Concentration of vanadium in crude oil and water using inductively-coupled plasma spectrometry

International Nuclear Information System (INIS)

Amin, Y.M.; Hassan, M.A.; Junkin, K.; Mahat, R.H.; Raphie, B.

1991-01-01

Vanadium is a trace element that is usually associated to crude oil and its products. In this study the concentration of vanadium in a few samples of local crude oil, sea and river water were determined using inductively-coupled plasma spectrometry (ICP). It is hoped that the concentration of vanadium in water can be used to indicate the possible extent of oil contamination

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

Online Coupling of Flow-Field Flow Fractionation and Single Particle Inductively Coupled Plasma-Mass Spectrometry: Characterization of Nanoparticle Surface Coating Thickness and Aggregation State

Science.gov (United States)

Surface coating thickness and aggregation state have strong influence on the environmental fate, transport, and toxicity of engineered nanomaterials. In this study, flow-field flow fractionation coupled on-line with single particle inductively coupled plasma-mass spectrometry i...

Minimally-invasive Laser Ablation Inductively Coupled Plasma Mass Spectrometry analysis of model ancient copper alloys

Energy Technology Data Exchange (ETDEWEB)

Walaszek, Damian [University of Warsaw, Faculty of Chemistry, Biological and Chemical Research Centre, Żwirki i Wigury 101, 02-089 Warszawa (Poland); Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Senn, Marianne; Wichser, Adrian [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Faller, Markus [Laboratory for Jointing Technology and Corrosion, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland); Wagner, Barbara; Bulska, Ewa [University of Warsaw, Faculty of Chemistry, Biological and Chemical Research Centre, Żwirki i Wigury 101, 02-089 Warszawa (Poland); Ulrich, Andrea [Laboratory for Analytical Chemistry, Swiss Federal Laboratories for Materials Science and Technology, Überlandstrasse 129, CH-8600 Dübendorf (Switzerland)

2014-09-01

This work describes an evaluation of a strategy for multi-elemental analysis of typical ancient bronzes (copper, lead bronze and tin bronze) by means of laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS).The samples originating from archeological experiments on ancient metal smelting processes using direct reduction in a ‘bloomery’ furnace as well as historical casting techniques were investigated with the use of the previously proposed analytical procedure, including metallurgical observation and preliminary visual estimation of the homogeneity of the samples. The results of LA-ICPMS analysis were compared to the results of bulk composition obtained by X-ray fluorescence spectrometry (XRF) and by inductively coupled plasma mass spectrometry (ICPMS) after acid digestion. These results were coherent for most of the elements confirming the usefulness of the proposed analytical procedure, however the reliability of the quantitative information about the content of the most heterogeneously distributed elements was also discussed in more detail. - Highlights: • The previously proposed procedure was evaluated by analysis of model copper alloys. • The LA-ICPMS results were comparable to the obtained by means of XRF and ICPMS. • LA-ICPMS results indicated the usefulness of the proposed analytical procedure.

Multielement determination of rare earth elements in rock sample by liquid chromatography / inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Hamanaka, Tadashi; Itoh, Akihide; Itoh, Shinya; Sawatari, Hideyuki; Haraguchi, Hiroki.

1995-01-01

Rare earth elements in geological standard rock sample JG-1 (granodiolite)issued from the Geological Survey of Japan have been determined by a combined system of liquid chromatography and inductively coupled plasma mass spectrometry. (author)

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)

Implementation of suitable flow injection/sequential-sample separation/preconcentration schemes for determination of trace metal concentrations using detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

DEFF Research Database (Denmark)

Hansen, Elo Harald; Wang, Jianhua

2002-01-01

Various preconditioning procedures encomprising appropriate separation/preconcentration schemes in order to obtain optimal sensitivity and selectivity characteristics when using electrothermal atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICPMS...

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

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.

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.

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

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

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.

Coupling nanoliter high-performance liquid chromatography to inductively coupled plasma mass spectrometry for arsenic speciation.

Science.gov (United States)

Cheng, Heyong; Shen, Lihuan; Liu, Jinhua; Xu, Zigang; Wang, Yuanchao

2018-04-01

Nanoliter high-performance liquid chromatography shows low consumption of solvents and samples, offering one of the best choices for arsenic speciation in precious samples in combination with inuctively coupled plasma mass spectrometry. A systematic investigation on coupling nanoliter high-performance liquid chromatography to inductively coupled plasma mass spectrometry from instrument design to injected sample volume and mobile phase was performed in this study. Nanoflow mobile phase was delivered by flow splitting using a conventional high-pressure pump with reuse of mobile phase waste. Dead volume was minimized to 60 nL for the sheathless interface based on the previously developed nanonebulizer. Capillary columns for nanoliter high-performance liquid chromatography were found to be sensitive to sample loading volume. An apparent difference was also found between the mobile phases for nanoliter and conventional high-performance liquid chromatography. Baseline separation of arsenite, arsenate, monomethylarsenic, and dimethylarsenic was achieved within 11 min on a 15 cm C 18 capillary column and within 12 min on a 25 cm strong anion exchange column. Detection limits of 0.9-1.8 μg/L were obtained with precisions variable in the range of 1.6-4.2%. A good agreement between determined and certified values of a certified reference material of human urine (GBW 09115) validated its accuracy along with good recoveries (87-102%). © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

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

Inductively coupled plasma-mass spectrometry: an initial assessment of the VG isotopes Plasmaquad

International Nuclear Information System (INIS)

Brown, R.M.; Pickford, C.J.

1985-04-01

The Chemical Analysis Group has been approached by a British Scientific instrument maker regarding the possibility of the group participating in a Department of Trade and Industry sponsored scheme whereby we would have a 12 month period to assess the advantages and disadvantages of a new analytical technique, Inductively Coupled Plasma-Mass Spectrometry. This report details our initial assessment of the instrument, carried out in order to decide whether to participate in the scheme. We have attempted to discover whether the instrument meets the claims made of it in advertising literature, and have attempted to compare the technique with another, proven technique, Inductively Coupled Plasma - Optical Emission Spectroscopy. The Plasmaquad offers excellent sensitivity for almost all of the elements of the periodic table, giving a distinct improvement over the Chemical Analysis Group's present capabilities for many elements. The isotope ratio measuring ability is important, as the Group has no such capability at the moment and a demand for this type of measurement is foreseen. Our conclusions, while inevitably somewhat subjective, form the basis for recommending Harwell to participate in the scheme. (author)

Gas chromatography--inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental water samples.

Science.gov (United States)

Heisterkamp, M; Adams, F C

2001-07-01

The application of inductively coupled plasma--time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental waters is described. Construction of the transfer line was achieved by means of a relatively simple and rapid coupling procedure. Derivatization of the ionic lead species was achieved by in-situ propylation with sodium tetrapropylborate; simultaneous extraction of the derivatized compounds in hexane was followed by separation and detection by capillary gas chromatography hyphenated to inductively coupled plasma-time-of-flight mass spectrometry. Detection limits for the different organolead species ranged from 10 to 15 fg (as Pb), corresponding to procedural detection limits between 50 and 75 ng L(-1), on the basis of a 50 mL snow sample, extraction with 200 microL hexane, and subsequent injection of 1 microL of the organic extract on to the column. The accuracy of the system was confirmed by additional analysis of the water samples by capillary gas chromatography coupled with microwave-induced plasma-atomic-emission spectrometry and the analysis of a standard reference material CRM 605 (road dust) with a certified content of trimethyllead.

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

Polyatomic ions in inductively coupled plasma-mass spectrometry

International Nuclear Information System (INIS)

Ferguson, Jill Wisnewski; Dudley, Timothy J.; Sears, Kyle C.; McIntyre, Sally M.; Gordon, Mark S.; Houk, R.S.

2009-01-01

Several polyatomic ions in inductively coupled plasma-mass spectrometry are studied experimentally and by computational methods. Novel calculations based on spin-restricted open shell second order perturbation theory (ZAPT2) and coupled cluster (CCSD(T)) theory are performed to determine the energies, structures and partition functions of the ions. These values are combined with experimental data to evaluate a dissociation constant and gas kinetic temperature (T gas ) value. In our opinion, the resulting T gas value can sometimes be interpreted to deduce the location where the polyatomic ion of interest is generated. The dissociation of N 2 H + to N 2 + leads to a calculated T gas of 4550 to 4900 K, depending on the computational data used. The COH + to CO + system yields a similar temperature, which is not surprising considering the similar energies and structures of COH + and N 2 H + . The dissociation of H 2 CO + to HCO + leads to a much lower T gas ( 2 COH + to HCOH + generates a T gas value between those from the other H x CO + ions studied here. All of these measured T gas values correspond to formation of extra polyatomic ion in the interface or extraction region. The computations reveal the existence of isomers such as HCO + and COH + , and H 2 CO + and HCOH + , which have virtually the same m/z values and need to be considered in the interpretation of results.

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

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.

Determination of trace and ultra-trace elements in Dergaon meteorite by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Balaram, V.; Gnaneswara Rao, T.; Anjaiah, K.V.; Phukon, N.; Majumdar, A.C.

2003-01-01

In this paper, a detailed methodology for high precision measurement of several trace and ultra-trace elements including REE and PGE have been presented using effective sample preparation techniques and inductively coupled plasma mass spectrometry. Discussion is focussed on aspects, such as total dissolution and recovery of all elements, minimization of oxide and doubly-charged and other polyatomic ion interferences, calibration by matrix matching standards, accuracy and precision

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.

Assessment of the analytical capabilities of inductively coupled plasma-mass spectrometry

Science.gov (United States)

Taylor, Howard E.; Garbarino, John R.

1988-01-01

A thorough assessment of the analytical capabilities of inductively coupled plasma-mass spectrometry was conducted for selected analytes of importance in water quality applications and hydrologic research. A multielement calibration curve technique was designed to produce accurate and precise results in analysis times of approximately one minute. The suite of elements included Al, As, B, Ba, Be, Cd, Co, Cr, Cu, Hg, Li, Mn, Mo, Ni, Pb, Se, Sr, V, and Zn. The effects of sample matrix composition on the accuracy of the determinations showed that matrix elements (such as Na, Ca, Mg, and K) that may be present in natural water samples at concentration levels greater than 50 mg/L resulted in as much as a 10% suppression in ion current for analyte elements. Operational detection limits are presented.

Experimental evidence of state-selective charge transfer in inductively coupled plasma-atomic emission spectrometry

International Nuclear Information System (INIS)

Chan, George C.-Y.; Hieftje, Gary M.

2004-01-01

State-selective charge-transfer behavior was observed for Fe, Cr, Mn and Cu in inductively coupled plasma (ICP)-atomic emission spectrometry. Charge transfer from Ar + to Fe, Cr and Mn is state-selective because of inefficient collisional mixing of the quasiresonant charge-transfer energy levels with nearby levels. This low efficiency is the consequence of differences in electronic configuration of the core electrons. The reason for state-selective charge-transfer behavior to Cu is not clear, although a tentative explanation based on efficiency of intramultiplet and intermultiplet mixing for this special case is offered

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...

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

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

Partial microwave-assisted wet digestion of animal tissue using a baby-bottle sterilizer for analyte determination by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Matos, Wladiana O.; Menezes, Eveline A.; Gonzalez, Mario H.; Costa, Leticia M.; Trevizan, Lilian C.; Nogueira, Ana Rita A.

2009-01-01

A procedure for partial digestion of bovine tissue is proposed using polytetrafluoroethylene (PTFE) micro-vessels inside a baby-bottle sterilizer under microwave radiation for multi-element determination by inductively coupled plasma optical emission spectrometry (ICP OES). Samples were directly weighed in laboratory-made polytetrafluoroethylene vessels. Nitric acid and hydrogen peroxide were added to the uncovered vessels, which were positioned inside the baby-bottle sterilizer, containing 500 mL of water. The hydrogen peroxide volume was fixed at 100 μL. The system was placed in a domestic microwave oven and partial digestion was carried out for the determination of Ca, Cu, Fe, Mg, Mn and Zn by inductively coupled plasma optical emission spectrometry. The single-vessel approach was used in the entire procedure, to minimize contamination in trace analysis. Better recoveries and lower residual carbon content (RCC) levels were obtained under the conditions established through a 2 4-1 fractional factorial design: 650 W microwave power, 7 min digestion time, 50 μL nitric acid and 50 mg sample mass. The digestion efficiency was ascertained according to the residual carbon content determined by inductively coupled plasma optical emission spectrometry. The accuracy of the proposed procedure was checked against two certified reference materials.

