, Georg; Wehe, Christoph A; Sperling, Michael; Karst, Uwe; Hauschild, Gregor; Höll, Steffen

    2014-01-07

    The distribution of different chemical elements from a nanosilver-coated bone implant was visualized, combining the benefits of two complementary methods for elemental bioimaging, the nondestructive micro X-ray fluorescence (μ-XRF), and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). Challenges caused by the physically inhomogeneous materials including bone and soft tissues were addressed by polymer embedding. With the use of μ-XRF, fast sample mapping was achieved obtaining titanium and vanadium signals from the metal implant as well as phosphorus and calcium signals representing hard bone tissue and sulfur distribution representing soft tissues. Only by the use of LA-ICP-MS, the required high sensitivity and low detection limits for the determination of silver were obtained. Metal distribution within the part of cancellous bone was revealed for silver as well as for the implant constituents titanium, vanadium, and aluminum. Furthermore, the detection of coinciding high local zirconium and aluminum signals at the implant surface indicates remaining blasting abrasive from preoperative surface treatment of the nanosilver-coated device.

  13. 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

  14. Aerosol Vacuum-Assisted Plasma Ionization (Aero-VaPI) Coupled to Ion Mobility-Mass Spectrometry

    Science.gov (United States)

    Blair, Sandra L.; Ng, Nga L.; Zambrzycki, Stephen C.; Li, Anyin; Fernández, Facundo M.

    2018-02-01

    In this communication, we report on the real-time analysis of organic aerosol particles by Vacuum-assisted Plasma Ionization-Mass Spectrometry (Aero-VaPI-MS) using a home-built VaPI ion source coupled to a Synapt G2-S HDMS ion mobility-mass spectrometry (IM-MS) system. Standards of organic molecules of interest in prebiotic chemistry were used to generate aerosols. Monocaprin and decanoic acid aerosol particles were successfully detected in both the positive and negative ion modes, respectively. A complex aerosol mixture of different sizes of polymers of L-malic acid was also examined through ion mobility (IM) separations, resulting in the detection of polymers of up to eight monomeric units. This noncommercial plasma ion source is proposed as a low cost alternative to other plasma ionization platforms used for aerosol analysis, and a higher-performance alternative to more traditional aerosol mass spectrometers. VaPI provides robust online ionization of organics in aerosols without extensive ion activation, with the coupling to IM-MS providing higher peak capacity and excellent mass accuracy. [Figure not available: see fulltext.

  15. Determination of metals content from wines by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Iordache, Andreea-Maria; Geana, Elisabeta-Irina

    2009-01-01

    Full text: Wine is a widely consumed beverage with thousands of years of tradition. Wine composition strongly determines its quality besides having a great relevance on wine characterization, tipyfication and frauds detection. Wine composition is influenced by many and diverse factors corresponding to the specific production area, such as grape variety, soil and climate, culture, yeast, winemaking practices, transport and storage. Daily consumption of wine in moderate quantities contributes significantly to the requirements of the human organism for essential elements such as Cr, Cu, Zn, Fe, Mn, Co, Ni and Sr. On the other hand, several metals, such as Pb and Cd , are known to be potentially toxic. The objective of this work was to develop a method to determine the metals content in wine samples from Romania. Three samples of difference white wines available in the supermarket was analyzed for identify the presence of: Cr, Cu, Zn, Fe, Mn, Pb, Cd, Co, Ni and Sr by inductively coupled plasma mass spectrometry (ICP-MS). (authors)

  16. Cu determination in crude oil distillation products by atomic absorption and inductively coupled plasma mass spectrometry after analyte transfer to aqueous solution

    International Nuclear Information System (INIS)

    Kowalewska, Zofia; Ruszczynska, Anna; Bulska, Ewa

    2005-01-01

    Cu was determined in a wide range of petroleum products from crude oil distillation using flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). Different procedures of sample preparation were evaluated: (i) mineralization with sulfuric acid in an open system (ii) mineralization in a closed microwave system (iii) combustion in hydrogen-oxygen flame in the Wickbold's apparatus (iv) matrix evaporation followed by acid dissolution, and (v) acidic extraction. All the above procedures led to the transfer of the analyte into an aqueous solution for the analytical measurement step. It was found that application of FAAS was limited to the analysis of the heaviest petroleum products of high Cu content. In ICP-MS, the use of internal reference method (with Rh or In as internal reference element) was required to eliminate the matrix effects in the analysis of extracts and the concentrated solutions of mineralized heavy petroleum products. The detection limits (in original samples) were equal to, respectively, 10, 86, 3.3, 0.9 and 0.4 ng g -1 in procedures i-v with ETAAS detection and 10, 78, 1.1 and 0.5 ng g -1 in procedures i-iii and v with ICP-MS detection. The procedures recommended here were validated by recovery experiments, certified reference materials analysis and comparison of results, obtained for a given sample, in different ways. The Cu content in the analyzed samples was: 50-110 ng g -1 in crude oil, -1 in gasoline, -1 in atmospheric oil, -1 in heavy vacuum oil and 140-300 ng g -1 in distillation residue

  17. Filterless preconcentration, flow injection analysis and detection by inductively-coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Andersen, Jens Enevold Thaulov

    The influence of interferences in the analysis of elements by inductively-coupled-plasma mass-spectrometry (ICP-MS) may be significantly diminished by utilising a protocol of flow-injection analysis (FIA). The method is based on filterless preconcentration of metallic elements at the walls...... of a knotted reactor that was made of nylon tubings. In the load mode, the preconcentration was accomplished by precipitation of metallic species in alkaline-buffered carriers onto the inner walls of the hydrofilic tube. After a preconcen-tration period of 40-120 seconds using sample volumes of 4-10 m...... of 10-30 were obtained in the analysis of aluminium, of chromium and of iron, which resulted in detection limits (3) down to 20 g/L at a sampling frequency of 50 per hour. The preconcentration protocol improves the selectivity thus allowing direct determination of the elements in saline media. Anionic...

  18. 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

  19. 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)

  20. Chemical characterization of airborne particulate matter in ambient air of Nagoya, Japan, as studied by the multielement determination with ICP-AES and ICP-MS

    International Nuclear Information System (INIS)

    Fukai, Taku; Kobayashi, Tatsuya; Sakaguchi, Masahiro; Aoki, Masanori; Saito, Tsuyoshi; Fujimori, Eiji; Haraguchi, Hiroki

    2007-01-01

    The multielement determination of PM 10 (airborne particulate matter smaller than 10 μm) samples, which was collected by a high volume air sampler at the urban site of Nagoya City, was carried out by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The present analytical method was validated by analyzing urban particulate matter standard reference material of NIST SRM 1648. The analytical data for ca. 30 elements in PM 10 samples collected during a period from 8 September to 9 October, 2003, were obtained in the concentration range from sub-μg g -1 to several-10 mg g -1 , but the data for 18 elements among ca. 30 elements were available for the characterization of PM 10 samples in ambient air, because of problems caused by the filter blanks. Then, the trends concerning the distributions of diverse elements in PM 10 samples were analyzed based on the enrichment factors and size distribution factors. The lithophile and siderophile elements were distributed more than 50% in coarse particle fraction (>2.1 μm), which was derived mainly from natural sources, such as soils and crustal minerals. On the other hand, chalcophile elements were distributed more than 50% in fine particle fraction ( 10 samples as well as their mining influence factors (MIFs) suggested their wide use in industrial productions. (author)

  1. 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.

  2. 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.

  3. 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.

  4. The determination of precious metals in geological samples by ICP - Mass Spectrometry

    International Nuclear Information System (INIS)

    Denoyer, E.; Ediger, R.; Hager, J.

    1989-01-01

    ICP - mass spectrometry with laser sampling has been used to determine gold directly in solid fire assay beads. A small portion of the lead bead is vaporized by Nd: YAG laser, and the resulting particulate material is passed by a flow of argon an ICP-mass spectrometer for quantitation of the gold content. Calibration with known geological materials gives linear calibration curves, and detection limits for gols are estimated to be 0.07 micrograms/gram in the original ore sample. The repeatability of the method is similar to that expected for traditional fire assay methods, and the analysis time for the solid lead bead is less than five minutes per sample. (author) [pt

  5. An investigation by LA-ICP-MS of possum tooth enamel as a model for identifying childhood geographical locations of historical and archaeological human remains from New Zealand

    International Nuclear Information System (INIS)

    Cameron, N.E.; Balks, M.; Littler, R.; Manley-Harris, M.; Te Awekotuku, N.

    2012-01-01

    LA-ICP-MS (laser ablation-inductively coupled plasma-mass spectrometry) has been used to analyse enamel from the teeth of brushtail possum (Trichosurus vulpecula) in order to model a method for identifying the childhood geographical origin of human remains within New Zealand. The model application of the method is promising for establishing locations of historical and archaeological human remains, including preserved heads, upoko tuhi. (author). 30 refs., 5 figs., 6 tabs.

  6. 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

  7. 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

  8. 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.

  9. The chemical speciation and analysis of trace elements in sediment with Neutron Activation Analytical method(NAA) and atomic mass spectrometry

    International Nuclear Information System (INIS)

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

    2003-01-01

    In this research, first of all, the analytical methods for the determination of major elements in sediment have been developed with ICP-MS (Inductively Coupled Plasma Mass Spectrometry). The analytical results of major elements (Al, Ca, K, Fe, Mg) with Cool ICP-MS were much better than those with normal ICP-MS. The analytical results were compared with those of NAA (Neutron Activation Analysis). NAA were a little superior to ICP-MS for the determination of major elements in sediment as a non-destructive trace analytical trace analytical method. The analytical methods for the determination of minor elements (Cr, Ce, U, Co, Pb, As, Se) have been also developed with ICP-MS. The analytical results by standard calibration curve with ICP-MS were not accurate due to the matrix interferences. Thus, the internal standard method was applied, then the analytical results for minor elements 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. Accordingly, the NAA will plan an important role in analysis of environment sample with complex matrix. ICP-MS also will play an important role because it has a great capability for the determination of Pb that could not be determined by NAA

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

    International Nuclear Information System (INIS)

    Yadav, Ravi; Salunke-Gawali, Sunita

    2013-01-01

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

  11. Determination of uranium isotopic composition and {sup 236}U content of soil samples and hot particles using inductively coupled plasma mass spectrometry

    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

    As a result of the accident at the Chernobyl nuclear power plant (NPP) the environment was contaminated with spent nuclear fuel. The {sup 236}U isotope was used in this study to monitor the spent uranium from nuclear fallout in soil samples collected in the vicinity of the Chernobyl NPP. Nuclear track radiography was applied for the identification and extraction of hot radioactive particles from soil samples. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on double-focusing inductively coupled plasma mass spectrometry (DF-ICP-MS) with a MicroMist nebulizer and a direct injection high-efficiency nebulizer (DIHEN). The performance of the DF-ICP-MS with a quartz DIHEN and plasma shielded torch was studied. Overall detection efficiencies of 4 x 10{sup -4} and 10{sup -3} counts per atom were achieved for {sup 238}U in DF-ICP-QMS with the MicroMist nebulizer and DIHEN, respectively. The rate of formation of uranium hydride ions UH{sup +}/U{sup +} was 1.2 x 10{sup -4} and 1.4 x 10{sup -4}, respectively. The precision of short-term measurements of uranium isotopic ratios (n = 5) in 1 {mu}g L{sup -1} NBS U-020 standard solution was 0.11% ({sup 238}U/{sup 235}U) and 1.4% ({sup 236}U/{sup 238}U) using a MicroMist nebulizer and 0.25% ({sup 235}U/{sup 238}U) and 1.9% ({sup 236}U/{sup 238}U) using a DIHEN. The isotopic composition of all investigated Chernobyl soil samples differed from those of natural uranium; i.e. in these samples the {sup 236}U/{sup 238}U ratio ranged from 10{sup -5} to 10{sup -3}. Results obtained with ICP-MS, {alpha}- and {gamma}-spectrometry showed differences in the migration properties of spent uranium, plutonium, and americium. The isotopic ratio of uranium was also measured in hot particles extracted from soil samples. (orig.)