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.

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...

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

Elemental analysis using instrumental neutron activation analysis and inductively coupled plasma atomic emission spectrometry: a comparative study

International Nuclear Information System (INIS)

Chung, Yong Sam; Choi, Kwang Soon; Moon, Jong Hwa; Kim, Sun Ha; Lim, Jong Myoung; Kim, Young Jin; Quraishi, Shamshad Begum

2003-05-01

Elemental analyses for certified reference materials were carried out using instrumental neutron activation analysis and inductively coupled plasma-atomic emission spectrometry. Five Certified Reference Materials (CRM) were selected for the study on comparative analysis of environmental samples. The CRM are Soil (NIST SRM 2709), Coal fly ash (NIST SRM 1633a), urban dust (NIST SRM 1649a) and air particulate on filter media (NIST SRM 2783 and human hair (GBW 09101)

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.

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)

Serum/plasma methylmercury determination by isotope dilution gas chromatography-inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Baxter, Douglas C., E-mail: douglas.baxter@alsglobal.com [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Faarinen, Mikko [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Osterlund, Helene; Rodushkin, Ilia [ALS Scandinavia AB, Aurorum 10, 977 75 Lulea (Sweden); Division of Geosciences, Lulea University of Technology, 977 87 Lulea (Sweden); Christensen, Morten [ALS Scandinavia AB, Maskinvaegen 2, 183 53 Taeby (Sweden)

2011-09-09

Highlights: {center_dot} We determine methylmercury in serum and plasma using isotope dilution calibration. {center_dot} Separation by gas chromatography and detection by inductively coupled plasma mass spectrometry. {center_dot} Data for 50 specimens provides first reference range for methylmercury in serum. {center_dot} Serum samples shown to be stable for 11 months in refrigerator. - Abstract: A method for the determination of methylmercury in plasma and serum samples was developed. The method uses isotope dilution with {sup 198}Hg-labeled methylmercury, extraction into dichloromethane, back-extraction into water, aqueous-phase ethylation, purge and trap collection, thermal desorption, separation by gas chromatography, and mercury isotope specific detection by inductively coupled plasma mass spectrometry. By spiking 2 mL sample with 1.2 ng tracer, measurements in a concentration interval of (0.007-2.9) {mu}g L{sup -1} could be performed with uncertainty amplification factors <2. A limit of quantification of 0.03 {mu}g L{sup -1} was estimated at 10 times the standard deviation of concentrations measured in preparation blanks. Within- and between-run relative standard deviations were <10% at added concentration levels of 0.14 {mu}g L{sup -1}, 0.35 {mu}g L{sup -1} and 2.8 {mu}g L{sup -1}, with recoveries in the range 82-110%. Application of the method to 50 plasma/serum samples yielded a median (mean; range) concentration of methylmercury of 0.081 (0.091; <0.03-0.19) {mu}g L{sup -1}. This is the first time methylmercury has been directly measured in this kind of specimen, and is therefore the first estimate of a reference range.

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.

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)

Multi-elemental analysis of aqueous geological samples by inductively coupled plasma-optical emission spectrometry

Science.gov (United States)

Todorov, Todor I.; Wolf, Ruth E.; Adams, Monique

2014-01-01

Typically, 27 major, minor, and trace elements are determined in natural waters, acid mine drainage, extraction fluids, and leachates of geological and environmental samples by inductively coupled plasma-optical emission spectrometry (ICP-OES). At the discretion of the analyst, additional elements may be determined after suitable method modifications and performance data are established. Samples are preserved in 1–2 percent nitric acid (HNO3) at sample collection or as soon as possible after collection. The aqueous samples are aspirated into the ICP-OES discharge, where the elemental emission signals are measured simultaneously for 27 elements. Calibration is performed with a series of matrix-matched, multi-element solution standards.

Evaluation of an inductively-coupled plasma with an extended-sleeve torch as an atomization cell for laser-excited fluorescence spectrometry.

Science.gov (United States)

Kosinski, M A; Uchida, H; Winefordner, J D

1983-05-01

An inductively-coupled plasma (ICP) with an extended-sleeve torch has been evaluated as an atomization cell for laser-excited fluorescence spectrometry. Limits of detection for 20 lines are given. The detection power is almost equivalent to that obtained by excitation with a hollow-cathode lamp. Interelement effects and spectral interferences are discussed.

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

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.

Determination of trace amounts of cerium in paint by inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Wong, K.L.

1981-01-01

The determination of Ce in paint by inductively coupled plasma atomic emission spectrometry (ICP-OES) is described, and the detection limit of ICP-OES of 0.0004 ppM is compared with that of other methods. The effects of the major elemental components of paint, Si, Pb, Cr, and Na on the ICP-OES determination of Ce were studied. The interference of 400 ppM of the other ions on the determination of 10 ppM Ce was small (0 to 3% error). The method is applicable to the range of 0.2 to 700 ppM Ce

Estimation of the quantification uncertainty from flow injection and liquid chromatography transient signals in inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Laborda, Francisco; Medrano, Jesus; Castillo, Juan R.

2004-01-01

The quality of the quantitative results obtained from transient signals in high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICPMS) and flow injection-inductively coupled plasma mass spectrometry (FI-ICPMS) was investigated under multielement conditions. Quantification methods were based on multiple-point calibration by simple and weighted linear regression, and double-point calibration (measurement of the baseline and one standard). An uncertainty model, which includes the main sources of uncertainty from FI-ICPMS and HPLC-ICPMS (signal measurement, sample flow rate and injection volume), was developed to estimate peak area uncertainties and statistical weights used in weighted linear regression. The behaviour of the ICPMS instrument was characterized in order to be considered in the model, concluding that the instrument works as a concentration detector when it is used to monitorize transient signals from flow injection or chromatographic separations. Proper quantification by the three calibration methods was achieved when compared to reference materials, although the double-point calibration allowed to obtain results of the same quality as the multiple-point calibration, shortening the calibration time. Relative expanded uncertainties ranged from 10-20% for concentrations around the LOQ to 5% for concentrations higher than 100 times the LOQ

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.

Multi-elemental determination of trace elements in deep seawater by inductively coupled plasma mass spectrometry with resin preconcentration

International Nuclear Information System (INIS)

Sumida, Takashi; Nakazato, Tetsuya; Tao, Hiroaki

2003-01-01

A miniaturized column (ca. 3 mm i.d., 40 mm length), packed with a chelating resin (0.2 g) with iminodiacetic acid groups (Muromac A-1), was tested for the preconcentration of trace elements in seawater. After preconcentration, the column was washed with ammonium acetate buffer (pH 5.5) and water to remove the major elements, such as Ca and Mg, and was then eluted with 4 ml of 2 mol l -1 nitric acid. Twenty-six trace elements were determined by inductively coupled plasma mass spectrometry and inductively coupled plasma emission spectrometry. The necessary volume of the seawater sample was only 200 ml. The recoveries for most of the elements tested were over 90%, although those for Al, V and Th were around 70%. The trueness and precision were evaluated by analyzing a standard reference material of seawater (NASS-4, NRC Canada). The observed values obtained with the present method showed good agreement with the certified values. The present method was also applied to deep seawater samples collected at Muroto, Japan. A difference in the rare earth element pattern, especially the Ce anomaly, between the deep seawater sample and the surface seawater sample was observed, as well as the differences of the concentrations of many trace elements. (author)

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.

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...

Cadmium, copper, lead, and zinc determination in precipitation: A comparison of inductively coupled plasma atomic emission spectrometry and graphite furnace atomization atomic absorption spectrometry

Science.gov (United States)

Reddy, M.M.; Benefiel, M.A.; Claassen, H.C.

1987-01-01

Selected trace element analysis for cadmium, copper, lead, and zinc in precipitation samples by inductively coupled plasma atomic emission Spectrometry (ICP) and by atomic absorption spectrometry with graphite furnace atomization (AAGF) have been evaluated. This task was conducted in conjunction with a longterm study of precipitation chemistry at high altitude sites located in remote areas of the southwestern United States. Coefficients of variation and recovery values were determined for a standard reference water sample for all metals examined for both techniques. At concentration levels less than 10 micrograms per liter AAGF analyses exhibited better precision and accuracy than ICP. Both methods appear to offer the potential for cost-effective analysis of trace metal ions in precipitation. ?? 1987 Springer-Verlag.

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)

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)

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

Determination of rare earth elements in tomato plants by inductively coupled plasma mass spectrometry techniques.

Science.gov (United States)

Spalla, S; Baffi, C; Barbante, C; Turetta, C; Turretta, C; Cozzi, G; Beone, G M; Bettinelli, M

2009-10-30

In recent years identification of the geographical origin of food has grown more important as consumers have become interested in knowing the provenance of the food that they purchase and eat. Certification schemes and labels have thus been developed to protect consumers and genuine producers from the improper use of popular brand names or renowned geographical origins. As the tomato is one of the major components of what is considered to be the healthy Mediterranean diet, it is important to be able to determine the geographical origin of tomatoes and tomato-based products such as tomato sauce. The aim of this work is to develop an analytical method to determine rare earth elements (RRE) for the control of the geographic origin of tomatoes. The content of REE in tomato plant samples collected from an agricultural area in Piacenza, Italy, was determined, using four different digestion procedures with and without HF. Microwave dissolution with HNO3 + H2O2 proved to be the most suitable digestion procedure. Inductively coupled plasma quadrupole mass spectrometry (ICPQMS) and inductively coupled plasma sector field plasma mass spectrometry (ICPSFMS) instruments, both coupled with a desolvation system, were used to determine the REE in tomato plants in two different laboratories. A matched calibration curve method was used for the quantification of the analytes. The detection limits (MDLs) of the method ranged from 0.03 ng g(-1) for Ho, Tm, and Lu to 2 ng g(-1) for La and Ce. The precision, in terms of relative standard deviation on six replicates, was good, with values ranging, on average, from 6.0% for LREE (light rare earth elements) to 16.5% for HREE (heavy rare earth elements). These detection limits allowed the determination of the very low concentrations of REE present in tomato berries. For the concentrations of REE in tomato plants, the following trend was observed: roots > leaves > stems > berries. Copyright 2009 John Wiley & Sons, Ltd.

Direct rare earth determination by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Marin, Sergio; Cornejo, Silvia; Rojas, Jacqueline

2003-01-01

In the present work, the use of the inductively coupled plasma optical emission spectrometry (ICP-OES), for the sequential determination of Rare Earth elements in the metallurgical process samples is described. In the first place, the optimum parameters for the determination of the elements in study are established, like instrumental calibration, wavelengths spectral selection and interference of matrix. Next, the methodology for the digestion of solid samples (system of digestion with pressure) and the recovery of the interest elements are presented. Two material rocks as of reference Syenite SY3 are used. In order to assure the validity of the obtained data, the reference materials SY2 and SY3 were analyzed by means of two different techniques, ICP-OES and ICP-Mass, this last one was made by an international laboratory and a fusion with lithium metaborate was used with digestion method. Finally, the obtained results demonstrate that the reproducibility in the recovery of rare earth analyzed by both techniques is comparable, and that the methodology of digestion used for these elements is statistically valid (author)

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....

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...

Cobalamin speciation using reversed-phase micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Yanes, Enrique G.; Miller-Ihli, Nancy J.

2004-01-01

Micro-high-performance liquid chromatography interfaced to inductively coupled plasma mass spectrometry was optimized for the determination and separation of a mixture of cobalt containing species. Four cobalamin species (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5'-deoxyadenosylcobalamin) representing the various forms of vitamin B12 as well as the harmful corrinoid analogue cobinamide dicyanide were separated using reversed-phase microcapillary chromatography with columns containing C18 packing material with a 2-μm particle size. Selection of organic solvents for the separation took into consideration compatibility with the inductively coupled plasma mass spectrometer being used for element specific detection. Optimized method conditions included use of a methanol gradient and make-up solution for the nebulizer. Some issues associated with dead volume were overcome by the extension of the gradient program. The total analysis time was 52 min. The column-to-column variability was evaluated and was found to be very reasonable (9% RSD on average), confirming that this method is rugged and that the technology should be easily transferred to other laboratories

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

Using inductively coupled plasma-mass spectrometry for calibration transfer between environmental CRMs.

Science.gov (United States)

Turk, G C; Yu, L L; Salit, M L; Guthrie, W F

2001-06-01

Multielement analyses of environmental reference materials have been performed using existing certified reference materials (CRMs) as calibration standards for inductively coupled plasma-mass spectrometry. The analyses have been performed using a high-performance methodology that results in comparison measurement uncertainties that are significantly less than the uncertainties of the certified values of the calibration CRM. Consequently, the determined values have uncertainties that are very nearly equivalent to the uncertainties of the calibration CRM. Several uses of this calibration transfer are proposed, including, re-certification measurements of replacement CRMs, establishing traceability of one CRM to another, and demonstrating the equivalence of two CRMs. RM 8704, a river sediment, was analyzed using SRM 2704, Buffalo River Sediment, as the calibration standard. SRM 1632c, Trace Elements in Bituminous Coal, which is a replacement for SRM 1632b, was analyzed using SRM 1632b as the standard. SRM 1635, Trace Elements in Subbituminous Coal, was also analyzed using SRM 1632b as the standard.

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)

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...

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

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

Uranium quantification in semen by inductively coupled plasma mass spectrometry

Science.gov (United States)

Todorov, Todor I.; Ejnik, John W.; Guandalini, Gustavo S.; Xu, Hanna; Hoover, Dennis; Anderson, Larry W.; Squibb, Katherine; McDiarmid, Melissa A.; Centeno, Jose A.

2013-01-01

In this study we report uranium analysis for human semen samples. Uranium quantification was performed by inductively coupled plasma mass spectrometry. No additives, such as chymotrypsin or bovine serum albumin, were used for semen liquefaction, as they showed significant uranium content. For method validation we spiked 2 g aliquots of pooled control semen at three different levels of uranium: low at 5 pg/g, medium at 50 pg/g, and high at 1000 pg/g. The detection limit was determined to be 0.8 pg/g uranium in human semen. The data reproduced within 1.4–7% RSD and spike recoveries were 97–100%. The uranium level of the unspiked, pooled control semen was 2.9 pg/g of semen (n = 10). In addition six semen samples from a cohort of Veterans exposed to depleted uranium (DU) in the 1991 Gulf War were analyzed with no knowledge of their exposure history. Uranium levels in the Veterans’ semen samples ranged from undetectable (<0.8 pg/g) to 3350 pg/g. This wide concentration range for uranium in semen is consistent with known differences in current DU body burdens in these individuals, some of whom have retained embedded DU fragments.

Direct determination of the samarium:neodymium ratio in geological materials by inductively coupled plasma quadrupole mass spectrometry with cryogenic desolvation. Comparison with isotope dilution thermal ionization mass spectrometry

International Nuclear Information System (INIS)

Pin, Christian; Telouk, Philippe; Imbert, J.-L.

1995-01-01

A cryogenic desolvation unit in the sample introduction system reduces differences in oxide formation between Sm and Nd to very low levels, enabling the direct, standardless determination of their ratio in bulk solutions by inductively coupled plasma mass spectrometry. The measured values are in reasonably good agreement with those determined by the isotope dilution thermal ionization mass spectrometry (ID-TIMS) reference technique. Although this method cannot, at present, compete with ID-TIMS in terms of precision and accuracy, it is much more straightforward and can be used in geochemistry for studies involving the screening of a large number of samples. (author)

Effect of Skimmer Cone Material on the Spectra of Inductively Coupled Plasma Mass Spectrometry

International Nuclear Information System (INIS)

Amr, M.A.; Zahran, N.F.; Helal, A.I.

2002-01-01

The inductively coupled plasma ion source for mass spectrometry is very sensitive for multielement analysis with detection limits down to sub part per trillion (ppt). Polyatomic ions which could be formed in the mass spectra may interfere in the analysis of some element. Experimental conditions have great influences on the formation of polyatomic ions. The present work demonstrates that the skimmer materials (Au, Ag, Ni, and Cu) are participating in the formation of polyatomic ions, meanwhile the sampler materials have no real effect. The mechanism of formation of polyatomic ions is explained. Heats of formation of polyatomic species formed from the skimmer materials such as: Au X, Ag X, Ni X and Cu X; where X= Ar, O, N, C and H are calculated by Gaussian program (G 94 W)

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...

Direct analysis of samples by mass spectrometry: From elements to bio-molecules using laser ablation inductively couple plasma mass spectrometry and laser desorption/ionization mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Perdian, David C. [Iowa State Univ., Ames, IA (United States)

2009-01-01

Mass spectrometric methods that are able to analyze solid samples or biological materials with little or no sample preparation are invaluable to science as well as society. Fundamental research that has discovered experimental and instrumental parameters that inhibit fractionation effects that occur during the quantification of elemental species in solid samples by laser ablation inductively coupled plasma mass spectrometry is described. Research that determines the effectiveness of novel laser desorption/ionization mass spectrometric methods for the molecular analysis of biological tissues at atmospheric pressure and at high spatial resolution is also described. A spatial resolution is achieved that is able to analyze samples at the single cell level.

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

Physicochemical characterization of titanium dioxide pigments using various techniques for size determination and asymmetric flow field flow fractionation hyphenated with inductively coupled plasma mass spectrometry

NARCIS (Netherlands)

Helsper, J.P.F.G.; Peters, R.J.B.; Bemmel, M.E.M. van; Rivera, Z.E.H.; Wagner, S.; Kammer, F. von der; Tromp, P.C.; Hofmann, T.; Weigel, S.

2016-01-01

Seven commercial titanium dioxide pigments and two other well-defined TiO2 materials (TiMs) were physicochemically characterised using asymmetric flow field flow fractionation (aF4) for separation, various techniques to determine size distribution and inductively coupled plasma mass spectrometry

Sulphate analysis in uranium leach iron(III) chloride solutions by inductively coupled argon plasma spectrometry

International Nuclear Information System (INIS)

Nirdosh, I.; Lakhani, S.; Yunus, M.Z.M.

1993-01-01

Inductively coupled Argon Plasma Spectrometry is used for the indirect determination of sulphate in iron(III) chloride leach solution of Elliot Lake uranium ores via addition of a known amount of barium ions and analyzing for excess of barium. The ore contains ∼ 7 wt% pyrite, FeS 2 , as the major mineral which oxidizes to generate sulphate during leaching with Fe(III). The effects of pH, the concentrations of Fe(III) and chloride ions and for presence of ethanol in the test samples on the accuracy of analysis are studied. It is found that unlike the Rhodizonate method, removal of iron(III) from or addition of ethanol to the test sample prior to analysis are not required. Linear calibration curves are obtained. (author)

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.

[Determination of 24 minerals in human milk by inductively coupled plasma mass spectrometry with microwave digestion].

Science.gov (United States)

Sun, Zhongqing; Yue, Bing; Yang, Zhenyu; Li, Xiaowei; Wu, Yongning; Yin, Shian

2013-05-01

To determine the levels of 24 minerals in human milk by inductively coupled plasma mass spectrometry with microwave digestion. The samples were digested by microwave. The contents of minerals were determined by inductively coupled plasma mass spectrometry. The standard reference minerals of 1849a and 1568a from National Institute of Science and Technology were used for quality control. The accuracy and reproduability for this method were evaluated with mix standards and 1849a and 1568a standard reference materials. The ranges of the levels of sodium, magnesium, phosphorus, potassium, calcium, aluminum, chromium, arsenic, selenium, iron, zinc, manganese, copper, molybdenum, vanadium, cobalt, nickel, gallium, cadmium, silver, strontium, cesium, barium, lead in human milk was 34.97-415.83 mg/kg, 19.00-39.52 mg/kg, 102.13-274.53 mg/kg, 351.19-713.99 mg/kg, 180.08-349.64 mg/kg, 0.06-0.44 mg/kg, 0.9-7.37 microg/kg, 0.92-2.72 microg/kg, 0.20-21.15 microg/kg, 0.10-0.70 mg/kg, 0.56-3.25 mg/kg, 3.00-16.12 micro.g/kg, 62.16-591.69 microg/kg, 0.02-6.91 microg/kg, 5.99-13.70 microg/kg, 0.07-2.11 microg/kg, 0.77-209.26 microg/kg, 0.005-0.28 microg/kg, 0.02-0.23 microg/kg, 0.02-0.71 microg/kg, 36.89-132.26 microg/kg, 0.01-4.72 microg/kg, 0.83-28.16 microg/kg, 2.5-5.3 microg/kg, respectively. The levels of minerals in human milk in present study were consisted with other similar studies. The experiment examined the levels of minerals in human milk satisfactorily. The method has high accuracy and good reproducibility, which could be used for understanding the levels of minerals in human milk.

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)

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...

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…

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.

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

Determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Yoshida, K.; Haraguchi, H.

1984-01-01

Inductively coupled plasma atomic emission spectrometry (ICP-AES) interfaced with high-performance liquid chromatography (HPLC) has been applied to the determination of rare earth elements. ICP-AES was used as an element-selective detector for HPLC. The separation of rare earth elements with HPLC helped to avoid erroneous analytical results due to spectral interferences. Fifteen rare earth elements (Y and 14 lanthanides) were determined selectively with the HPLC/ICP-AES system using a concentration gradient method. The detection limits with the present HPLC/ICP-AES system were about 0.001-0.3 μg/mL with a 100-μL sample injection. The calibration curves obtained by the peak height measurements showed linear relationships in the concentration range below 500 μg/mL for all rare earth elements. A USGS rock standard sample, rare earth ores, and high-purity lanthanide reagents (>99.9%) were successfully analyzed without spectral interferences

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

Radiochemical determination of zirconium by inductively coupled plasma mass spectrometry (ICPMS)

International Nuclear Information System (INIS)

Oliveira, Thiago C.; Oliveira, Arno Heeren de

2013-01-01

The zirconium isotope 93 Zr is a long-lived pure β-particle-emitting radionuclide thus occurring as one of the radionuclides found in nuclear reactors. It's produced from 235 U fission and from 92 Zr neutron activation. Due to its long half-life, 93 Zr is one of the interest radionuclides for assessment studies performance 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 apply a selective radiochemical separation methodology for 93 Zr determination in nuclear waste and analyze it by Inductively Coupled Plasma Mass Spectrometry (ICPMS). To set up the zirconium radiochemical separation procedure, a zirconium tracer solution was used in order to follow the zirconium behavior during the radiochemical separation. A tracer solution containing the main interferences, Ba, Co, Eu, Fe, Mn, Nb, Ni, Sr, and Y was used in order to verify the decontamination factor during separation process. The limit of detection of 0,039 ppb was obtained for zirconium standard solutions by ICPMS. Then, the protocol will be applied to low level waste (LLW) and intermediate level waste (ILW) from nuclear power plants. (author)

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

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

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.

Inductively coupled plasma optical emission spectrometry analysis of lanthanum, samarium and gadolinium oxides for rare earths impurities

International Nuclear Information System (INIS)

Reino, L.C.P.; Lordello, A.R.