  12. Upconversion nanoparticle as elemental tag for the determination of alpha-fetoprotein in human serum by inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Liu, Zhengru; Yang, Bin; Chen, Beibei; He, Man; Hu, Bin

    2016-12-19

    Upconversion nanoparticles (UCNPs) have received increasing attention due to their unique optical properties. Recognizing that UCNPs are lanthanide-doped nanoparticles, we incorporated UCNPs into an immunoassay with inductively coupled plasma mass spectrometry (ICP-MS) detection for the determination of specific proteins, e.g., alpha-fetoprotein (AFP). The sensitivity of the assay was enhanced because of the ICP-MS detection of UCNPs that contained large numbers of lanthanide elemental tags. Conjugates of UCNPs and antibodies were prepared and the morphology of the conjugates was characterized by transmission electron microscopy. After a sandwich immunoreaction, the AFP was determined by the ICP-MS analysis of UCNPs. Under the optimized conditions, a limit of detection (3σ) of 0.31 ng mL -1 based on 89 Y signal and 0.22 ng mL -1 based on 174 Yb signal was obtained for AFP, with a dynamic range of 0.5-35 ng mL -1 and a relative standard deviation of 4.8% (c = 5 ng mL -1 , n = 9). The developed method was applied to the determination of AFP in human serum and the recovery for the spiked sample was in the range of 98.6-123%. The proposed method is simple, rapid, selective and sensitive, and has a good tolerance for the complex biological matrix, indicating great potential for the application of UCNP in biological research as an elemental tag.

  13. Cerium oxide-deposited mesoporous silica nanoparticles for the determination of carcinoembryonic antigen in serum using inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Choi, H.W.; Lee, K.H.; Hur, N.H.; Lim, H.B.

    2014-01-01

    Highlights: • Sandwich-type immunoassay using ICP-MS and nanoparticles to determine biomarkers. • CeO 2 -deposited mesoporous silica nanoparticles were synthesized as a probe. • Ratiometric measurement significantly improved the calibration linearity. • Excellent detection limit was achieved by signal amplification. - Abstract: CeO 2 -deposited mesoporous silica nanoparticles were synthesized as a probe to determine carcinoembryonic antigen (CEA) in serum by inductively coupled plasma-mass spectrometry (ICP-MS). The prepared mesoporous nanoparticles were modified and tagged to the target for sandwich-type immunoassay. Fe 3 O 4 magnetic nanoparticles (MNPs) were also synthesized and immobilized with antibody to extract the target biomarker. The calibration curve of the synthesized CeO 2 -deposited silica nanoparticles, which was plotted by the signal ratio of 140 Ce/ 57 Fe measured by ICP-MS vs. the concentration of CEA, showed excellent linearity and sensitivity owing to the signal amplification and low spectral interference. Under optimal conditions, the sandwich-type analytical method was applied to determine CEA in serum spiked in the range of 0.001–5 ng mL −1 and showed a limit of detection of 0.36 ng mL −1 . Since the deposited CeO 2 in the mesoporous silica layer can be substituted by other metal compounds, various kinds of metal-deposited nanoparticles can be prepared as probe materials for multiplex detection in bioanalysis

  14. Identification of phosphorylated butyrylcholinesterase in human plasma using immunoaffinity purification and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Aryal, Uma K.; Lin, Chiann Tso; Kim, Jong Seo; Heibeck, Tyler H.; Wang, Jun; Qian, Weijun; Lin, Yuehe

    2012-04-20

    Paraoxon (diethyl 4-nitrophenyl phosphate) is an active metabolite of the common insecticide parathion and is acutely toxic due to the inhibition of cholinesterase (ChE) activity in the nervous systems. The Inhibition of butyrylcholinesterase (BChE) activity by paraoxon is due to the formation of phosphorylated BChE adduct, and the detection of the phosphorylated BChE adduct in human plasma can serve as an exposure biomarker of organophosphate pesticides and nerve agents. In this study, we performed immunoaffinity purification and liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis for identifying phosphorylated BChE in human plasma treated by paraoxon. BChE was captured by biotinylated anti-BChE polyclonal antibodies conjugated to streptavidin magnetic beads. Western blot analysis showed that the antibody was effective to recognize both native and modified BChE with high specificity. The exact phosphorylation site of BChE was confirmed on Serine 198 by MS/MS with a 108 Da modification mass and accurately measured parent ion masses. The phosphorylated BChE peptide was also successfully detected in the immunoaffinity purified sample from paraoxon treated human plasma. Thus, immunoaffinity purification combined with mass spectrometry represents a viable approach for the detection of paraoxon-modified BChE and other forms of modified BChE as exposure biomarkers of organophosphates and nerve agents.

  15. Simultaneous determination of amoxicillin and clavulanic acid in the human plasma by high performance liquid chromatography: Mass spectrometry (UPLC/MS

    Directory of Open Access Journals (Sweden)

    Ćirić Biljana

    2010-01-01

    Full Text Available Background/Aim. Quantitative analysis of amoxicillin and clavulanic acid in biological matrices requires sensitive and specific methods which allow determination of therapeutic concentration in μg/mL range. Analytical methods for determination of their concentrations in body fluids described in literature include high performance liquid chromatography coupled to UV detector (HPLC-UV and liquid chromatography-mass spectrometry (LC-MS. The aim of this study was to develop sensitive and specific ultra performance liquid chromatography/ mass spectrometry (UPLC/MS method which could be used for the spectral identification and quantification of the low concentrations of amoxicillin and clavulanic acid in the human plasma. Method. A sensitive and specific UPLC/MS method for amoxicillin and clavulanic acid determination was developed in this study. The samples were taken from the adult healthy volunteers receiving per os one tablet of amoxicillin (875 mg in combination with clavulanic acid (125 mg. Results. Plasma samples were pretreated by direct deproteinization with perchloric acid. Quantification limit of 0.01 μg/ml for both amoxicillin and clavulanic acid was achieved. The method was reproducible day by day (RSD < 7 %. Analytical recoveries for amoxicillin ranged from 98.82% to 100.9% (for concentrations of 1, 5 and 20 μg/mL, and recoveries for clavulanic acid were 99,89% to 100.1% (for concentrations of 1, 2 and 5 μg/mL. This assay was successfully applied to a pilot pharmacokinetic study in healthy volunteers after a single-oral administration of amoxicillin/ clavulanic combination. The determined plasma concentrations of both amoxicillin and clavulanic acid were in the range of the expected values upon the literature data for HPLC-UV and LC-MS methods. Conclusion. The described method provided a few advantages comparing with LC/MS-MS method. The method is faster using running time of 5 minute, has lower limit of quantification (LOQ and it

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

    Science.gov (United States)

    Solomon, Paige; Nelson, Jenny

    2018-03-01

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

  17. [Determination of Heavy Metal Elements in Diatomite Filter Aid by Inductively Coupled Plasma Mass Spectrometry].

    Science.gov (United States)

    Nie, Xi-du; Fu, Liang

    2015-11-01

    This study established a method for determining Be, Cr, Ni, As, Cd, Sb, Sn, Tl, Hg and Pb, total 10 heavy metals in diatomite filter aid. The diatomite filter aid was digested by using the mixture acid of HNO₃ + HF+ H₃PO₄ in microwave system, 10 heavy metals elements were determined by inductively coupled plasma mass spectrometry (ICP-MS). The interferences of mass spectrometry caused by the high silicon substrate were optimized, first the equipment parameters and isotopes of test metals were selected to eliminate these interferences, the methane was selected as reactant gas, and the mass spectral interferences were eliminated by dynamic reaction cell (DRC). Li, Sc, Y, In and Bi were selected as the internal standard elements to correct the interferences caused by matrix and the drift of sensitivity. The results show that the detection limits for analyte is in the range of 3.29-15.68 ng · L⁻¹, relative standard deviations (RSD) is less than 4.62%, and the recovery is in the range of 90.71%-107.22%. The current method has some advantages such as, high sensitivity, accurate, and precision, which can be used in diatomite filter aid quality control and safety estimations.

  18. The impact of whole human blood on the kinetic inertness of platinum(iv) prodrugs - an HPLC-ICP-MS study.

    Science.gov (United States)

    Theiner, Sarah; Grabarics, Márkó; Galvez, Luis; Varbanov, Hristo P; Sommerfeld, Nadine S; Galanski, Markus; Keppler, Bernhard K; Koellensperger, Gunda

    2018-04-17

    The potential advantage of platinum(iv) complexes as alternatives to classical platinum(ii)-based drugs relies on their kinetic stability in the body before reaching the tumor site and on their activation by reduction inside cancer cells. In this study, an analytical workflow has been developed to investigate the reductive biotransformation and kinetic inertness of platinum(iv) prodrugs comprising different ligand coordination spheres (respectively, lipophilicity and redox behavior) in whole human blood. The distribution of platinum(iv) complexes in blood pellets and plasma was determined by inductively coupled plasma-mass spectrometry (ICP-MS) after microwave digestion. An analytical approach based on reversed-phase (RP)-ICP-MS was used to monitor the parent compound and the formation of metabolites using two different extraction procedures. The ligand coordination sphere of the platinum(iv) complexes had a significant impact on their accumulation in red blood cells and on their degree of kinetic inertness in whole human blood. The most lipophilic platinum(iv) compound featuring equatorial chlorido ligands showed a pronounced penetration into blood cells and a rapid reductive biotransformation. In contrast, the more hydrophilic platinum(iv) complexes with a carboplatin- and oxaliplatin-core exerted kinetic inertness on a pharmacologically relevant time scale with notable amounts of the compound accumulated in the plasma fraction.

  19. Laser ablation microprobe inductively coupled plasma mass spectrometry study on diffusion of uranium into cement materials

    International Nuclear Information System (INIS)

    Sugiyama, D.; Chida, T.; Cowper, M.