1990-09-01

An inductively coupled plasma optical emission spectrometry method is described for the determination of Sm, Eu, La, Gd, Dy, Pr, Ho, Nd, Tb and Y in purified oxides of lanthanum, samarium and gadolinium. The method enables a simple, precise and readily available determination. Dissolution of the samples is achieved with diluted hydrochloric acid (1:1). The solutions are diluted to volume for a concentration of 1mg/ml. The lowest determination limit is 0,01% for most elements and 0,05 or 0,1% for a few rare earths in samarium and gadolinium matrices. Lanthanum, Samarium and Gadolinium concentrates with purity grade of 99,9%, 99,6% and 99,8%, respectively, can be analysed by this procedure. (author)

Multielement determination of rare earth elements by liquid chromatography/inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Sawatari, Hideyuki; Asano, Takaaki; Hu, Xincheng; Saizuka, Tomoo; Itoh, Akihide; Hirose, Akio; Haraguchi, Hiroki

1995-01-01

The rapid determination of rare earth elements (REEs) has been investigated by an on-line system of high performance liquid chromatography/multichannel inductively coupled plasma atomic emission spectrometry. In the present system, all REEs could be detected simultaneously in a single chromatographic measurement without spectral interferences. Utilizing a cation exchange column and 2-hydroxy-2-methylpropanoic acid aqueous solution as the mobile phase, the detection limits of 0.4-30 ng ml -1 for all REEs were obtained. The system was applied to the determination of REEs in geological standard rock samples and rare earth impurities in high purity rare earth oxides. The REEs in standard rocks could be determined by the present HPLC/ICP-AES system without pretreatment after acid digestion, although the detection limits were not sufficient for the analysis of rare earth oxides. (author)

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).

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

Methods for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry

Science.gov (United States)

Chan, George C. Y. [Bloomington, IN; Hieftje, Gary M [Bloomington, IN

2010-08-03

A method for detecting and correcting inaccurate results in inductively coupled plasma-atomic emission spectrometry (ICP-AES). ICP-AES analysis is performed across a plurality of selected locations in the plasma on an unknown sample, collecting the light intensity at one or more selected wavelengths of one or more sought-for analytes, creating a first dataset. The first dataset is then calibrated with a calibration dataset creating a calibrated first dataset curve. If the calibrated first dataset curve has a variability along the location within the plasma for a selected wavelength, errors are present. Plasma-related errors are then corrected by diluting the unknown sample and performing the same ICP-AES analysis on the diluted unknown sample creating a calibrated second dataset curve (accounting for the dilution) for the one or more sought-for analytes. The cross-over point of the calibrated dataset curves yields the corrected value (free from plasma related errors) for each sought-for analyte.

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

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.)

Accuracy and Precision in Elemental Analysis of Environmental Samples using Inductively Coupled Plasma-Atomic Emission Spectrometry

International Nuclear Information System (INIS)

Quraishi, Shamsad Begum; Chung, Yong-Sam; Choi, Kwang Soon

2005-01-01

Inductively Coupled Plasma-Atomic Emission Spectrometry followed by micro-wave digestion have been performed on different environmental Certified Reference Materials (CRMs). Analytical results show that accuracy and precision in ICP-AES analysis were acceptable and satisfactory in case of soil and hair CRM samples. The relative error of most of the elements in these two CRMs is within 10% with few exceptions and coefficient of variation is also less than 10%. Z-score as an analytical performance was also within the acceptable range (±2). ICP-AES was found as an inadequate method for Air Filter CRM due to incomplete dissolution, low concentration of elements and very low mass of the sample. However, real air filter sample could have been analyzed with high accuracy and precision by increasing sample mass during collection. (author)

[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.

Tin Content Determination in Canned Fruits and Vegetables by Hydride Generation Inductively Coupled Plasma Optical Emission Spectrometry

Directory of Open Access Journals (Sweden)

Sanda Rončević

2012-01-01

Full Text Available Tin content in samples of canned fruits and vegetables was determined by hydride generation inductively coupled plasma atomic emission spectrometry (HG-ICP-OES, and it was compared with results obtained by standard method of flame atomic absorption spectrometry (AAS. Selected tin emission lines intensity was measured in prepared samples after addition of tartaric acid and followed by hydride generation with sodium borohydride solution. The most favorable line at 189.991 nm showed the best detection limit (1.9 μg L−1 and limit of quantification (6.4 μg kg−1. Good linearity and sensitivity were established from time resolved analysis and calibration tests. Analytical accuracy of 98–102% was obtained by recovery study of spiked samples. Method of standard addition was applied for tin determination in samples from fully protected tinplate. Tin presence at low-concentration range was successfully determined. It was shown that tenth times less concentrations of Sn were present in protected cans than in nonprotected or partially protected tinplate.

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.

Ultra-sensitive quantification of lysozyme based on element chelate labeling and capillary electrophoresis–inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Yang, MingWei; Wu, WeiHua; Ruan, YaJuan; Huang, LiMei; Wu, Zujian; Cai, Yong; Fu, FengFu

2014-01-01

Graphical abstract: An ultra-sensitive method for the determination of lysozyme was developed based on the Gd 3+ chelate labeling and CE–ICP–MS. The proposed method has an extremely low detection limit of 3.89 attomole and has been successfully used to detect lysozyme in saliva sample, showing excellent reliability. The success of the present method provides a new possibility for biological assays and clinical diagnoses. -- Highlights: •An ultra-sensitive method for detecting lysozyme based on CE–ICP–MS was described. •The proposed method has an extremely low detection limit of 3.89 attomole. •It can be used to detect trace lysozyme in saliva sample with a satisfied recovery. •The method provides a new potential for sensitive detection of low-abundant proteins. -- Abstract: In this study, an ultra-sensitive method for the quantification of lysozyme based on the Gd 3+ diethylenetriamine-N,N,N′,N″,N″-pentaacetic acid labeling and capillary electrophoresis–inductively coupled plasma mass spectrometry (CE–ICP–MS) was described. The Gd 3+ -tagged lysozyme was effectively separated by capillary electrophoresis (CE) and sensitively determined by inductively coupled plasma mass spectrometry (ICP–MS). Based on the gadolinium-tagging and CE–ICP–MS, the lysozyme was determined within 12 min with an extremely low detection limit of 3.89 attomole (3.89 × 10 −11 mol L −1 for 100 nL of sample injection) and a RSD < 6% (n = 5). The proposed method has been successfully used to detect lysozyme in saliva samples with a recovery of 91–106%, suggesting that our method is sensitive and reliable. The success of the present method provides a new potential for the biological assays and sensitive detection of low-abundant proteins

Arsenic speciation by liquid chromatography coupled with ionspray tandem mass spectrometry

DEFF Research Database (Denmark)

Corr, J. J.; Larsen, Erik Huusfeldt

1996-01-01

Ionspray mass spectrometry, a well established organic analysis technique, has been coupled to high-performance liquid chromatography for speciation of organic arsenic compounds, The ionspray source and differentially pumped interface of the mass spectrometer were operated in dual modes...... fragmentation patterns showing molecular dissociation through an expected common product ion were obtained for the four arsenosugars, Molecular mode detection was utilized for qualitative verification of speciation analysis by high-performance liquid chromatography coupled to inductively coupled plasma mass...

Direct determination of trace rare earth elements in ancient porcelain samples with slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Xiang Guoqiang; Jiang Zucheng; He Man; Hu Bin

2005-01-01

A method for the direct determination of trace rare earth elements in ancient porcelain samples by slurry sampling fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry was developed with the use of polytetrafluoroethylene as fluorinating reagent. It was found that Si, as a main matrix element in ancient porcelain sample, could be mostly removed at the ashing temperature of 1200 deg. C without considerable losses of the analytes. However, the chemical composition of ancient porcelain sample is very complicated, which makes the influences resulting from other matrix elements not be ignored. Therefore, the matrix effect of ancient porcelain sample was also investigated, and it was found that the matrix effect is obvious when the matrix concentration was larger than 0.8 g l -1 . The study results of particle size effect indicated that when the sample particle size was less than 0.057 mm, the particle size effect is negligible. Under the optimized operation conditions, the detection limits for rare earth elements by fluorinating electrothermal vaporization inductively coupled plasma mass spectrometry were 0.7 ng g -1 (Eu)-33.3 ng g -1 (Nd) with the precisions of 4.1% (Yb)-10% (La) (c = 1 μg l -1 , n = 9). The proposed method was used to directly determine the trace rare earth elements in ancient porcelain samples produced in different dynasty (Sui, Ming and Qing), and the analytical results are satisfactory

[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.

Determination of Micro minerals in Milk from Farm and Pasture-reared Cow, Goat and Camel; using Inductively Coupled Plasma-Optical Emission Spectrometry

OpenAIRE

SirelkhatimBalla Elhardallou; Ashraf Yehia El-naggar

2016-01-01

This study covers raw fresh milk of cow, goat and camel (farm and pasture-reared),in addition to two brands of commercial milk samples, liquid milk of powder origin and drinking yoghurt samples. Camel milk showed a relatively lower pH range (6.15 - 6.46) compared cow, goat and commercial milk. The pH of drinking yoghurt was found (4.35 - 4.47).Microwave digestion, was selected followed by mineral analysis using Inductively Coupled Plasma-Optical Emission Spectrometry. Micro minerals; Cd, Cr...

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.

Semi-automatic determination of tin in marine materials by continuous flow hydride generation inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Feng Yonglai; Narasaki, Hisataki; Chen Hongyuan; Tian Liching

1997-01-01

A semi-automated continuous flow hydride generation system with inductively coupled plasma atomic emission spectrometry (ICP-AES) was used for the determination of tin in marine materials. The effects of acids (H 2 SO 4 and HCl) were studied. The analytical parameters were thoroughly investigated. Under optimized conditions, the detection limit is 0.4 ng/ml. Interferences from transition elements were investigated and seven masking reagents were tested. L-cysteine hydrochloride monohydrate (1%) was used to mask the interferences from foreign ions. Finally, the accuracy, checked with a marine standard reference material obtained from the National Research Council (NRC), was within the certified value. (orig.). With 6 figs., 4 tabs

Determination of 238U in marine organisms by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Ishii, Toshiaki; Nakahara, Motokazu; Matsuba, Mitsue; Ishikawa, Masafumi

1991-01-01

Determination of 238 U in fifty-five species of marine organisms was carried out by inductively coupled plasma mass spectrometry which showed some advantages such as high sensitivity, wide dynamic range and small interferences from matrices for the analysis of high mass elements. The concentrations of 238 U in soft tissues of marine animals ranged from 0.076 to 5000 ng/g wet wt. Especially, the branchial heart of cephalopod molluscs showed the specific accumulation of 238 U. The concentration factor of the branchial heart of Octopus vulgaris, which indicated the highest value, was calculated to be about 10 3 by comparing it with the concentration of 238 U (3.2±0.2 ng/ml) in coastal seawaters of Japan. The concentrations of 238 U in hard tissues of marine invertebrates were similar to those in soft tissues. In contrast, hard tissues like bone, scale, fin, etc. of fishes showed much higher concentrations of 238 U than soft tissues like muscle and liver. The concentrations of 238 U of twenty species of algae ranged from 10 to 3700 ng/g dry wt. (author)

High-precision lead isotope ratio measurement by inductively coupled plasma multiple collector mass spectrometry

International Nuclear Information System (INIS)

Walder, A.J.; Furuta, Naoki.

1993-01-01

An inductively coupled plasma (ICP) ion source coupled to a magnetic sector mass analyser equipped with seven Faraday detectors has been used to measure the lead isotope ratios in solutions of Sanshiro Pond sediment collected at the University of Tokyo, airborne particulates collected at Shinjuku in Tokyo and Merck multielement standard product number 97279494. A thallium correction technique was utilized to allow a simultaneous correction for mass bias. This work followed an earlier interlaboratory comparison study of the above-mentioned solutions using ICP quadrupole mass spectrometry, and has demonstrated a considerable improvement in analytical precision. The following isotope ratio measurements were recorded. Pond sediment solution containing 82 ng ml -1 lead: 206 Pb/ 204 Pb=17.762±0.014; 206 Pb/ 207 Pb=1.1424±0.0009; 208 Pb/ 204 Pb=37.678±0.034. Airborne particulate solution containing 45 ng ml -1 lead: 206 Pb/ 204 Pb=17.969±0.006; 206 Pb/ 207 Pb=1.1528±0.0003; 208 Pb/ 204 Pb=37.915±0.021. Merck multielement standard solution containing 100 ng ml -1 lead: 206 Pb/ 204 Pb=19.255±0.015; 206 Pb/ 207 Pb=1.2238±0.0004; 208 Pb/ 204 Pb=38.476±0.021 (All errors are given as ±2 standard deviations). (author)

Use of magnesium as a test element for inductively coupled plasma atomic emission spectrometry diagnosis

International Nuclear Information System (INIS)

Mermet, J.M.

1991-01-01

To optimize atomization and ionization processes in an inductively coupled plasma used as a source in atomic emission spectrometry, the Mg II 280.270-nm/Mg I 285-213-nm line intensity ratio is used. A theoretic ratio is calculated assuming a local thermodynamic equilibrium.A review of previously published experimental values of the ratio is given as a function of the parameters influencing the energy transfer between the plasma and injected species. In particular, the effects of the power, the carrier gas flow-rate, the i.d. of the torch injector, the use of a sheathing gas and the presence of hydrogen are described. Values of the ratio close to the theoretical values are obtained with a high power (>1.4 kW), a lower carrier gas flow-rate ( -1 ) and a large i.d. of the injector (>2 mm). This optimization can also be applied to the minimization of interference effects due to the presence of sodium. (author). 64 refs.; 9 figs.; 1 tab

[Determination of arsenic speciation in Scomberomorus niphonius by capillary electrophoresis-inductively coupled plasma mass spectrometry].

Science.gov (United States)

Chen, Fa-rong; Zheng, Li; Wang, Zhi-Guang; Sun, Jie; Han, Li-Hui; Wang, Xiao-ru

2014-06-01

A method for the detection of arsenocholine (AsC), arsenobetaine (AsB), As(III), dimethylarsinic (DMA), monomethylarsonic (MMA) and As (V) by capillary electrophoresis-inductively coupled plasma mass spectrometry (CE-ICP-MS) was established. The results showed that the six species of arsenic were separated within 20 min under the optimized conditions. Good linearities of 6 arsenic species were observed in the range from 2 to 50 μg x L(-1) with the linear correlation greater than 0.996, the detection limits were 0.10-1.08 μg x L(-1) and the RSDs (n = 5) of the peak areas were smaller than 7%. The method was successfully adopted to the determination of the species in Scomberomorus niphonius. The recoveries were between 93% and 98%, and we found the arsenobetaine (AsB) was the main species in the sample. The method was suitable for the analysis of other biological samples with the advantages of good stability, less sample consumption, short analysis time and convenience.

Urinary elimination of molybdenum by healthy subjects as determined by inductively coupled plasma mass spectrometry.

Science.gov (United States)

Allain, P; Berre, S; Prémel-Cabic, A; Mauras, Y; Cledes, A; Cournot, A

The concentration of molybdenum was measured by inductively coupled plasma mass spectrometry (ICPMS) in the urines of two groups of healthy people living in two areas of France, Brest and Paris, about 500 km away. The concentration of Mo in the 24-hour urines of 10 healthy subjects from the Brest region was 25 +/- 10 micrograms/l, 38 +/- 20 micrograms/24 h and 21 +/- 9 micrograms/g creatinine. The concentration of Mo in the morning urines of 23 healthy men of the Paris region was 41 +/- 34 micrograms/l and 21 +/- 15 micrograms/g creatinine. Thus the mean elimination of Mo per gram of creatinine was the same in the two groups (21 +/- 9 and 21 +/- 15). Since the three main isotopes of Mo m/z = 95, 96 and 98, corresponding to an abundance percentage of 16, 17 and 24.5, respectively, were simultaneously analyzed in each sample and led to similar results, the ICPMS method seems reliable.

Urinary nickel: measurement of exposure by inductively coupled plasma argon emission spectrometry.

Science.gov (United States)

Koizumi, Chisato; Usuda, Kan; Hayashi, Satsuki; Dote, Tomotaro; Kono, Koichi

2004-09-01

Nickel is a rare earth metal and is widely used in modern industry. Its overexposure in human beings can provoke significant effects including lung, cardiovascular and kidney diseases. As an index of occupational exposure, urine is widely used for the monitoring of nickel concentration because it is a minimally invasive method. Recent studies have used atomic absorption spectrometry to measure nickel concentration. In this study, we introduced novel inductively coupled plasma argon emission spectrometry (ICPAES) which enables us to measure multiple elements simultaneously with smaller volume and with lower detection limits compared to conventional atomic absorption emission spectrometry, and we established the new measuring method by determining the appropriate wavelengths for nickel concentration. Furthermore, using the established new measuring method, we investigated the correlation between a single oral administration of nickel and urine elimination in rats. As a result, different concentrations of nickel standard solutions were measured by ICPAES, and among five specific wavelengths of nickel, 221.647 and 231.604 nm were chosen because they had the highest inclines of both signal to background ratio and emission intensity in simple linear regression analysis. Next, by using healthy human urine samples that had not been exposed to nickel, 231.604 nm was determined to be the most appropriate wavelength because it did not present abnormal intensity due to obstacle wavelength. Male Wistar rats received an oral administration of nickel ranging from 0.025 to 250 mg/kg, which is equivalent to 0.0015 - 15% of LD50, and during the following 24 h, urine samples were collected and the nickel concentration was measured by ICPAES. With a single oral administration of nickel, there was an increase in urine nickel concentration in a dose-dependent manner and the appropriate equation was developed. Acute renal failure was not observed in this dosage of oral nickel

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.

Inductively coupled plasma--atomic emission spectrometry: trace elements in oil matrices

Energy Technology Data Exchange (ETDEWEB)

Peterson, Charlie Albert [Iowa State Univ., Ames, IA (United States)

1977-12-01

The simultaneous determination of up to 20 trace elements in various oil matrices by inductively coupled plasma-atomic emission spectrometry is reported. The oil matrices investigated were lubricating oils (for wear metals), fuel oil, centrifuged coal liquefaction product, crude soybean oil, and commercial edible oils. The samples were diluted with appropriate organic solvents and injected into the plasma as an aerosol generated by a pneumatic nebulization technique. Detection limits of the 28 elements studied ranged from 0.0006 to 9 μg/g with the majority falling in the 0.01 to 0.1 μg/g range. Analytical calibration curves were linear over at least two orders of magnitude and for some elements this linearity extended over 4.5 orders of magnitude. Relevant data on precision and accuracy are included. Because metals often occur as particles in lubricating oil and coal liquefaction products, the effect of particles on the analytical results was examined. Wear metal particles in used oil did not appear to affect the analytical results. However, incomplete recovery relative to organometallic reference solutions was obtained for iron particles with a nominal mean diameter of 3.0 μm suspended in oil. It was shown that the following factors contributed to incomplete recovery for the particles: settling of the suspended particles in the flask, a difference in nebulization efficiency between particle suspensions and organometallic solutions, and indications of incomplete vaporization of the larger particles in the plasma.

Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

International Nuclear Information System (INIS)

Papadopoulou, D.N.; Zachariadis, G.A.; Anthemidis, A.N.; Tsirliganis, N.C.; Stratis, J.A.

2004-01-01

Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level)

Comparison of a portable micro-X-ray fluorescence spectrometry with inductively coupled plasma atomic emission spectrometry for the ancient ceramics analysis

Energy Technology Data Exchange (ETDEWEB)

Papadopoulou, D.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Zachariadis, G.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Anthemidis, A.N. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece); Tsirliganis, N.C. [Archaeometry Laboratory, Cultural and Educational Technology Institute, Tsimiski 58, GR-67100, Xanthi (Greece); Stratis, J.A. [Laboratory of Analytical Chemistry, Faculty of Chemistry, Aristotle University, GR-54124, Thessaloniki (Greece)]. E-mail: jstratis@chem.auth.gr

2004-12-01

Two multielement instrumental methods of analysis, micro X-ray fluorescence spectrometry (micro-XRF) and inductively coupled plasma atomic emission spectrometry (ICP-AES) were applied for the analysis of 7th and 5th century B.C. ancient ceramic sherds in order to evaluate the above two methods and to assess the potential to use the current compact and portable micro-XRF instrument for the in situ analysis of ancient ceramics. The distinguishing factor of interest is that micro-XRF spectrometry offers the possibility of a nondestructive analysis, an aspect of primary importance in the compositional analysis of cultural objects. Micro-XRF measurements were performed firstly directly on the ceramic sherds with no special pretreatment apart from surface cleaning (micro-XRF on sherds) and secondly on pressed pellet disks which were prepared for each ceramic sherd (micro-XRF on pellet). For the ICP-AES determination of elements, test solutions were prepared by the application of a microwave-assisted decomposition procedure in closed high-pressure PFA vessels. Also, the standard reference material SARM 69 was used for the efficiency calibration of the micro-XRF instrument and was analysed by both methods. In order to verify the calibration, the standard reference materials NCS DC 73332 and SRM620 as well as the reference materials AWI-1 and PRI-1 were analysed by micro-XRF. Elemental concentrations determined by the three analytical procedures (ICP-AES, micro-XRF on sherds and micro-XRF on pellets) were statistically treated by correlation analysis and Student's t-test (at the 95% confidence level)

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.

Multiplexed microRNA detection using lanthanide-labeled DNA probes and laser ablation inductively coupled plasma mass spectrometry

DEFF Research Database (Denmark)

de Bang, Thomas Christian; Shah, Pratik; Cho, Seok Keun

2014-01-01

coupled plasma mass spectrometry (LA-ICPMS). Three miRNAs from Arabidopsis thaliana were analyzed simultaneously with high specificity, and the sensitivity of the method was comparable to radioactive detection (low femtomol range). The perspective of the developed method is highly multiplexed......In the past decade, microRNAs (miRNAs) have drawn increasing attention due to their role in regulation of gene expression. Especially, their potential as biomarkers in disease diagnostics has motivated miRNA research, including the development of simple, accurate, and sensitive detection methods....... The narrow size range of miRNAs (20-24 nucleotides) combined with the chemical properties of conventional reporter tags has hampered the development of multiplexed miRNA assays. In this study, we have used lanthanide-labeled DNA probes for the detection of miRNAs on membranes using laser ablation inductively...

Mass spectrometric evidence for suprathermal ionization in an inductively coupled argon plasma

International Nuclear Information System (INIS)

Houk, R.S.; Svec, H.J.; Fassel, V.A.

1981-01-01

Mass spectra have been obtained of species in the axial channel of an inductively coupled argon plasma by extracting ions from the inductively coupled plasma into a vacuum system housing a quadrupole mass spectrometer. Ionization temperatures (T/sub ion/) are obtained from relative count rates of m/z-resolved ions according to two general types of ionization equilibrium considerations: (a) the radio of doubly/singly charged ions of the same element, and (b) the ratio of singly charged ions from two elements of different ionization energy. The T/sub ion/ values derived from measurement of Ar +2 /Ar + , Ba +2 /Ba + , Sr +2 /Sr + , and Cd + /I + are all greater than those expected from excitation temperatures measured by other workers. The latter three values for T/sub ion/ are in reasonable agreement with values obtained by optical spectrometry for a variety of argon inductively coupled plasmas

Determination of antimony compounds in waters and juices using ion chromatography-inductively coupled plasma mass spectrometry.