    2008-01-01

    The diffusion of uranium (U(VI)) in solid cement monoliths of ordinary portland cement (OPC) and low-heat portland cement containing 30 wt.% fly ash (FAC) was measured by an in-diffusion technique. Detailed sharp depth profiles of uranium in the solid cement matrices were successively and quantitatively measured using laser ablation microprobe inductively coupled plasma mass spectrometry (LAMP-ICP-MS), and the apparent (D a ) and effective (D e ) diffusion coefficient of uranium in cement matrix were calculated as: D a =∝ 4 x 10 -16 m 2 s -1 and D e =∝ 3 x 10 -11 m 2 s -1 for OPC, and D a =∝ 2 x 10 -17 m 2 s -1 and D e =∝ 6 x 10 -13 m 2 s -1 for FAC. (orig.)

  20. Mass Spectrometric Investigation of Silicon Extremely Enriched in (28)Si: From (28)SiF4 (Gas Phase IRMS) to (28)Si Crystals (MC-ICP-MS).

    Science.gov (United States)

    Pramann, Axel; Rienitz, Olaf

    2016-06-07

    A new generation of silicon crystals even further enriched in (28)Si (x((28)Si) > 0.999 98 mol/mol), recently produced by companies and institutes in Russia within the framework of a project initiated by PTB, were investigated with respect to their isotopic composition and molar mass M(Si). A modified isotope dilution mass spectrometric (IDMS) method treating the silicon as the matrix containing a so-called virtual element (VE) existing of the isotopes (29)Si and (30)Si solely and high resolution multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) were applied in combination. This method succeeds also when examining the new materials holding merely trace amounts of (29)Si (x((29)Si) ≈ 5 × 10(-6) mol/mol) and (30)Si (x((30)Si) ≈ 7 × 10(-7) mol/mol) extremely difficult to detect with lowest uncertainty. However, there is a need for validating the enrichment in (28)Si already in the precursor material of the final crystals, silicon tetrafluoride (SiF4) gas prior to crystal production. For that purpose, the isotopic composition of selected SiF4 samples was determined using a multicollector magnetic sector field gas-phase isotope ratio mass spectrometer. Contaminations of SiF4 by natural silicon due to storing and during the isotope ratio mass spectrometry (IRMS) measurements were observed and quantified. The respective MC-ICP-MS measurements of the corresponding crystal samples show-in contrast-several advantages compared to gas phase IRMS. M(Si) of the new crystals were determined to some extent with uncertainties urel(M) < 1 × 10(-9). This study presents a clear dependence of the uncertainty urel(M(Si)) on the degree of enrichment in (28)Si. This leads to a reduction of urel(M(Si)) during the past decade by almost 3 orders of magnitude and thus further reduces the uncertainty of the Avogadro constant NA which is one of the preconditions for the redefinition of the SI unit kilogram.

  1. Accurate determination of sulfur in gasoline and related fuel samples using isotope dilution ICP-MS with direct sample injection and microwave-assisted digestion.

    Science.gov (United States)

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

    2004-09-01

    Inductively coupled plasma isotope-dilution mass spectrometry (ICP-IDMS) with direct injection of isotope-diluted samples into the plasma, using a direct injection high-efficiency nebulizer (DIHEN), was applied for accurate sulfur determinations in sulfur-free premium gasoline, gas oil, diesel fuel, and heating oil. For direct injection a micro-emulsion consisting of the corresponding organic sample and an aqueous 34S-enriched spike solution with additions of tetrahydronaphthalene and Triton X-100, was prepared. The ICP-MS parameters were optimized with respect to high sulfur ion intensities, low mass-bias values, and high precision of 32S/34S ratio measurements. For validation of the DIHEN-ICP-IDMS method two certified gas oil reference materials (BCR 107 and BCR 672) were analyzed. For comparison a wet-chemical ICP-IDMS method was applied with microwave-assisted digestion using decomposition of samples in a closed quartz vessel inserted into a normal microwave system. The results from both ICP-IDMS methods agree well with the certified values of the reference materials and also with each other for analyses of other samples. However, the standard deviation of DIHEN-ICP-IDMS was about a factor of two higher (5-6% RSD at concentration levels above 100 mircog g(-1)) compared with those of wet-chemical ICP-IDMS, mainly due to inhomogeneities of the micro-emulsion, which causes additional plasma instabilities. Detection limits of 4 and 18 microg g(-1) were obtained for ICP-IDMS in connection with microwave-assisted digestion and DIHEN-ICP-IDMS, respectively, with a sulfur background of the used Milli-Q water as the main limiting factor for both methods.

  2. Accurate determination of sulfur in gasoline and related fuel samples using isotope dilution ICP-MS with direct sample injection and microwave-assisted digestion

    Energy Technology Data Exchange (ETDEWEB)

    Heilmann, Jens; Boulyga, Sergei F.; Heumann, Klaus G. [Johannes Gutenberg-University, Institute of Inorganic Chemistry and Analytical Chemistry, Mainz (Germany)

    2004-09-01

    Inductively coupled plasma isotope-dilution mass spectrometry (ICP-IDMS) with direct injection of isotope-diluted samples into the plasma, using a direct injection high-efficiency nebulizer (DIHEN), was applied for accurate sulfur determinations in sulfur-free premium gasoline, gas oil, diesel fuel, and heating oil. For direct injection a micro-emulsion consisting of the corresponding organic sample and an aqueous {sup 34}S-enriched spike solution with additions of tetrahydronaphthalene and Triton X-100, was prepared. The ICP-MS parameters were optimized with respect to high sulfur ion intensities, low mass-bias values, and high precision of {sup 32}S/{sup 34}S ratio measurements. For validation of the DIHEN-ICP-IDMS method two certified gas oil reference materials (BCR 107 and BCR 672) were analyzed. For comparison a wet-chemical ICP-IDMS method was applied with microwave-assisted digestion using decomposition of samples in a closed quartz vessel inserted into a normal microwave system. The results from both ICP-IDMS methods agree well with the certified values of the reference materials and also with each other for analyses of other samples. However, the standard deviation of DIHEN-ICP-IDMS was about a factor of two higher (5-6% RSD at concentration levels above 100 {mu}g g{sup -1}) compared with those of wet-chemical ICP-IDMS, mainly due to inhomogeneities of the micro-emulsion, which causes additional plasma instabilities. Detection limits of 4 and 18 {mu}g g{sup -1} were obtained for ICP-IDMS in connection with microwave-assisted digestion and DIHEN-ICP-IDMS, respectively, with a sulfur background of the used Milli-Q water as the main limiting factor for both methods. (orig.)

  3. 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.

  4. Investigation of mercury-containing proteins by enriched stable isotopic tracer and size-exclusion chromatography hyphenated to inductively coupled plasma-isotope dilution mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shi Junwen [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]|[Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Feng Weiyue [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]. E-mail: fengwy@mail.ihep.ac.cn; Wang Meng [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]|[Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Zhang Fang [Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Li Bai [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Wang Bing; Zhu Motao [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]|[Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Chai Zhifang [Laboratory for Bio-Environmental Health Sciences of Nanoscale Materials and Key Laboratory of Nuclear Analytical Techniques, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China)]|[Institute of Nuclear Technology, Shenzhen University, Shenzhen 518060 (China)]|[Institute of Nanochemistry and Nanosafety, Shanghai University, Shanghai (China)

    2007-01-30

    In order to investigate trace mercury-containing proteins in maternal rat and their offspring, a method of enriched stable isotopic tracer ({sup 196}Hg and {sup 198}Hg) combined with size-exclusion chromatography (SEC) coupled to inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS) was developed. Prior to the analysis, {sup 196}Hg- and {sup 198}Hg-enriched methylmercury was administrated to the pregnant rats. Then the mercury-containing proteins in serum and brain cytosol of the dam and pup rats were separated by size-exclusion columns and the mercury was detected by ICP-MS. The ICP-MS spectrogram of the tracing samples showed significantly elevated {sup 196}Hg and {sup 198}Hg isotopic signals compared with the natural ones, indicating that the detection sensitivity could be increased by the tracer method. The contents of mercury in chromatographic fractions of the dam and pup rat brain cytosol were quantitatively estimated by post-column reverse ID-ICP-MS. The quantitative speciation differences of mercury in brain cytosol between the dam and pup rats were observed, indicating that such studies could be useful for toxicological estimation. Additionally, the isotopic ratio measurement of {sup 198}Hg/{sup 202}Hg in the tracing samples could be used to identify the artifact mercury species caused in the analytical procedure. The study demonstrates that the tracer method combined with high-performance liquid chromatography (HPLC)-ICP-IDMS could provide reliably qualitative and quantitative information on mercury-containing proteins in organisms.

  5. Investigation of mercury-containing proteins by enriched stable isotopic tracer and size-exclusion chromatography hyphenated to inductively coupled plasma-isotope dilution mass spectrometry

    International Nuclear Information System (INIS)

    Shi Junwen; Feng Weiyue; Wang Meng; Zhang Fang; Li Bai; Wang Bing; Zhu Motao; Chai Zhifang

    2007-01-01

    In order to investigate trace mercury-containing proteins in maternal rat and their offspring, a method of enriched stable isotopic tracer ( 196 Hg and 198 Hg) combined with size-exclusion chromatography (SEC) coupled to inductively coupled plasma-isotope dilution mass spectrometry (ICP-IDMS) was developed. Prior to the analysis, 196 Hg- and 198 Hg-enriched methylmercury was administrated to the pregnant rats. Then the mercury-containing proteins in serum and brain cytosol of the dam and pup rats were separated by size-exclusion columns and the mercury was detected by ICP-MS. The ICP-MS spectrogram of the tracing samples showed significantly elevated 196 Hg and 198 Hg isotopic signals compared with the natural ones, indicating that the detection sensitivity could be increased by the tracer method. The contents of mercury in chromatographic fractions of the dam and pup rat brain cytosol were quantitatively estimated by post-column reverse ID-ICP-MS. The quantitative speciation differences of mercury in brain cytosol between the dam and pup rats were observed, indicating that such studies could be useful for toxicological estimation. Additionally, the isotopic ratio measurement of 198 Hg/ 202 Hg in the tracing samples could be used to identify the artifact mercury species caused in the analytical procedure. The study demonstrates that the tracer method combined with high-performance liquid chromatography (HPLC)-ICP-IDMS could provide reliably qualitative and quantitative information on mercury-containing proteins in organisms

  6. A micro-fluidic sub-microliter sample introduction system for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry using external aqueous calibration

    Science.gov (United States)