Science.gov (United States)

Lin, Ya-An; Jiang, Shiuh-Jen; Sahayam, A C

2017-09-01

A method was developed by coupling ion chromatography (IC) and inductively coupled plasma mass spectrometry (ICP-MS) for the speciation of antimony. In this study, antimony species such as antimonite [Sb(III)], antimonate [Sb(V)] and trimethyl antimony(V) (TMeSb) were separated in less than 8min using anion exchange chromatography with a Hamilton PRP-X100 column as the stationary phase. Mobile phase A was 20mmolL -1 ethylenediaminetetraacetic acid (EDTA), 2mmolL -1 potassium hydrogen phthalate (KHP) in 1% v/v methanol (pH 5.5) and 20mmolL -1 EDTA, 2mmolL -1 KHP, 40mmolL -1 (NH 4 ) 2 CO 3 in 1% v/v methanol (pH 9.0) formed mobile phase B. Detection limits and relative standard deviations (RSD) were 0.012-0.032ngmL -1 and 2.2-2.8% respectively. This method was applied to bottled waters and fruit juices purchased in Kaohsiung, Taiwan. In water samples, Sb(V) was the major species where as in juices organometallic Sb species were also present. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

Online Determination of Sm, Eu and Yb in Environmental Samples by Inductively Coupled Plasma – Optical Emission Spectrometry

Directory of Open Access Journals (Sweden)

J. Dilip Kumar

2007-01-01

Full Text Available A procedure was developed for the determination of Sm, Eu and Yb in water samples by inductively coupled plasma-optical emission spectrometry (ICP-OES after preconcentration on synthesized 5-(4-pyridyl azo-8-quinolinol supported by Borassus flabellifer inflorescence (BFI. The sorbed element was subsequently eluted with 0.4 M HNO3 and the acid eluates were analyzed by ICP-OES. Under the optimal conditions, Sm, Eu and Yb in aqueous samples were concentrated 100-fold. Recoveries were obtained by the proposed method in the range of 98.6 -99.8%. This method was also applied for the analysis of spiked and natural water samples. The results provide strong evidence to support the hypothesis of an adsorption mechanism.

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)

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

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

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.

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

Determination of selenite and selenate in human urine by ion chromatography and inductively coupled plasma mass spectrometry

DEFF Research Database (Denmark)

Gammelgaard, Bente; Jons, O.

2000-01-01

The selenium species selenite, selenate and selenomethionine were separated in aqueous solution by ion chromatography. The separation was performed on an IonPac AG11 in series with an AS11 anion exchange column by elution with 25 mM sodium hydroxide in 2% methanol. The Se-78 and Se-82 isotopes were...... monitored in the inductively coupled plasma mass spectrometry (ICP-MS) detector. When the chromatographic system was applied to analysis of urine samples diluted 1 + 1, the selenomethionine signal appeared in the front together with other unresolved selenium species, while the selenite and selenate signals...... and selenate, respectively, corresponding to absolute amounts of 8 and 16 pg, respectively. Calculations were based on peak height measurements of the Se-82 isotope. In 23 analysed urine samples, the concentration of selenite was in the range selenium...

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.

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.

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

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.

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.

Accurate determination of silver nanoparticles in animal tissues by inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Veverková, Lenka [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Hradilová, Šárka [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Milde, David, E-mail: david.mlde@upol.cz [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Panáček, Aleš [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Skopalová, Jana [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Kvítek, Libor [Regional Centre of Advanced Technologies and Materials, Department of Physical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); Petrželová, Kamila [Regional Centre of Advanced Technologies and Materials, Department of Analytical Chemistry, Faculty of Science, Palacky University, 17.listopadu 12, CZ 771 46 Olomouc (Czech Republic); National Reference Laboratory for Chemical Elements, Department of Residues in Kroměříž, State Veterinary Institute Olomouc, Hulínská 2286, CZ 767 60 Kroměříž (Czech Republic); and others

2014-12-01

This study examined recoveries of silver determination in animal tissues after wet digestion by inductively coupled plasma mass spectrometry. The composition of the mineralization mixture for microwave assisted digestion was optimized and the best recoveries were obtained for mineralization with HNO{sub 3} and addition of HCl promptly after digestion. The optimization was performed on model samples of chicken meat spiked with silver nanoparticles and a solution of ionic silver. Basic calculations of theoretical distribution of Ag among various silver-containing species were implemented and the results showed that most of the silver is in the form of soluble complexes AgCl{sub 2}{sup −} and AgCl{sub 3}{sup 2−} for the optimized composition of the mineralization mixture. Three animal tissue certified reference materials were then analyzed to verify the trueness and precision of the results. - Highlights: • We performed detailed optimization of microwave assisted digestion procedure of animal tissue used prior to Ag determination by ICP-MS. • We provide basic equilibrium calculations to give theoretical explanation of results from optimization of tested mineralization mixtures. • Results from method validation that was done by analysis of several matrix CRMs are presented.

Sample diagnosis using indicator elements and non-analyte signals for inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Antler, Margaret; Ying Hai; Burns, David H.; Salin, Eric D.

2003-01-01

A sample diagnosis procedure that uses both non-analyte and analyte signals to estimate matrix effects in inductively coupled plasma-mass spectrometry is presented. Non-analyte signals are those of background species in the plasma (e.g. N + , ArO + ), and changes in these signals can indicate changes in plasma conditions. Matrix effects of Al, Ba, Cs, K and Na on 19 non-analyte signals and 15 element signals were monitored. Multiple linear regression was used to build the prediction models, using a genetic algorithm for objective feature selection. Non-analyte elemental signals and non-analyte signals were compared for diagnosing matrix effects, and both were found to be suitable for estimating matrix effects. Individual analyte matrix effect estimation was compared with the overall matrix effect prediction, and models used to diagnose overall matrix effects were more accurate than individual analyte models. In previous work [Spectrochim. Acta Part B 57 (2002) 277], we tested models for analytical decision making. The current models were tested in the same way, and were able to successfully diagnose matrix effects with at least an 80% success rate

On-line preconcentration and determination of chromium in parenteral solutions by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Gil, R.A.; Cerutti, S.; Gasquez, J.A.; Olsina, R.A.; Martinez, L.D.

2005-01-01

A method for the preconcentration and speciation of chromium was developed. On-line preconcentration and determination were obtained using inductively coupled plasma optical emission spectrometry (ICP-OES) coupled with flow injection. To determinate the chromium (III) present in parenteral solutions, chromium was retained on activated carbon at pH 5.0. On the other hand, a step of reduction was necessary in order to determine total chromium content. The Cr(VI) concentration was then determined by difference between the total chromium concentration and that of Cr(III). A sensitivity enrichment factor of 70-fold was obtained with respect to the chromium determination by ICP-OES without preconcentration. The detection limit for the preconcentration of 25 ml of sample was 29 ng l -1 . The precision for the 10 replicate determinations at the 5 μg l -1 Cr level was 2.3% relative standard deviation, calculated with the peak heights. The calibration graph using the preconcentration method for chromium species was linear with a correlation coefficient of 0.9995 at levels near the detection limits up to at least 60 μg l -1 . The method can be applied to the determination and speciation of chromium in parenteral solutions

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)

Intercomparison study of inductively coupled plasma mass spectrometry, thermal ionization mass spectrometry and fission track analysis of μBq quantities of 239Pu in synthetic urine

International Nuclear Information System (INIS)

Inn, K.G.W.; McCurdy, D.; Kuruvilla, L.; Barss, N.M.; Bell III, R.T.; Pietrzak, R.; Kaplan, E.; Inkret, W.; Efurd, W.; Rokop, D.; Lewis, D.; Gautier, P.

2001-01-01

Even today, some Marshall Islanders are looking forward to permanently resettling their islands after five decades. The U.S. Department of Energy and the resettled residents require reasonable but cost-prudent assurance that the doses to resident from residual 239 Pu will not exceed recognized international standards or recommendations, as estimated from the excretion of 239 Pu in urine. The goal of this study was to evaluate the bias, uncertainty and sensitivity of analytical techniques that measure 3-56 μBq 239 Pu in synthetic urine. The analytical techniques studied in this work included inductively coupled plasma mass spectrometry, thermal ionization mass spectrometry and fission track analysis. The results of the intercomparison demonstrated that all three techniques were capable of marking the measurements, although not with equal degree of bias and uncertainty. The estimated minimum detectable activity was 1 μBq of 239 Pu per synthetic urine sample. This exercise is also the first effort to certify test materials of plutonium in the nBqxg -1 range. (author)

Coupling between chip based isotachophoresis and multi-collector inductively coupled plasma mass spectrometry for separation and measurement of lanthanides

International Nuclear Information System (INIS)

Vio, Laurent; Cretier, Gerard; Rocca, Jean-Louis; Chartier, Frederic; Geertsen, Valerie; Gourgiotis, Alkiviadis; Isnard, Helene; Morin, Pierre

2012-01-01

This paper presents the conception and fabrication of a micro-system for lanthanides separation and its coupling with a multi-collector inductively coupled plasma mass spectrometer for isotope ratio measurements. The lanthanides separation is based on the isotachophoresis technique and the micro-system conception has been adapted in order to fit with glove box limitations in view of future spent nuclear fuels analysis. The micro-device was tested by using a mixture of standard solutions of natural elements and the separation of 13 lanthanides was successfully performed. The micro-device was then coupled to a multi-collector inductively coupled plasma mass spectrometer for the on-line measurements of Nd and Sm isotope ratios. The isotopes of Nd and Sm were acquired online in multi-collection mode after separation of the two elements with an injection amount of 5 ng. Results obtained on the Nd and Sm isotope ratio measurements on transient signals are presented and discussed. (authors)

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.

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.

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.

Determination of daily intake of elements from Philippine total diet samples using inductively coupled plasma-atomic emission spectrometry

International Nuclear Information System (INIS)

Leon, G.C. de; Shiraishi, K.; Kawamura, H.; Igaraishi, Y.; Palattao, M.V.; Azanon, E.M.

1990-10-01

Total diet samples were analyzed for major elements (Na, K, Ca, Mg, P) and some minor trace elements (Fe, Zn, Mn, Al, Sr, Cu, Ba, Yt) using inductively coupled plasma-atomic emission spectrometry (ICP-AES). Samples analyzed were classified into sex and age groups. Results for some elements (Na, K, Mg, Zn, Cu, Mn) were compared with values from Bataan dietary survey calculated using the Philippine composition table. Exceot for Na, analytical results were similar to calculated values. Analytical results for Ca and Fe were also compared with the values from Food and Nutrition Research Institute. In general, values obtained in the study were lower than the FNRI values. Comparison of the analytical and calculated results with the Japanese and ICRP data showed that Philippine values were lower than foreign values. (Auth.). 22 refs., 9 tabs

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

Science.gov (United States)

de Oliveira Souza, Sidnei; da Costa, Silvânio Silvério Lopes; Santos, Dayane Melo; dos Santos Pinto, Jéssica; Garcia, Carlos Alexandre Borges; Alves, José do Patrocínio Hora; Araujo, Rennan Geovanny Oliveira

2014-06-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg- 1 for Mn to 77.3 mg kg- 1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento - MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES).

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

The determination of low level trace elements in coals by laser ablation-inductively coupled plasma-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Booth, C.A.; Spears, D.A.; Krause, P.; Cox, A.G. [University of Sheffield, Sheffield (United Kingdom). Dept. of Earth Sciences

1999-11-01

The rapid determination of elements present in low level concentrations in bituminous coals is possible using laser abalation-inductively coupled plasma-mass spectrometry (l.a.-i.c.p.-m.s.). A wide range of trace elements can routinely be determined using this technique but it is for environmentally sensitive elements, such as As, Cd, Mo, Sb, Se and Hg, that it is of most use due to the low levels of detection. Calibration of the i.c.p.-m.s. was achieved using a series of uncertified coals and the method evaluated using the South African certified coals, Sarm 18, 19 and 20. A critical evaluation of the data obtained shows that for many of the elements studied the results obtained are both accurate and precise, even at very low concentrations, with the limits of detection for all of the elements being in the {mu}g/kg (parts per billion) range. 6 refs., 3 figs., 9 tabs.

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.

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.

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.

Classification of Antarctic algae by applying Kohonen neural network with 14 elements determined by inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Balbinot, L. [Departamento de Quimica Analitica-Instituto de Quimica-Unicamp, PO Box 6154, CEP: 13083-971, Campinas, SP (Brazil); Smichowski, P. [Comision Nacional de Energia Atomica, Unidad de Actividad Quimica, Centro Atomico Constituyentes, Av. Gral Paz 1499, B1650KNA, San Martin, Provincia de Buenos Aires (Argentina); Farias, S. [Comision Nacional de Energia Atomica, Unidad de Actividad Quimica, Centro Atomico Constituyentes, Av. Gral Paz 1499, B1650KNA, San Martin, Provincia de Buenos Aires (Argentina); Arruda, M.A.Z. [Departamento de Quimica Analitica-Instituto de Quimica-Unicamp, PO Box 6154, CEP: 13083-971, Campinas, SP (Brazil); Vodopivez, C. [Instituto Antartico Argentino, Cerrito 1010, C1248AAZ, Buenos Aires (Argentina); Poppi, R.J. [Departamento de Quimica Analitica-Instituto de Quimica-Unicamp, PO Box 6154, CEP: 13083-971, Campinas, SP (Brazil)]. E-mail: ronei@iqm.unicamp.br

2005-06-30

Optical emission spectrometers can generate results, which sometimes are not easy to interpret, mainly when the analyses involve classifications. To make simultaneous data interpretation possible, the Kohonen neural network is used to classify different Antarctic algae according to their taxonomic groups from the determination of 14 analytes. The Kohonen neural network architecture used was 5x5 neurons, thus reducing 14-dimension input data to two-dimensional space. The input data were 14 analytes (As, Co, Cu, Fe, Mn, Sr, Zn, Cd, Cr, Mo, Ni, Pb, Se, V) with their concentrations, determined by inductively coupled plasma optical emission spectrometry in 11 different species of algae. Three taxonomic groups (Rhodophyta, Phaeophyta and Cholorophyta) can be differentiated and classified through only their Cu content.

Classification of Antarctic algae by applying Kohonen neural network with 14 elements determined by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Balbinot, L.; Smichowski, P.; Farias, S.; Arruda, M.A.Z.; Vodopivez, C.; Poppi, R.J.

2005-01-01

Optical emission spectrometers can generate results, which sometimes are not easy to interpret, mainly when the analyses involve classifications. To make simultaneous data interpretation possible, the Kohonen neural network is used to classify different Antarctic algae according to their taxonomic groups from the determination of 14 analytes. The Kohonen neural network architecture used was 5x5 neurons, thus reducing 14-dimension input data to two-dimensional space. The input data were 14 analytes (As, Co, Cu, Fe, Mn, Sr, Zn, Cd, Cr, Mo, Ni, Pb, Se, V) with their concentrations, determined by inductively coupled plasma optical emission spectrometry in 11 different species of algae. Three taxonomic groups (Rhodophyta, Phaeophyta and Cholorophyta) can be differentiated and classified through only their Cu content

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

Characterization of a sealed Americium-Beryllium (AmBe) source by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Sommers, J.; Jimenez, M.; Adamic, M.; Giglio, J.; Carney, K.

2009-01-01

Two Americium-Beryllium neutron sources were dismantled, sampled (sub-sampled) and analyzed via inductively coupled plasma mass spectrometry (ICP-MS). Characteristics such as 'age' since purification, actinide content, trace metal content and inter and intra source composition were determined. The 'age' since purification of the two sources was determined to be 25.0 and 25.4 years, respectively. The systematic uncertainties in the 'age' determination were ±4% 2σ. The amount and isotopic composition of U and Pu varied substantially between the sub-samples of Source 2 (n = 8). This may be due to the physical means of sub-sampling or the way the source was manufactured. Source 1 was much more consistent in terms of content and isotopic composition (n = 3 sub-samples). The Be-Am ratio varied greatly between the two sources. Source 1 had an Am-Be ratio of 6.3 ± 52% (1σ). Source 2 had an Am-Be ratio of 9.81 ± 3.5% (1σ). In addition, the trace element content between the samples varied greatly. Significant differences were determined between Sources 1 and 2 for Sc, Sr, Y, Zr, Mo, Ba and W. (author)

Trace determination of Pu by LIF in an inductively coupled plasma

International Nuclear Information System (INIS)

Mauchien, P.; Briand, A.; Moulin, C.

1989-01-01

Inductively Coupled Plasma/Emission Spectrometry (ICP/ES) technique is largely used in the nuclear industry as an elementary analytical technique. Nevertheless, when the sample to analyse presents elements with a lot of emission spectral lines, spectral interferences lead to limited sensitivity. This is the case for Pu determination in presence of large U concentration. In pure aqueous solution, the limit of detection (LOD) for Pu is 10 μg/1. In presence of U, the LOD is determined by a ratio U/Pu = 1000. Pulsed Laser Induced Fluorescence (LIF) spectrometry is known to be a very selective technique when associated with an Inductively Coupled Plasma source. The absolute sensitivity is better by 2 or 3 orders of magnitude; its principle is based on selective excitation of the ionic species in the plasma followed by fluorescence radiation detection of these species; this radiation being practically free from spectral interferences, it is possible to improve the relative LOD. In this presentation, experimental results performed at Cogema/Marcoule laboratory are presented. After the experimental set-up description, first results of LIF are shown: - very good selectivity is effectively obtained, - a series of analytical results obtained with excitation scanning from the visible to the U.V. show that sensitivity of LIF technique is strictly related to the spectroscopic scheme

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.

Improved documentation of spectral lines for inductively coupled plasma emission spectrometry

Science.gov (United States)

Doidge, Peter S.

2018-05-01

An approach to improving the documentation of weak spectral lines falling near the prominent analytical lines used in inductively coupled plasma optical emission spectrometry (ICP-OES) is described. Measurements of ICP emission spectra in the regions around several hundred prominent lines, using concentrated solutions (up to 1% w/v) of some 70 elements, and comparison of the observed spectra with both recent published work and with the output of a computer program that allows calculation of transitions between the known energy levels, show that major improvements can be made in the coverage of spectral atlases for ICP-OES, with respect to "classical" line tables. It is argued that the atomic spectral data (wavelengths, energy levels) required for the reliable identification and documentation of a large majority of the weak interfering lines of the elements detectable by ICP-OES now exist, except for most of the observed lines of the lanthanide elements. In support of this argument, examples are provided from a detailed analysis of a spectral window centered on the prominent Pb II 220.353 nm line, and from a selected line-rich spectrum (W). Shortcomings in existing analyses are illustrated with reference to selected spectral interferences due to Zr. This approach has been used to expand the spectral-line library used in commercial ICP-ES instruments (Agilent 700-ES/5100-ES). The precision of wavelength measurements is evaluated in terms of the shot-noise limit, while the absolute accuracy of wavelength measurement is characterised through comparison with a small set of precise Ritz wavelengths for Sb I, and illustrated through the identification of Zr III lines; it is further shown that fractional-pixel absolute wavelength accuracies can be achieved. Finally, problems with the wavelengths and classifications of certain Au I lines are discussed.

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.

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.

Separation and analysis of lanthanides by isotachophoresis coupled with inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Vio, Laurent; Cretier, Gerard; Rocca, Jean-Louis; Chartier, Frederic; Geertsen, Valerie; Gourgiotis, Alkiviadis; Isnard, Helene

2012-01-01

This study is a large project initiated by the French Nuclear Agency, and concerns the development of a new electrolyte system for the separation of lanthanides by isotachophoresis. This new system is based on a leading electrolyte that incorporates 2-hydroxy-2-methylbutyric acid as complexing agent. The optimization of separation conditions (complexing agent concentration, pH, capillary dimensions, injection conditions, and current intensity) performed by experiments on a commercial capillary instrument with contactless conductivity detection, which allows to improve the separation of 13 lanthanides (La to Lu, except Pm and Ho). We have also directly coupled the isotachophoresis to an inductively coupled plasma mass spectrometer to visualize the mono-elementary elution bands and demonstrate the potentiality of the method for isotope ratio measurements. The application to a simulated solution representative of a fraction of fission products present in a MOX spent fuel is presented in this paper to demonstrate the possible application in future on nuclear fuel samples. (authors)

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, ...

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

Determination of Cd and Pb in human blood by isotope dilution inductively coupled plasma mass spectrometry : International comparison

International Nuclear Information System (INIS)

Park, Chang Joon; Suh, Jeong Ki; Lee, Sang Hwa

1996-01-01

Inorganic analytical laboratory of Korea Research Institute of Standards and Science participated in an interlaboratory comparison program operated by Quebec Toxicology Centre of Canada in 1994 and again in 1995. The objective of this program is to enable participating laboratories to assess reproducibility and accuracy of their analytical results for trace toxic elements in human biological fluids. This laboratory determined Cd and Pb concentrations in 3 levels of human blood samples by isotope dilution inductively coupled plasma mass spectrometry. 0.5 mL of blood sample is added to the digestion bomb together with 2 mL of nitric acid and enriched spike isotopes and then decomposed in the microwave digestion system. The decomposed sample is diluted to 10 mL and nebulized into ICP-MS. The Cd and Pb values reported by all participating laboratories are presented and compared. The values reported by this laboratory are within the acceptable range of target values. (author)

Barium determination in gastric contents, blood and urine by inductively coupled plasma mass spectrometry in the case of oral barium chloride poisoning.

Science.gov (United States)

Łukasik-Głębocka, Magdalena; Sommerfeld, Karina; Hanć, Anetta; Grzegorowski, Adam; Barałkiewicz, Danuta; Gaca, Michał; Zielińska-Psuja, Barbara

2014-01-01

A serious case of barium intoxication from suicidal ingestion is reported. Oral barium chloride poisoning with hypokalemia, neuromuscular and cardiac toxicity, treated with intravenous potassium supplementation and hemodialysis, was confirmed by the determination of barium concentrations in gastric contents, blood, serum and urine using the inductively coupled plasma mass spectrometry method. Barium concentrations in the analyzed specimens were 20.45 µg/L in serum, 150 µg/L in blood, 10,500 µg/L in urine and 63,500 µg/L in gastric contents. Results were compared with barium levels obtained from a non-intoxicated person. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Line width and line shape analysis in the inductively coupled plasma by high resolution Fourier transform spectrometry

International Nuclear Information System (INIS)

Faires, L.M.; Palmer, B.A.; Brault, J.W.

1984-01-01

High resolution Fourier transform spectrometry has been used to perform line width and line shape analysis of eighty-one iron I emision lines in the spectral range 290 to 390nm originating in the normal analytical zone of an inductively coupled plasma. Computer programs using non-linear least squares fitting techniques for line shape analysis were applied to the fully resolved spectra to determine Gaussian and Lorentzian components of the total observed line width. The effect of noise in the spectrum on the precision of the line fitting technique was assessed, and the importance of signal to noise ratio for line shape analysis is discussed. Translational (Doppler) temperatures were calculated from the Gaussian components of the line width and were found to be on the order of 6300 0 K. The excitation temperature of iron I was also determined from the same spectral data by the spectroscopic slope method based on the Einstein-Boltzmann expression for spectral intensity and was found to be on the order of 4700 0 K. 31 references

[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.

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

Determination of zinc stable isotopes in biological materials using isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Patterson, K.Y.; Veillon, Claude

1992-01-01

A method is described for using isotope dilution to determine both the amount of natural zinc and enriched isotopes of zinc in biological samples. Isotope dilution inductively coupled plasma mass spectrometry offers a way to quantify not only the natural zinc found in a sample but also the enriched isotope tracers of zinc. Accurate values for the enriched isotopes and natural zinc are obtained by adjusting the mass count rate data for measurable instrumental biases. Analytical interferences from the matrix are avoided by extracting the zinc from the sample matrix using diethylammonium diethyldithiocarbamate. The extraction technique separates the zinc from elements which form interfering molecular ions at the same nominal masses as the zinc isotopes. Accuracy of the method is verified using standard reference materials. The detection limit is 0.06 μg Zn per sample. Precision of the abundance ratios range from 0.3-0.8%. R.S.D. for natural zinc concentrations is about 200-600 μg g -1 . The accuracy and precision of the measurements make it possible to follow enriched isotopic tracers of zinc in biological samples in metabolic tracer studies. (author). 19 refs.; 1 fig., 4 tabs

Aluminium content of some processed foods, raw materials and food additives in China by inductively coupled plasma-mass spectrometry.