    Cheng, Heyong; Liu, Jinhua; Xu, Zigang; Yin, Xuefeng

    2012-07-01

    A microfluidic sub-microliter sample introducing system was developed for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry (ICP-MS). It consisted of a microfluidic chip integrating variable-volume sampling channels (0.1-0.8 μL), an eight-way multi-functional valve used in flow injection analysis (FIA), a syringe pump and a peristaltic pump of the Ar ICP-MS instrument. Three solutions, i.e., 15, 40 and 100 g L- 1 glucose in 20% ethanol were used to simulate Chinese rice wine of the dry type, the semidry type and the semisweet type, each. The effects of their volume introduced into ICP-MS on the plasma stability and ICP-MS intensities were studied. The experimental results showed that neither alteration of plasma stability nor carbon deposition was observed when the sampling volume of 20% ethanol containing 100 g L- 1 glucose was downscaled to 0.8 μL. Further reducing the sampling volume to 0.4 μL, no significant difference between the intensities of multi-element standard prepared in three simulated Chinese rice wine matrices and those in aqueous solution was observed. It indicated no negative effect of Chinese rice wine matrix on the ICP-MS intensities. A sampling volume of 0.4 μL was considered to be a good compromise between sensitivity and matrix effect. The flow rate of the carrier was chosen as 20 μL min- 1 for obtaining peaks with the highest peak height within the shortest time. Based on these observations, a microflow injection (μFI) method for the direct determination of cadmium and lead in Chinese rice wine by ICP-MS using an external aqueous calibration was developed. The sample throughput was 45 h- 1 with the detection limit of 19.8 and 10.4 ng L- 1 for Cd and Pb, respectively. The contents of Cd and Pb in 10 Chinese rice wine samples were measured. The results agreed well with those determined by ICP-MS with the conventional sampling system after microwave assisted digestion. The recoveries of three Chinese

  7. A fast and feasible method for Br and I determination in whole egg powder and its fractions by ICP-MS.

    Science.gov (United States)

    Toralles, Isis Gonçalves; Coelho, Gilberto Silva; Costa, Vanize Cadeira; Cruz, Sandra Meinen; Flores, Erico Marlon Moraes; Mesko, Marcia Foster

    2017-04-15

    A method for Br and I determination in whole egg powder and its fractions (egg white and yolk) was developed by combining microwave-induced combustion (MIC) and inductively coupled plasma mass spectrometry (ICP-MS). Using the MIC method, 350mg of whole egg powder and its fractions were efficiently digested using 50mmolL -1 NH 4 OH as an absorbing solution. The limits of detection for Br and I using the MIC method followed by ICP-MS determination were 0.039 and 0.015μgg -1 , respectively. Using the proposed method, agreements with the reference values between 97 and 104% for Br and I were obtained by analysis of reference material NIST 8435. Finally, it was possible to observe that Br concentration (4.59-5.29μgg -1 ) was higher than I (0.150-2.28μgg -1 ) for all the evaluated samples. Copyright © 2016 Elsevier Ltd. All rights reserved.

  8. Investigation of metallodrug-protein interactions by size-exclusion chromatography coupled with inductively coupled plasma mass spectrometry (ICP-MS)

    International Nuclear Information System (INIS)

    Szpunar, J.; Makarov, A.; Pieper, T.; Keppler, B.K.; Lobinski, R.

    1999-01-01

    The coupling of size-exclusion HPLC with ICP-MS was developed for the studies of the kinetics of metallodrug binding to human serum proteins. Two platinum- and three ruthenium-based drugs were investigated. Various SEC columns (of different lengths and with different packings) were compared for the separation of the protein-bound and unbound fractions of a metallodrug prior to on-line detection of the metal (Ru or Pt). The approach developed offers considerable advantages over the methods based on ultrafiltration followed by the off-line metal determination in terms of speed, simplicity, precision and selectivity regarding the molecular weight of the complexes involved. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  9. Simultaneous determination of creatinine and creatine in human serum by double-spike isotope dilution liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-mass spectrometry (GC-MS).

    Science.gov (United States)

    Fernández-Fernández, Mario; Rodríguez-González, Pablo; Añón Álvarez, M Elena; Rodríguez, Felix; Menéndez, Francisco V Álvarez; García Alonso, J Ignacio

    2015-04-07

    This work describes the first multiple spiking isotope dilution procedure for organic compounds using (13)C labeling. A double-spiking isotope dilution method capable of correcting and quantifying the creatine-creatinine interconversion occurring during the analytical determination of both compounds in human serum is presented. The determination of serum creatinine may be affected by the interconversion between creatine and creatinine during sample preparation or by inefficient chemical separation of those compounds by solid phase extraction (SPE). The methodology is based on the use differently labeled (13)C analogues ((13)C1-creatinine and (13)C2-creatine), the measurement of the isotopic distribution of creatine and creatinine by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and the application of multiple linear regression. Five different lyophilized serum-based controls and two certified human serum reference materials (ERM-DA252a and ERM-DA253a) were analyzed to evaluate the accuracy and precision of the proposed double-spike LC-MS/MS method. The methodology was applied to study the creatine-creatinine interconversion during LC-MS/MS and gas chromatography-mass spectrometry (GC-MS) analyses and the separation efficiency of the SPE step required in the traditional gas chromatography-isotope dilution mass spectrometry (GC-IDMS) reference methods employed for the determination of serum creatinine. The analysis of real serum samples by GC-MS showed that creatine-creatinine separation by SPE can be a nonquantitative step that may induce creatinine overestimations up to 28% in samples containing high amounts of creatine. Also, a detectable conversion of creatine into creatinine was observed during sample preparation for LC-MS/MS. The developed double-spike LC-MS/MS improves the current state of the art for the determination of creatinine in human serum by isotope dilution mass spectrometry (IDMS), because corrections are made for all the possible errors

  10. Functional speciation of metal-dissolved organic matter complexes by size exclusion chromatography coupled to inductively coupled plasma mass spectrometry and deconvolution analysis

    International Nuclear Information System (INIS)

    Laborda, Francisco; Ruiz-Begueria, Sergio; Bolea, Eduardo; Castillo, Juan R.

    2009-01-01

    High performance size exclusion chromatography coupled to inductively coupled plasma mass spectrometry (HP-SEC-ICP-MS), in combination with deconvolution analysis, has been used to obtain multielemental qualitative and quantitative information about the distributions of metal complexes with different forms of natural dissolved organic matter (DOM). High performance size exclusion chromatography coupled to inductively coupled plasma mass spectrometry chromatograms only provide continuous distributions of metals with respect to molecular masses, due to the high heterogeneity of dissolved organic matter, which consists of humic substances as well as biomolecules and other organic compounds. A functional speciation approach, based on the determination of the metals associated to different groups of homologous compounds, has been followed. Dissolved organic matter groups of homologous compounds are isolated from the aqueous samples under study and their high performance size exclusion chromatography coupled to inductively coupled plasma mass spectrometry elution profiles fitted to model Gaussian peaks, characterized by their respective retention times and peak widths. High performance size exclusion chromatography coupled to inductively coupled plasma mass spectrometry chromatograms of the samples are deconvoluted with respect to these model Gaussian peaks. This methodology has been applied to the characterization of metal-dissolved organic matter complexes in compost leachates. The most significant groups of homologous compounds involved in the complexation of metals in the compost leachates studied have been hydrophobic acids (humic and fulvic acids) and low molecular mass hydrophilic compounds. The environmental significance of these compounds is related to the higher biodegradability of the low molecular mass hydrophilic compounds and the lower mobility of humic acids. In general, the hydrophilic compounds accounted for the complexation of around 50% of the leached

  11. Improved sample preparation method for environmental plutonium analysis by ICP-SFMS and alpha-spectrometry

    International Nuclear Information System (INIS)

    Varga, Z.; Stefanka, Z.; Suranyi, G.; Vajda, N.

    2007-01-01

    A rapid and simple sample preparation method for plutonium determination in environmental samples by inductively coupled plasma sector field mass spectrometry (ICP-SFMS) and alpha-spectrometry is described. The developed procedure involves a selective CaF 2 co-precipitation for preconcentration followed by extraction chromatographic separation. The proposed method effectively eliminates the possible interferences in mass spectrometric analysis and also removes interfering radionuclides that may disturb alpha-spectrometric measurement. For 239 Pu, 240 Pu and 241 Pu limits of detection of 9.0 fg x g -1 (0.021 mBq), 1.7 fg x g -1 (0.014 mBq) and 3.1 fg x g -1 (11.9 mBq) were achieved by ICP-SFMS, respectively, and 0.02 mBq by alpha-spectrometry. Results of certified reference materials agreed well with the recommended values. (author)

  12. Determination of Arsenic in Sinus Wash and Tap Water by Inductively Coupled Plasma-Mass Spectrometry

    Science.gov (United States)

    Donnell, Anna M.; Nahan, Keaton; Holloway, Dawone; Vonderheide, Anne P.

    2016-01-01

    Arsenic is a toxic element to which humans are primarily exposed through food and water; it occurs as a result of human activities and naturally from the earth's crust. An experiment was developed for a senior level analytical laboratory utilizing an Inductively Coupled Plasma-Mass Spectrometer (ICP-MS) for the analysis of arsenic in household…

  13. Determination of fission products and actinides by inductively coupled plasma-mass spectrometry using isotope dilution analysis. A study of random and systematic errors

    International Nuclear Information System (INIS)

    Ignacio Garcia Alonso, Jose

    1995-01-01

    The theory of the propagation of errors (random and systematic) for isotope dilution analysis (IDA) has been applied to the analysis of fission products and actinide elements by inductively coupled plasma-mass spectrometry (ICP-MS). Systematic errors in ID-ICP-MS arising from mass-discrimination (mass bias), detector non-linearity and isobaric interferences in the measured isotopes have to be corrected for in order to achieve accurate results. The mass bias factor and the detector dead-time can be determined by using natural elements with well-defined isotope abundances. A combined method for the simultaneous determination of both factors is proposed. On the other hand, isobaric interferences for some fission products and actinides cannot be eliminated using mathematical corrections (due to the unknown isotope abundances in the sample) and a chemical separation is necessary. The theory for random error propagation in IDA has been applied to the determination of non-natural elements by ICP-MS taking into account all possible sources of uncertainty with pulse counting detection. For the analysis of fission products, the selection of the right spike isotope composition and spike to sample ratio can be performed by applying conventional random propagation theory. However, it has been observed that, in the experimental determination of the isotope abundances of the fission product elements to be determined, the correction for mass-discrimination and the correction for detector dead-time losses contribute to the total random uncertainty. For the instrument used in the experimental part of this study, it was found that the random uncertainty on the measured isotope ratios followed Poisson statistics for low counting rates whereas, for high counting rates, source instability was the main source of error

  14. Direct atomic spectrometric analysis by slurry atomisation: Pt. 7. Analysis of coal using inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Ebdon, Les; Foulkes, M E; Parry, H G.M.; Tye, C T

    1988-09-01

    The application of slurry atomisation - inductively coupled plasma mass spectrometry (ICP-MS) to major, minor and trace element determination in coals has been investigated. Eight certified reference material (CRM) coals have been ground by the bottle and bead method and analysed using both rapid scan semi-quantitative analysis, employing a single rhodium internal standard, and full quantitative analysis using simple aqueous standards for calibration. The semi-quantitative mode, which determines the concentration using the mass-response curve for 68 elements against the single internal standard, produced values which were within a factor of two of the certified reference value, in most instances. The full quantitative determination gave excellent agreement with the certified reference material coals for a large number of elemental constituents. The results from the determination of 16 elements of interest are discussed including the effects of polyatomic interferents and isotope sensitivity.

  15. Ultra-sensitive speciation analysis of mercury by CE-ICP-MS together with field-amplified sample stacking injection and dispersive solid-phase extraction.

    Science.gov (United States)

    Chen, YiQuan; Cheng, Xian; Mo, Fan; Huang, LiMei; Wu, Zujian; Wu, Yongning; Xu, LiangJun; Fu, FengFu

    2016-04-01

    A simple dispersive solid-phase extraction (DSPE) used to extract and preconcentrate ultra-trace MeHg, EtHg and Hg(2+) from water sample, and a sensitive method for the simultaneous analysis of MeHg, EtHg and Hg(2+) by using capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) with field-amplified sample stacking injection (FASI) were first reported in this study. The DSPE used thiol cotton particles as adsorbent, and is simple and effective. It can be used to extract and preconcentrate ultra-trace mercury compounds in water samples within 30 min with a satisfied recovery and no mercury species alteration during the process. The FASI enhanced the sensitivity of CE-ICP-MS with 25-fold, 29-fold and 27-fold for MeHg, EtHg and Hg(2+) , respectively. Using FASI-CE-ICP-MS together with DSPE, we have successfully determined ultra-trace MeHg, EtHg and Hg(2+) in tap water with a limits of quantification (LOQs) of 0.26-0.45 pg/mL, an RSD (n = 3) mercury. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Application of isotope dilution for the determination of thorium in biological samples by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Igarashi, Yasuhito; Shiraishi, Kunio; Takaku, Yuichi; Masuda, Kimihiko; Seki, Riki; Yamamoto, Masayoshi.

    1992-01-01

    The applicability of isotope dilution-inductively coupled plasma mass spectrometry (ID-ICP-MS) was examined for Th in biological samples. A naturally occurring isotope of Th(Th-230) was used as the spiking isotope. The concentration of Th-230 in the final sample solution was about 50 - 60 pg/ml; an isotope ratio of 232/230 could be measured with a relative standard deviation of less than 2%. The error magnification depended on the amount of Th-232 being concomitant with the Th-230. Though it was shown that one ng of Th-232 could be determined with reasonable precision with a tracer of the present purity, more care should be taken to reduce any source of systematic error. (author)

  17. Speciation of the oxidation states of plutonium in aqueous solutions by UV/Vis spectroscopy, CE-ICP-MS and CE-RIMS

    International Nuclear Information System (INIS)

    Buerger, S.; Banik, N.L.; Buda, R.A.; Kratz, J.V.; Kuczewski, B.; Trautmann, N.

    2007-01-01

    For the speciation of the plutonium oxidation states in aqueous solutions, the online coupling of capillary electrophoresis (CE) with inductively coupled plasma mass spectrometry (ICP-MS) has been developed. Depending on the radius/electrical charge ratio, the oxidation states III, IV, V, and VI of plutonium are separated by CE, based on the different migration times through the capillary and are detected by ICP-MS. The detection limit is 20 ppb, i.e. 10 9 -10 10 atoms (10 -12 -10 -13 g) for one oxidation state with an uncertainty of the reproducibility of the migration times of ≤ 1% and ≤ 5% for the peak area. The redox kinetics of the different plutonium oxidation states in the presence of humic substances (humic and fulvic acid) have been studied. A relatively rapid reduction of Pu(VI) (10 to 1000 h) in contact with Gorleben fulvic or Aldrich humic acid could be observed, depending on the pH of the solution. Furthermore, at pH=1, a reduction to Pu(III) and Pu(IV) in a mixture of all four oxidation states in contact with Gorleben fulvic acid after one month has been observed. In order to improve the sensitivity of the CE method, the offline coupling of CE to resonance ionization mass spectrometry (RIMS) has been explored. First applications of this new speciation method are presented. (orig.)

  18. 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.

  19. Experimental and theoretical investigations about the vaporization of laser-produced aerosols and individual particles inside inductively-coupled plasmas — Implications for the extraction efficiency of ions prior to mass spectrometry

    International Nuclear Information System (INIS)

    Flamigni, Luca; Koch, Joachim; Günther, Detlef

    2012-01-01

    Current quantification capabilities of laser ablation inductively-coupled plasma mass spectrometry (LA-ICP-MS) are known to be restricted by elemental fractionation as a result of LA-, transport-, and ICP-induced effects which, particularly, may provoke inaccuracies whenever calibration strategies on the basis of non-matrix matched standard materials are applied. The present study is dealing with the role of ICP in this complex scenario. Therefore, the vaporization process of laser-produced aerosols and subsequent diffusion losses occurring inside ICP sources were investigated using 2-D optical emission spectrometry (OES) and ICP-quadrupole (Q)MS of individual particles. For instance, Na- and Ca-specific OES of aerosols produced by LA of silicate glasses or metals revealed axial shifts in the onset and maximum position of atomic emission which were in the range of a few millimeters. The occurrence of these shifts was found to arise from composition-dependent particle/aerosol penetration depths, i.e. the displacement of axial vaporization starting points controlling the ion extraction efficiency through the ICP-MS vacuum interface due to a delayed, diffusion-driven expansion of oxidic vs. metallic aerosols. Furthermore, ICP-QMS of individual particles resulted in 1/e half-value signal durations of approximately 100 μs, which complies with modeled values if OES maxima are assumed to coincide with positions of instantaneous vaporization and starting points for atomic diffusion. To prove phenomena observed for their consistency, in addition, “ab initio” as well as semi-empirical simulations of particle/aerosol penetration depths followed by diffusion-driven expansion was accomplished indicating differences of up to 15% in the relative ion extraction efficiency depending on whether analytes are supplied as metals or oxides. Implications of these findings on the accuracy achievable by state-of-the-art LA-ICP-MS systems are outlined. - Highlights: ► Specification

  20. Mass spectrometry in nuclear technology - a review of application of thermal ionization mass spectrometry in fuel reprocessing plants. PD-7-1

    International Nuclear Information System (INIS)

    Dakshinamoorthy, A.

    2007-01-01

    Mass spectrometry finds the widespread application in nuclear science and technology due to the fact that it can be employed for isotope composition measurements of different elements of interest and also concentration measurements of these elements using isotope dilution techniques. Thermal ionization mass spectrometer (TIMS), Inductively coupled plasma mass spectrometer (ICP-MS) and gas chromatography mass spectrometer (GC-MS) are the different types of mass spectrometers used in nuclear industry for the analyses of isotope composition of special nuclear material, trace impurities in nuclear fuels and components and characterization of various solvents respectively. Among them, TIMS plays a vital role in the nuclear fuel cycle in determining precisely the isotope composition of uranium, plutonium, D/H ratio in heavy water etc. TIMS is an indispensable analytical tool for nuclear material accounting at the input stage of a reprocessing plant by carrying out precise and accurate concentration measurement of plutonium and uranium by isotope dilution mass spectrometry (IDMS). It is the only accepted measurement technique for the purpose because of its high precision, better sensitivity and no quantitative separation is needed. The isotope abundance measurements of uranium and plutonium at this point are also useful for burn-up studies and isotope correlations. Mass spectrometric analysis of uranium and plutonium is also required for nuclear data measurements and calibrating other chemical methods

  1. Development of sedimentation field-flow fractionation-inductively coupled plasma mass-spectrometry for the characterization of environmental colloids

    International Nuclear Information System (INIS)

    Ranville, J.F.; Shanks, F.; Morrison, R.J.S.; Harris, T.; Doss, F.; Beckett, R.; Chittleborough, D.J.

    1999-01-01

    A relatively new hyphenated technique for the simultaneous size separation and elemental analysis of colloids has been further developed and applied to the characterization of soil colloids. Sedimentation field-flow fractionation (SdFFF) was directly interfaced to an inductively coupled plasma-mass spectrometer (ICP-MS) to provide high-resolution sizing and elemental analysis of colloids in the range 0.05-1.0 μm. For this work our existing SdFFF instrument was modified by addition of an upgraded motor and software for centrifuge speed control and data collection. Analytical techniques were developed for the calibration and drift correction of the ICP-MS data collected during on-line SdFFF-ICP-MS analyses. Software was developed to allow off-line computation of drift-corrected, elemental concentrations across the colloid size range. SdFFF-ICP-MS examination of two colloid samples isolated from surface soil horizons showed significant enrichment in iron-containing phases in both the smaller and larger colloids relative to intermediate particle sizes (∼0.3 0.3 μm). These results demonstrate the utility of SdFFF-ICP-MS for examination of soil chemistry and mineralogy and suggests the technique will have application to other environmental and geochemical studies. (Copyright (c) 1999 Elsevier Science B.V., Amsterdam. All rights reserved.)

  2. A micro-fluidic sub-microliter sample introduction system for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry using external aqueous calibration

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Heyong [Institute of Microanalytical Systems, Department of Chemistry, Zhejiang University, Hangzhou, 310027 (China); College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036 (China); Liu, Jinhua [College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036 (China); Xu, Zigang [Institute of Analytical and Applied Chemistry, Department of Chemistry, Zhejiang University, Hangzhou, 310027 (China); Yin, Xuefeng, E-mail: yinxf@zju.edu.cn [Institute of Microanalytical Systems, Department of Chemistry, Zhejiang University, Hangzhou, 310027 (China); College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036 (China)

    2012-07-15

    A microfluidic sub-microliter sample introducing system was developed for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry (ICP-MS). It consisted of a microfluidic chip integrating variable-volume sampling channels (0.1-0.8 {mu}L), an eight-way multi-functional valve used in flow injection analysis (FIA), a syringe pump and a peristaltic pump of the Ar ICP-MS instrument. Three solutions, i.e., 15, 40 and 100 g L{sup -1} glucose in 20% ethanol were used to simulate Chinese rice wine of the dry type, the semidry type and the semisweet type, each. The effects of their volume introduced into ICP-MS on the plasma stability and ICP-MS intensities were studied. The experimental results showed that neither alteration of plasma stability nor carbon deposition was observed when the sampling volume of 20% ethanol containing 100 g L{sup -1} glucose was downscaled to 0.8 {mu}L. Further reducing the sampling volume to 0.4 {mu}L, no significant difference between the intensities of multi-element standard prepared in three simulated Chinese rice wine matrices and those in aqueous solution was observed. It indicated no negative effect of Chinese rice wine matrix on the ICP-MS intensities. A sampling volume of 0.4 {mu}L was considered to be a good compromise between sensitivity and matrix effect. The flow rate of the carrier was chosen as 20 {mu}L min{sup -1} for obtaining peaks with the highest peak height within the shortest time. Based on these observations, a microflow injection ({mu}FI) method for the direct determination of cadmium and lead in Chinese rice wine by ICP-MS using an external aqueous calibration was developed. The sample throughput was 45 h{sup -1} with the detection limit of 19.8 and 10.4 ng L{sup -1} for Cd and Pb, respectively. The contents of Cd and Pb in 10 Chinese rice wine samples were measured. The results agreed well with those determined by ICP-MS with the conventional sampling system after microwave assisted digestion

  3. A micro-fluidic sub-microliter sample introduction system for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry using external aqueous calibration

    International Nuclear Information System (INIS)

    Cheng, Heyong; Liu, Jinhua; Xu, Zigang; Yin, Xuefeng

    2012-01-01

    A microfluidic sub-microliter sample introducing system was developed for direct analysis of Chinese rice wine by inductively coupled plasma mass spectrometry (ICP-MS). It consisted of a microfluidic chip integrating variable-volume sampling channels (0.1–0.8 μL), an eight-way multi-functional valve used in flow injection analysis (FIA), a syringe pump and a peristaltic pump of the Ar ICP-MS instrument. Three solutions, i.e., 15, 40 and 100 g L −1 glucose in 20% ethanol were used to simulate Chinese rice wine of the dry type, the semidry type and the semisweet type, each. The effects of their volume introduced into ICP-MS on the plasma stability and ICP-MS intensities were studied. The experimental results showed that neither alteration of plasma stability nor carbon deposition was observed when the sampling volume of 20% ethanol containing 100 g L −1 glucose was downscaled to 0.8 μL. Further reducing the sampling volume to 0.4 μL, no significant difference between the intensities of multi-element standard prepared in three simulated Chinese rice wine matrices and those in aqueous solution was observed. It indicated no negative effect of Chinese rice wine matrix on the ICP-MS intensities. A sampling volume of 0.4 μL was considered to be a good compromise between sensitivity and matrix effect. The flow rate of the carrier was chosen as 20 μL min −1 for obtaining peaks with the highest peak height within the shortest time. Based on these observations, a microflow injection (μFI) method for the direct determination of cadmium and lead in Chinese rice wine by ICP-MS using an external aqueous calibration was developed. The sample throughput was 45 h −1 with the detection limit of 19.8 and 10.4 ng L −1 for Cd and Pb, respectively. The contents of Cd and Pb in 10 Chinese rice wine samples were measured. The results agreed well with those determined by ICP-MS with the conventional sampling system after microwave assisted digestion. The recoveries of three

  4. Application of slurry nebulization to trace elemental analysis of some biological samples by inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Mochizuki, T.; Sakashita, A.; Iwata, H.; Ishibashi, Y.; Gunji, N.

    1991-01-01

    The application of slurry nebulization/inductively coupled plasma mass spectrometry (ICP-MS) to trace elemental analysis of biological samples has been investigated. Three standard samples of the National Institute of Standards and Technology (NIST) were dispersed in 1% aqueous Triton X-100 solution by grinding with a planetary micronizing mill. The resulting slurries were nebulized into an ICP without any additional treatments. The 1% (m/v) slurry of the NIST bovine liver showed no significant influence on cone blockage and signal suppression/enhancement. Detection limit, precision and accuracy were discussed for the determination of 24 elements of interest in bovine liver, rice flour and pine needles. Detection limits ranged from 0.0001 μg g -1 for U to 0.52 μg g -1 for Zn at the effective integrating time of 10 s. For high mass elements, low blank values were obtained, yielding excellent limits ( -1 ). Acceptable accuracy and precision were obtained for most of the elements in the NIST bovine liver and rice flour, even for the volatile elements, such as As, Se and Br. However, relatively poor accuracy was obtained for the analysis of pine needles. (orig.)

  5. Resin bead-thermal ionization mass spectrometry for determination of plutonium concentration in irradiated fuel dissolver solution

    International Nuclear Information System (INIS)

    Paul, Sumana; Shah, R.V.; Aggarwal, S.K.; Pandey, A.K.

    2015-01-01

    Determination of isotopic composition (IC) and concentration of plutonium (Pu) is necessary at various stages of nuclear fuel cycle which involves analysis of complex matrices like dissolver solution of irradiated fuel, nuclear waste stream etc. Mass spectrometry, e.g. thermal ionization mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICP-MS) are commonly used for determination of IC and concentration of plutonium. However, to circumvent matrix interferences, efficient separation as well as preconcentration of Pu is required prior to mass spectrometric analysis. Purification steps employing ion-exchange resins are widely used for the separation of Pu from dissolver solution or from mixture of other actinides e.g. U, Am. However, an alternative way is to selectively preconcentrate Pu on a resin bead, followed by direct loading of the bead on the filament of thermal ionization mass spectrometer

  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. Measurement of 240Pu/239Pu isotopic ratios in soils from the Marshall Islands using ICP-MS.

    Science.gov (United States)

    Muramatsu, Y; Hamilton, T; Uchida, S; Tagami, K; Yoshida, S; Robison, W

    2001-10-20

    Nuclear weapons tests conducted by the United States in the Marshall Islands produced significant quantities of regional or tropospheric fallout contamination. Here we report on some preliminary inductively coupled plasma-mass spectrometry (ICP-MS) measurements of plutonium isolated from seven composite soil samples collected from Bikini, Enewetak and Rongelap Atolls in the northern Marshall Islands. These data show that 240Pu/239Pu isotopic signatures in surface soils from the Marshall Island vary significantly and could potentially be used to help quantify the range and extent of fallout deposition (and associated impacts) from specific weapons tests. 137Cs and 60Co were also determined on the same set of soil samples for comparative purposes.

  8. Measurement of 240Pu/239Pu isotopic ratios in soils from the Marshall Islands using ICP-MS

    Energy Technology Data Exchange (ETDEWEB)

    Muramatsu, Y.; Uchida, S.; Tagami, K.; Yoshida, S. [Environmental and Toxicological Researches Group, National Institute of Radiological Sciences, Anagawa 4-9-1, Inage-ku, 263-8555 Chiba (Japan); Hamilton, T.; Robison, W. [Health and Ecological Assessment Division, Lawrence Livermore National Laboratory, P.O. Box 808, L-453, 94551-0808 Livermore, CA (United States)

    2001-10-20

    Nuclear weapons tests conducted by the United States in the Marshall Islands produced significant quantities of regional or tropospheric fallout contamination. Here we report on some preliminary inductively coupled plasma-mass spectrometry (ICP-MS) measurements of plutonium isolated from seven composite soil samples collected from Bikini, Enewetak and Rongelap Atolls in the northern Marshall Islands. These data show that 240Pu/239Pu isotopic signatures in surface soils from the Marshall Island vary significantly and could potentially be used to help quantify the range and extent of fallout deposition (and associated impacts) from specific weapons tests. 137Cs and 60Co were also determined on the same set of soil samples for comparative purposes.

  9. Measurement of 240Pu/239Pu isotopic ratios in soils from the Marshall Islands using ICP-MS

    International Nuclear Information System (INIS)

    Muramatsu, Y.; Uchida, S.; Tagami, K.; Yoshida, S.; Hamilton, T.; Robison, W.

    2001-01-01

    Nuclear weapons tests conducted by the United States in the Marshall Islands produced significant quantities of regional or tropospheric fallout contamination. Here we report on some preliminary inductively coupled plasma-mass spectrometry (ICP-MS) measurements of plutonium isolated from seven composite soil samples collected from Bikini, Enewetak and Rongelap Atolls in the northern Marshall Islands. These data show that 240Pu/239Pu isotopic signatures in surface soils from the Marshall Island vary significantly and could potentially be used to help quantify the range and extent of fallout deposition (and associated impacts) from specific weapons tests. 137Cs and 60Co were also determined on the same set of soil samples for comparative purposes

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1999-07-01

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

  11. Determination of albendazole sulfoxide in human plasma by using liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Saraner, Nihal; Özkan, Güler Yağmur; Güney, Berrak; Alkan, Erkin; Burul-Bozkurt, Nihan; Sağlam, Onursal; Fikirdeşici, Ezgi; Yıldırım, Mevlüt

    2016-06-01

    A rapid, simple and sensitive method was developed and validated using liquid chromatography-tandem mass spectrometry (LC-MS/MS) for determination of albendazole sulfoxide (ABZOX) in human plasma. The plasma samples were extracted by protein precipitation using albendazole sulfoxide-d3 as internal standard (IS). The chromatographic separation was performed on Waters Xbridge C18Column (100×4.6mm, 3.5μm) with a mobile phase consisting of ammonia solution, water and methanol at a flow rate of 0.70mL/min. ABZOX was detected and identified by mass spectrometry with electrospray ionization (ESI) in positive ion and multiple-reaction monitoring (MRM) mode. The method was linear in the range of 3-1500ng/mL for ABZOX. This method was successfully applied to the bioequivalence study in human plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. [Simultaneous determination of 7 arsenic species in chicken muscle and chicken liver with high performance liquid chromatography-inductively coupled plasma mass spectrometry].

    Science.gov (United States)

    Yang, Lijun; Hu, Qiaoru; Guo, Wei; Liu, Yumin; Song, Xiaohua; Zhang, Pengcheng

    2011-05-01

    A method for the simultaneous determination of 7 arsenic species was developed with high performance liquid chromatography and inductively coupled plasma mass spectrometry (HPLC-ICP-MS). The sample was extracted with artificial gastric juice. The HPLC separation was performed on an anion analytical column utilizing a gradient elution program of ammonium carbonate and water as the mobile phase. Identification and quantification were achieved by ICP-MS. Good linearities of 7 arsenic species were observed in the range from 1 microg/kg to 50 microg/kg with the correlation coefficients greater than 0.999. The average recoveries of 7 arsenic species spiked at the three levels of 1, 2 and 10 microg/kg ranged from 84.3% to 106.6% with the relative standard deviations of 1.4%-4.2%. The quantification limits of 7 arsenic species were 1 microg/kg. The method was proved to be good reproducibility, high sensitivity and simple preprocessing. This method is suitable for the simultaneous determination of 7 arsenic species in chicken muscle and chicken liver.

  13. Profiling metals in Cordyceps sinensis by using inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Wei, Xin; Hu, Hankun; Zheng, Baogeng; Arslan, Zikri; Huang, Hung-Chung; Mao, Weidong; Liu, Yi-Ming

    2017-01-28

    Cordyceps sinensis ( C. sinensis ) is a natural product that has diverse nutritional and medicinal values. Since the availability of natural C. sinensis becomes limited its authentication and quality control is of high significance. Herein we report on profiling of metals in C. sinensis by using inductively coupled plasma mass spectrometry (ICP-MS). The analysis reveals that C. sinensis contains a wide array of essential elements, including P, Mg, Zn, Cu, Fe, etc. Toxic metals detected are Cd, Pb, and As. In all five samples analyzed Pb contents are below 2.0 ppm. Arsenic level in C. sinensis caterpillar is significantly higher than that in its mycelium and varies from 3.0 to 32 ppm likely due to soil contamination. It's for the first time demonstrated in this work that clustering analysis on the proposed metal profiles consisting of 24 elements is very useful to identify "abnormal" C. sinensis samples, thus adding another dimension to the effective means for authentication and quality assessment of this highly demanded previous natural product.

  14. [Study on the determination of 14 inorganic elements in coffee by inductively coupled plasma mass spectrometry].

    Science.gov (United States)

    Nie, Xi-Du; Fu, Liang

    2013-07-01

    Samples of coffee were digested by microwave digestion, and inorganic elements amounts of Na, Mg, P, Ca, Cr, Mn, Fe, Co, Cu, Zn, As, Se, Mo and Pb in sample solutions were determined by inductively coupled plasma mass spectrometry (ICP-MS). HNO3 + H2O2 was used to achieve the complete decomposition of the organic matrix in a closed-vessel microwave oven. The working parameters of the instrument were optimized. The results showed that the relative standard deviation (RSD) was less than 3.84% for all the elements, and the recovery was found to be 92.00% -106.52% by adding standard recovery experiment. This method was simple, sensitive and precise and can perform simultaneous multi-elements determination of coffee, which could satisfy the sample examination request and provide scientific rationale for determining inorganic elements of coffee.

  15. Identification of platinum nanoparticles in road dust leachate by single particle inductively coupled plasma-mass spectrometry.

    Science.gov (United States)

    Folens, Karel; Van Acker, Thibaut; Bolea-Fernandez, Eduardo; Cornelis, Geert; Vanhaecke, Frank; Du Laing, Gijs; Rauch, Sebastien

    2018-02-15

    Elevated platinum (Pt) concentrations are found in road dust as a result of emissions from catalytic converters in vehicles. This study investigates the occurrence of Pt in road dust collected in Ghent (Belgium) and Gothenburg (Sweden). Total Pt contents, determined by tandem ICP-mass spectrometry (ICP-MS/MS), were in the range of 5 to 79ngg -1 , comparable to the Pt content in road dust of other medium-sized cities. Further sample characterization was performed by single particle (sp) ICP-MS following an ultrasonic extraction procedure using stormwater runoff for leaching. The method was found to be suitable for the characterization of Pt nanoparticles in road dust leachates. The extraction was optimized using road dust reference material BCR-723, for which an extraction efficiency of 2.7% was obtained by applying 144kJ of ultrasonic energy. Using this method, between 0.2% and 18% of the Pt present was extracted from road dust samples. spICP-MS analysis revealed that Pt in the leachate is entirely present as nanoparticles of sizes between 9 and 21nm. Although representing only a minor fraction of the total content in road dust, the nanoparticulate Pt leachate is most susceptible to biological uptake and hence most relevant in terms of bioavailability. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Laser ablation - inductive coupled plasma - mass spectrometer (LA-ICP-MS) geochemistry characterization of albitites associated to uranium in Lagoa da Rabicha deposit, Lagoa Real, BA (Brazil)

    International Nuclear Information System (INIS)

    Oliveira, Lucilia A. Ramos de; Rios, Francisco Javier; Amorim, Lucas Eustaquio Dias; Souza, Aurelio da Silva; Prates, Sonia Pinto; Yardley, Bruce; Matos, Evando Carele

    2009-01-01

    The LA-ICP-MS technique is a good tool for mineral geochemical characterization. The technique has high spatial resolution, elevated sensibility, low detection limits and multi-elementary analysis possibility. Almost all chemistry elements can be analyzed by this methodology. Briefly, this methodology consists in vaporize the sample by Laser Ablation, which is dragged by argon into the Plasma where are created and accelerated the ions. They are separated by their mass/charge ratio into the Mass Spectrometer, being conveyed to a detector that convert the signals in specters. In this work LA-ICP-MS analyses were performed in two albitites thin sections, a mineralized and a non mineralized sample. Both samples are from the Lagoa da Rabicha Deposit, Uranium Lagoa Real Province, BA. From these analysis it was possible to chemically characterize the minerals present in the samples and better understand the trace elements on them. The results for plagioclase in both samples show that it is albite (NaAlSi 3 O 8 ). The albite from sample 200907-20 shows traces of strontium, lanthanum, cerium, neodymium, samarium and thorium in one crystal. The albite from sample 200907-23 has strontium with uranium, yttrium and lead in smaller quantities. The results obtained in this work are very important and contribute to a better understanding of the uranium origin in Lagoa Real deposits. (author)

  17. An environmentally-friendly, highly efficient, gas pressure-assisted sample introduction system for ICP-MS and its application to detection of cadmium and lead in human plasma.

    Science.gov (United States)

    Cao, Yupin; Deng, Biyang; Yan, Lizhen; Huang, Hongli

    2017-05-15

    An environmentally friendly and highly efficient gas pressure-assisted sample introduction system (GPASIS) was developed for inductively-coupled plasma mass spectrometry. A GPASIS consisting of a gas-pressure control device, a customized nebulizer, and a custom-made spray chamber was fabricated. The advantages of this GPASIS derive from its high nebulization efficiencies, small sample volume requirements, low memory effects, good precision, and zero waste emission. A GPASIS can continuously, and stably, nebulize 10% NaCl solution for more than an hour without clogging. Sensitivity, detection limits, precision, long-term stability, double charge and oxide ion levels, nebulization efficiencies, and matrix effects of the sample introduction system were evaluated. Experimental results indicated that the performance of this GPASIS, was equivalent to, or better than, those obtained by conventional sample introduction systems. This GPASIS was successfully used to determine Cd and Pb by ICP-MS in human plasma. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  19. Investigation of Elemental Mass Spectrometry in Pharmacology for Peptide Quantitation at Femtomolar Levels.

    Directory of Open Access Journals (Sweden)

    Emmanuelle Cordeau

    Full Text Available In the search of new robust and environmental-friendly analytical methods able to answer quantitative issues in pharmacology, we explore liquid chromatography (LC associated with elemental mass spectrometry (ICP-MS to monitor peptides in such complex biological matrices. The novelty is to use mass spectrometry to replace radiolabelling and radioactivity measurements, which represent up-to now the gold standard to measure organic compound concentrations in life science. As a proof of concept, we choose the vasopressin (AVP/V1A receptor system for model pharmacological assays. The capacity of ICP-MS to provide highly sensitive quantitation of metallic and hetero elements, whatever the sample medium, prompted us to investigate this technique in combination with appropriate labelling of the peptide of interest. Selenium, that is scarcely present in biological media, was selected as a good compromise between ICP-MS response, covalent tagging ability using conventional sulfur chemistry and peptide detection specificity. Applying selenium monitoring by elemental mass spectrometry in pharmacology is challenging due to the very high salt content and organic material complexity of the samples that produces polyatomic aggregates and thus potentially mass interferences with selenium detection. Hyphenation with a chromatographic separation was found compulsory. Noteworthy, we aimed to develop a straightforward quantitative protocol that can be performed in any laboratory equipped with a standard macrobore LC-ICP-MS system, in order to avoid time-consuming sample treatment or special implementation of instrumental set-up, while allowing efficient suppression of all mass interferences to reach the targeted sensitivity. Significantly, a quantification limit of 57 ng Se L-1 (72 femtomoles of injected Se was achieved, the samples issued from the pharmacological assays being directly introduced into the LC-ICP-MS system. The established method was successfully

  20. Asymmetric flow field-flow fractionation coupled to inductively coupled plasma mass spectrometry for the quantification of quantum dots bioconjugation efficiency.

    Science.gov (United States)

    Menéndez-Miranda, Mario; Encinar, Jorge Ruiz; Costa-Fernández, José M; Sanz-Medel, Alfredo

    2015-11-27

    Hyphenation of asymmetric flow field-flow fractionation (AF4) to an on-line elemental detection (inductively coupled plasma-mass spectrometry, ICP-MS) is proposed as a powerful diagnostic tool for quantum dots bioconjugation studies. In particular, conjugation effectiveness between a "model" monoclonal IgG antibody (Ab) and CdSe/ZnS core-shell Quantum Dots (QDs), surface-coated with an amphiphilic polymer, has been monitored here by such hybrid AF4-ICP-MS technique. Experimental conditions have been optimized searching for a proper separation between the sought bioconjugates from the eventual free reagents excesses employed during the bioconjugation (QDs and antibodies). Composition and pH of the carrier have been found to be critical parameters to ensure an efficient separation while ensuring high species recovery from the AF4 channel. An ICP-MS equipped with a triple quadropole was selected as elemental detector to enable sensitive and reliable simultaneous quantification of the elemental constituents, including sulfur, of the nanoparticulated species and the antibody. The hyphenated technique used provided nanoparticle size-based separation, elemental detection, and composition analysis capabilities that turned out to be instrumental in order to investigate in depth the Ab-QDs bioconjugation process. Moreover, the analytical strategy here proposed allowed us not only to clearly identify the bioconjugation reaction products but also to quantify nanoparticle:antibodies bioconjugation efficiency. This is a key issue in future development of analytical and bioanalytical photoluminescent QDs applications. Copyright © 2015 Elsevier B.V. All rights reserved.

  1. Direct determination of mercury in cosmetic samples by isotope dilution inductively coupled plasma mass spectrometry after dissolution with formic acid

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Ying; Shi, Zeming; Zong, Qinxia; Wu, Peng; Su, Jing [Sichuan Provincial Key Laboratory of Nuclear Technology in Geology, College of Nuclear Technology and Automation Engineering, Chengdu University of Technology, Chengdu 610059 (China); Liu, Rui, E-mail: liur.ray@gmail.com [Mineral Resources Chemistry Key Laboratory of Sichuan Higher Education Institutions, College of Materials and Chemistry and Chemical Engineering, Chengdu University of Technology, Chengdu 610059 (China)

    2014-02-17

    Graphical abstract: -- Highlights: •Simple, sensitive, and accurate method is established for mercury determination in cosmetics. •The sample preparation procedure is highly simplified. •Isotope dilution efficiently eliminates matrix effect. •First report of using formic acid based method in combination with PVG-ID-ICP MS for mercury quantitation in cosmetics. -- Abstract: A new method was proposed for the accurate determination of mercury in cosmetic samples based on isotopic dilution (ID)-photochemical vapor generation (PVG)-inductively coupled plasma mass spectrometry (ICP MS) measurement. Cosmetic samples were directly dissolved in formic acid solution and subsequently subjected to PVG for the reduction of mercury into vapor species following by ICP MS detection. Therefore, the risks of analyte contamination and loss were avoided. Highly enriched {sup 201}Hg isotopic spike is added to cosmetics and the isotope ratios of {sup 201}Hg/{sup 202}Hg were measured for the quantitation of mercury. With ID calibration, the influences originating from sample matrixes for the determination of mercury in cosmetic samples have been efficiently eliminated. The effects of several experimental parameters, such as the concentration of the formic acid, and the flow rates of carrier gas and sample were investigated. The method provided good reproducibility and the detection limits were found to be 0.6 pg mL{sup −1}. Finally, the developed method was successfully applied for the determination of mercury in six cosmetic samples and a spike test was performed to verify the accuracy of the method.

  2. Cerium oxide-deposited mesoporous silica nanoparticles for the determination of carcinoembryonic antigen in serum using inductively coupled plasma-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Choi, H.W. [Department of Chemistry, NSBI, Dankook University, 126 Jukjeon-dong, Suji-gu, Yongin-si, Gyeonggi-do 448-701 (Korea, Republic of); Lee, K.H.; Hur, N.H. [Department of Chemistry, Sogang University, Shinsu-dong, Mapo-gu, Seoul (Korea, Republic of); Lim, H.B., E-mail: plasma@dankook.ac.kr [Department of Chemistry, NSBI, Dankook University, 126 Jukjeon-dong, Suji-gu, Yongin-si, Gyeonggi-do 448-701 (Korea, Republic of)

    2014-10-17

    Highlights: • Sandwich-type immunoassay using ICP-MS and nanoparticles to determine biomarkers. • CeO{sub 2}-deposited mesoporous silica nanoparticles were synthesized as a probe. • Ratiometric measurement significantly improved the calibration linearity. • Excellent detection limit was achieved by signal amplification. - Abstract: CeO{sub 2}-deposited mesoporous silica nanoparticles were synthesized as a probe to determine carcinoembryonic antigen (CEA) in serum by inductively coupled plasma-mass spectrometry (ICP-MS). The prepared mesoporous nanoparticles were modified and tagged to the target for sandwich-type immunoassay. Fe{sub 3}O{sub 4} magnetic nanoparticles (MNPs) were also synthesized and immobilized with antibody to extract the target biomarker. The calibration curve of the synthesized CeO{sub 2}-deposited silica nanoparticles, which was plotted by the signal ratio of {sup 140}Ce/{sup 57}Fe measured by ICP-MS vs. the concentration of CEA, showed excellent linearity and sensitivity owing to the signal amplification and low spectral interference. Under optimal conditions, the sandwich-type analytical method was applied to determine CEA in serum spiked in the range of 0.001–5 ng mL{sup −1} and showed a limit of detection of 0.36 ng mL{sup −1}. Since the deposited CeO{sub 2} in the mesoporous silica layer can be substituted by other metal compounds, various kinds of metal-deposited nanoparticles can be prepared as probe materials for multiplex detection in bioanalysis.

  3. Trends in preconcentration procedures for metal determination using atomic spectrometry techniques

    International Nuclear Information System (INIS)

    Godoi Pereira, M. de; Arruda, M.A.Z.

    2003-01-01

    Methods for metal preconcentration are often described in the literature. However, purposes are often different, depending on whether the methods are applied in environmental, clinical or technological fields. The respective method needs to be efficient, give high sensitivity, and ideally also is selective which is useful when used in combination with atomic spectroscopy. This review presents the actual tendencies in metal preconcentration using techniques such as flame atomic absorption spectrometry (FAAS), electrothermal atomic absorption spectrometry (ETAAS), hydride generation atomic absorption spectrometry (HGAAS), inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry (ICP-MS). Procedures based on related to electrochemical, coprecipitation/precipitation, liquid-liquid and solid-liquid extraction and atom trapping mechanisms are presented. (author)

  4. Ultra-Sensitive Elemental Analysis Using Plasmas 5.Speciation of Arsenic Compounds in Biological Samples by High Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry System

    Science.gov (United States)

    Kaise, Toshikazu

    Arsenic originating from the lithosphere is widely distributed in the environment. Many arsenicals in the environment are in organic and methylated species. These arsenic compounds in drinking water or food products of marine origin are absorbed in human digestive tracts, metabolized in the human body, and excreted viatheurine. Because arsenic shows varying biological a spects depending on its chemical species, the biological characteristics of arsenic must be determined. It is thought that some metabolic pathways for arsenic and some arsenic circulation exist in aqueous ecosystems. In this paper, the current status of the speciation analysis of arsenic by HPLC/ICP-MS (High Performance Liquid Chromatography-Inductively Coupled Plasma Mass spectrometry) in environmental and biological samples is summarized using recent data.

  5. Determination of selenium in red blood cells by inductively coupled plasma mass spectrometry (ICP-MS) after microwave digestion

    International Nuclear Information System (INIS)

    Tinggi, U.; Francis, R.; Shanin, M.; Scheelings, P.; Gianduzzo, T.; Nicol, D.

    2004-01-01

    Selenium is an essential trace element and its levels in blood have been widely used for assessing Se status in humans. A suitable method for the determination of Se in red blood cells (RBC) using ICP-MS after microwave digestion was developed. The blood samples were obtained from patients with benign prostatic hyperplasia (BPH), who attended urology clinics at the Princess Alexandra hospital, Brisbane, Australia. No apparent polyatomic and matrix interferences were encountered when 82 Se isotope was used for the analysis of Se levels in RBC. Whole Blood Seronorm Trace Elements (SERO, Norway) and dogfish muscle (DORM-1, NRCC) were used as reference materials for method validation. The method was rapid and accurate, and ideal for routine analysis of Se in RBC, and in particular for assessing of Se status in humans. (author)

  6. Application of neutron activation analysis and inductively coupled plasma mass spectrometry to the determination of toxic and essential elements in Australian foods

    International Nuclear Information System (INIS)

    Fardy, J.J.; McOrist, G.D.; Farrar, Y.J.; Bowles, C.J.; Warner, I.M.; Tan Mingguang

    1994-01-01

    Current Australian Legislation specifies the maximum permitted levels of nine toxic elements in food while the National Health and Medical Research Council (NH and MRC) has listed recommended daily intake figures for seven essential elements. This investigation examined the compliance of Australian foods with both these requirements. Australia-wide samples of representative foods from the diets of Australians were used in this study after the NH and MRC kindly permitted us to join their Market Basket (Noxious Substance) Survey. Both toxic and essential element concentrations in these foods were determined using the advanced analytical techniques of instrumental (INAA) and radiochemical neutron activation analysis (RNAA) and inductively coupled plasma mass spectrometry (ICP-MS). With very few exceptions, foods do not exceed the maximum permitted levels for toxic substances. Daily intake figures for essential elements generally lie close to the maximum recommended values listed by NH and MRC. Since another source of toxic element intake is drinking water, samples from different locations were analyzed by NAA and inductively coupled plasma atomic emission spectroscopy (ICP-AES). They were extremely low in trace elements with the exception of copper, iron, zinc and lead which approached the maximum permitted concentrations. The performance of NAA and ICP-MS for analyzing biological materials were compared. NAA cannot match the superior sensitivity for a wider range of elements obtained by ICP-MS. This has been verified for a wide range of food materials. While NAA is an inconvenient and time-consuming technique for many applications, it does not suffer from blank problems after irradiation of the sample and becomes the preferred technique where low limits of detection are required for trace concentrations in solid samples. (author). 22 refs, 27 figs, 21 tabs

  7. Determination of rivaroxaban in patient's plasma samples by anti-Xa chromogenic test associated to High Performance Liquid Chromatography tandem Mass Spectrometry (HPLC-MS/MS).

    Science.gov (United States)

    Derogis, Priscilla Bento Matos; Sanches, Livia Rentas; de Aranda, Valdir Fernandes; Colombini, Marjorie Paris; Mangueira, Cristóvão Luis Pitangueira; Katz, Marcelo; Faulhaber, Adriana Caschera Leme; Mendes, Claudio Ernesto Albers; Ferreira, Carlos Eduardo Dos Santos; França, Carolina Nunes; Guerra, João Carlos de Campos

    2017-01-01

    Rivaroxaban is an oral direct factor Xa inhibitor, therapeutically indicated in the treatment of thromboembolic diseases. As other new oral anticoagulants, routine monitoring of rivaroxaban is not necessary, but important in some clinical circumstances. In our study a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was validated to measure rivaroxaban plasmatic concentration. Our method used a simple sample preparation, protein precipitation, and a fast chromatographic run. It was developed a precise and accurate method, with a linear range from 2 to 500 ng/mL, and a lower limit of quantification of 4 pg on column. The new method was compared to a reference method (anti-factor Xa activity) and both presented a good correlation (r = 0.98, p plasma samples for rivaroxaban measurement by HPLC-MS/MS without interferences. The chromogenic and HPLC-MS/MS methods were highly correlated and should be used as clinical tools for drug monitoring. The method was applied successfully in a group of 49 real-life patients, which allowed an accurate determination of rivaroxaban in peak and trough levels.

  8. Developments in and applications of capillary electrophoresis inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    Taylor, K.A.

    1999-08-01

    This project has set out to design and optimise a robust and efficient interface for capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) and to investigate the application of the technique in elemental speciation studies. An interface was constructed using a commercial microconcentric nebuliser (MCN) and a cyclonic spray chamber. The cyclonic spray chamber was designed specifically to provide rapid sample response and washout and to minimise sample dispersion. Isoforms of the heavy metal binding protein, metallothionein, were separated and the bound metals detected to characterise the interface. Suction from the self-aspirating nebuliser was identified as the principal factor controlling electrophoretic resolution. To maintain resolution, two methods for counterbalancing the nebuliser suction were investigated. In the first method an optimised make-up flow was employed, and in the second a negative pressure was applied to the buffer vial during the separation. The negative pressure method was preferred because it did not significantly compromise sensitivity. The MCN was found to be prone to regular blocking which compromised the analytical precision of the system. A second interface was constructed using a glass MicroMist nebuliser. The MicroMist nebuliser was found to be less prone to blocking than the MCN and significantly improved the precision of the system to less than 4.3% RSD. The MicroMist nebuliser did, however, provide a lower sensitivity. The advantage of employing an electroosmotic flow marker to correct for migration time drifts was demonstrated. A CE-ICP-MS method was developed for the speciation of selenium in selenium enriched yeasts and nutritional supplements. Selenoamino acids and inorganic selenium species were separated, as anions, under strong electroosmotic flow conditions. Methods to enhance the selenium sensitivity were investigated. A proteolytic enzyme extraction method was employed and the effect of the

  9. Application of inductively coupled plasma mass spectrometry for multielement analysis in small sample amounts of thyroid tissue from Chernobyl area

    International Nuclear Information System (INIS)

    Becker, J.S.; Dietze, H.J.; Boulyga, S.F.; Bazhanova, N.N.; Kanash, N.V.; Malenchenko, A.F.

    2000-01-01

    As a result of the Chernobyl nuclear power plant accident in 1986, thyroid pathologies occurred among children in some regions of belarus. Besides the irradiation of children's thyroids by radioactive iodine and caesium nuclides, toxic elements from fallout are a direct risk to health. Inductively coupled plasma quadrupole-based mass spectrometry (Icp-Ms) and instrumental neutron activation analysis (IAA) were used for multielement determination in small amounts (I-10 mg) of human thyroid tissue samples. The accuracy of the applied analytical technique for small biological sample amounts was checked using NIST standard reference material oyster tissue (SRM 1566 b). Almost all essential elements as well as a number of toxic elements such as Cd, Pb, Hg, U etc. Were determined in a multitude of human thyroid tissues by quadrupole-based Icp-Ms using micro nebulization. In general, the thyroid tissue affected by pathology is characterized by higher calcium content. Some other elements, among them Sr, Zn, Fe, Mn, V, As, Cr, Ni, Pb, U, Ba, Sb, were also Accumulated in such tissue. The results obtained will be used as initial material for further specific studies of the role of particular elements in thyroid pathology development

  10. Analysis of humic colloid borne trace elements by flow field-flow fractionation, gel permeation chromatography and icp-mass spectrometry

    International Nuclear Information System (INIS)

    Ngo, Manh Thang; Beck, H.P; Geckeis, H.; Kim, J.I.

    1999-01-01

    Groundwater samples containing aquatic