Science.gov (United States)

Deng, Gui-Fang; Li, Ke; Ma, Jing; Liu, Fen; Dai, Jing-Jing; Li, Hua-Bin

2011-01-01

The level of aluminium in 178 processed food samples from Shenzhen city in China was evaluated using inductively coupled plasma-mass spectrometry. Some processed foods contained a concentration of up to 1226 mg/kg, which is about 12 times the Chinese food standard. To establish the main source in these foods, Al levels in the raw materials were determined. However, aluminium concentrations in raw materials were low (0.10-451.5 mg/kg). Therefore, aluminium levels in food additives used in these foods was determined and it was found that some food additives contained a high concentration of aluminium (0.005-57.4 g/kg). The results suggested that, in the interest of public health, food additives containing high concentrations of aluminium should be replaced by those containing less. This study has provided new information on aluminium levels in Chinese processed foods, raw materials and a selection of food additives.

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)

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

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.

Use of oxidative and reducing vapor generation for reducing the detection limits of iodine in biological samples by inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Vtorushina, Eh.A.; Saprykin, A.I.; Knapp, G.

2009-01-01

Procedures of microwave combustion in an oxygen flow and microwave acid decomposition of biological samples were optimized for the subsequent determination of iodine. A new method was proposed for the generation of molecular iodine from periodate iona using hydrogen peroxide as a reductant. Procedures were developed for determining iodine in biological samples by inductively coupled plasma atomic emission spectrometry (ICP-AES) using oxidative and reducing vapor generation; these allowed the detection limit for iodine to be lowered by 3-4 orders of magnitude. The developed procedures were used to analyze certified reference materials of milk (Skim Milk Powder BCR 150) and seaweed (Sea Lettuce BCR 279) and a Supradyn vitamin complex

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

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

A Tightly Coupled Non-Equilibrium Magneto-Hydrodynamic Model for Inductively Coupled RF Plasmas

Science.gov (United States)

2016-02-29

development a tightly coupled magneto-hydrodynamic model for Inductively Coupled Radio- Frequency (RF) Plasmas. Non Local Thermodynamic Equilibrium (NLTE...for Inductively Coupled Radio-Frequency (RF) Plasmas. Non Local Thermodynamic Equilibrium (NLTE) effects are described based on a hybrid State-to-State...Inductively Coupled Plasma (ICP) torches have wide range of possible applications which include deposition of metal coatings, synthesis of ultra-fine powders

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.

Ultra-trace determination of iodine in sediments and biological material using UV photochemical generation-inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Grinberg, Patricia [Institute for National Measurements Standards, National Research Council Canada, Ottawa, Ontario, K1A 0R6 (Canada)], E-mail: patricia.grinberg@nrc.ca; Sturgeon, Ralph E. [Institute for National Measurements Standards, National Research Council Canada, Ottawa, Ontario, K1A 0R6 (Canada)

2009-03-15

Several sample preparation techniques have been evaluated for the determination of iodine using UV-photochemical generation-quadrupole inductively coupled plasma mass spectrometry. Thermal decomposition of samples at 1000 {sup o}C followed by capture of the liberated iodine in dilute acetic acid permitted subsequent UV-photochemical generation of a volatile iodine species that serves to enhance sensitivity 25-fold over conventional solution nebulization, delivering reagent blank detection limits of 8.75 pg g{sup -1127}I and 0.075 pg g{sup -1129}I for solid samples (400 mg test mass). The methodology was validated through determination of total iodine in several Standard Reference Materials, including NIST 1572 Citrus leaves, NIST 1549 Non-fat milk powder, NIST 1566a Oyster tissue and NIST 2709 San Joaquin Soil. Liberation of iodine from samples and its collection as well as photochemical generation were quantitative, permitting calibration to be achieved using standards prepared in dilute acetic acid.

Determination of the mineral compositions of in six beans by microwave digestion with inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Yan, Q.; Yang, L.; Chen, S.; Liu, X.; Ma, X.

2012-01-01

In the study, microwave digestion procedure optimized was applied for digesting beans. Nineteen mineral element concentrations were determined by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES). The result indicated detection limits for the 19 elements were less than 0.0998, and relative standard deviations were 1.01% - 5.02% for all the elements, and recoveries were 90.89% - 104.55% by adding standard recovery experiment. The study showed the beans selected were abundant in mineral element contents in human nutrition, determination mineral element contents by ICP-AES with microwave digestion technology were a lot of merits of small environmental pollution, fast and accurate determination result, which could satisfy the examination request of bean samples. The results provided evidence that the six beans were a good source of K, P, Mg and Ca. This study is to give important reference value to people due to individual differences by adjusting the dietary to complement the different mineral elements. (author)

Chromatographic retention of molybdenum, titanium and uranium complexes for removal of some interferences in inductively-coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Jiang, S.-J.; Palmieri, M.D.; Fritz, J.S.; Houk, R.S.; Iowa State Univ., of Science and Technology, Ames

1987-01-01

Complexes of molybdenum(VI) or titanium(IV) with N-methylfurohydroxamic acid (N-MFHA) are retained on a column packed with polystyrene/divinylbenzene. At the pH values chosen, copper, zinc and cadmium are washed rapidly through the column and are detected by inductively-coupled plasma mass spectrometry without interference from metal oxide ions of titanium or molybdenum. Detection limits are 1 to 2 μg l -1 , and analyte recoveries are essentially 100%. The resin capacity for the titanium and molybdenum complexes is sufficient for several hundred injections, and the complexes can be readily washed from the column. Uranium(VI) also forms a stable complex with N-MFHA, and ionization interference caused by excess of uranium can be avoided by chromatographic removal of the uranium complex. Various other potentially interfering elements with aqueous oxidation states of +4 or higher (e.g. Sn, W, Hf or Zr) could also be separated by this technique. 33 refs.; 4 figs.; 3 tabs

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

Determination of stable cesium and strontium in rice samples by inductively coupled plasma mass spectrometry

Science.gov (United States)

Srinuttrakul, W.; Yoshida, S.

2017-06-01

For long-term radiation dose assessment models, food ingestion is one of the major exposure pathways to human. In general, the stable isotopes can serve as analogues of radioisotopes. In this study, rice samples were collected from 30 paddy fields in Si Sa Ket, Yasothon and Roi Et in the northeast of Thailand in November 2014. The concentrations of stable cesium (Cs-133) and strontium (Sr-88) in polished rice were determined by inductively coupled plasma mass spectrometry (ICP-MS). The standard reference material of rice flour (NIST 1568a) with spiked Cs and Sr was used to validate the analytical method. The concentration of Cs in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.158 ± 0.167 mg kg-1, 0.090 ± 0.117 mg kg-1 and 0.054 ± 0.031 mg kg-1, respectively. The concentration of Sr in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.351 ± 0.108 mg kg-1, 0.364 ± 0.215 mg kg-1 and 0.287 ± 0.102 mg kg-1, respectively. Comparison of the results with Japanese data before the Fukushima Di-ichi nuclear power plant accident showed that the concentrations of both Cs and Sr for Thai rice were higher than those for Japanese rice.

Determination of stable cesium and strontium in rice samples by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Srinuttrakul, W; Yoshida, S

2017-01-01

For long-term radiation dose assessment models, food ingestion is one of the major exposure pathways to human. In general, the stable isotopes can serve as analogues of radioisotopes. In this study, rice samples were collected from 30 paddy fields in Si Sa Ket, Yasothon and Roi Et in the northeast of Thailand in November 2014. The concentrations of stable cesium (Cs-133) and strontium (Sr-88) in polished rice were determined by inductively coupled plasma mass spectrometry (ICP-MS). The standard reference material of rice flour (NIST 1568a) with spiked Cs and Sr was used to validate the analytical method. The concentration of Cs in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.158 ± 0.167 mg kg -1 , 0.090 ± 0.117 mg kg -1 and 0.054 ± 0.031 mg kg -1 , respectively. The concentration of Sr in polished rice from Si Sa Ket, Yasothon and Roi Et was 0.351 ± 0.108 mg kg -1 , 0.364 ± 0.215 mg kg -1 and 0.287 ± 0.102 mg kg -1 , respectively. Comparison of the results with Japanese data before the Fukushima Di-ichi nuclear power plant accident showed that the concentrations of both Cs and Sr for Thai rice were higher than those for Japanese rice. (paper)

Standard test method for determination of impurities in nuclear grade uranium compounds by inductively coupled plasma mass spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2010-01-01

1.1 This test method covers the determination of 67 elements in uranium dioxide samples and nuclear grade uranium compounds and solutions without matrix separation by inductively coupled plasma mass spectrometry (ICP-MS). The elements are listed in Table 1. These elements can also be determined in uranyl nitrate hexahydrate (UNH), uranium hexafluoride (UF6), triuranium octoxide (U3O8) and uranium trioxide (UO3) if these compounds are treated and converted to the same uranium concentration solution. 1.2 The elements boron, sodium, silicon, phosphorus, potassium, calcium and iron can be determined using different techniques. The analyst's instrumentation will determine which procedure is chosen for the analysis. 1.3 The test method for technetium-99 is given in Annex A1. 1.4 The values stated in SI units are to be regarded as standard. 1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish ...

On-line system for preconcentration and determination of metals in vegetables by Inductively Coupled Plasma Optical Emission Spectrometry

International Nuclear Information System (INIS)

Bezerra, Marcos A.; Santos, Walter N.L. dos; Lemos, Valfredo A.; Korn, Maria das Gracas A.; Ferreira, Sergio L.C.

2007-01-01

A procedure has been developed for the simultaneous determination of trace amounts of cadmium, copper, chromium, nickel and lead in digested vegetable samples. The method involves solid-phase extraction of the metals using a minicolumn of Amberlite XAD-4 modified with dihydroxybenzoic acid (DHB) and detection by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The elution of the metals from minicolumn was performed with 1.0 mol L -1 hydrochloric acid. Variables associated with flow preconcentration system performance, such as pH, buffer concentration, eluent concentration and sampling flow rate, were optimized. The developed procedure provides enrichment factors of 100, 72, 16, 91 and 53, for cadmium, copper, chromium, nickel and lead, respectively. Detection limits (3σ B ) were 0.02 (Cd), 0.23 (Cu), 0.58 (Cr), 0.060 (Ni) and 0.54 (Pb) μg L -1 . The procedure was applied for determination of metals in samples of guarana and cabbage. The accuracy of the method was checked by the analysis of a certified reference material (NIST 1571, Orchard leaves). Results found were in agreement with certified values

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)

Rapid Determination of Plutonium Isotopes in Environmental Samples Using Sequential Injection Extraction Chromatography and Detection by Inductively Coupled Plasma Mass Spectrometry

DEFF Research Database (Denmark)

Qiao, Jixin; Hou, Xiaolin; Roos, Per

2009-01-01

This article presents an automated method for the rapid determination of 239Pu and 240Pu in various environmental samples. The analytical method involves the in-line separation of Pu isotopes using extraction chromatography (TEVA) implemented in a sequential injection (SI) network followed...... by detection of isolated analytes with inductively coupled plasma mass spectrometry (ICP-MS). The method has been devised for the determination of Pu isotopes at environmentally relevant concentrations, whereby it has been successfully applied to the analyses of large volumes/amounts of samples, for example......, 100−200 g of soil and sediment, 20 g of seaweed, and 200 L of seawater following analyte preconcentration. The investigation of the separation capability of the assembled SI system revealed that up to 200 g of soil or sediment can be treated using a column containing about 0.70 g of TEVA resin...

Speciation of the bio-available iodine and bromine forms in edible seaweed by high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry

International Nuclear Information System (INIS)

Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Jorge; Moreda-Piñeiro, Antonio

2012-01-01

Highlights: ► Bioavailable iodine and bromine speciation in edible seaweed were developed. ► In vitro dialyzability was used to assess the bioavailable fractions. ► AEC hyphenated with inductively coupled plasma-mass spectrometry was used. ► Iodide, MIT, DIT, bromide and bromate were found in dialyzates from edible seaweed. ► Positive correlation between bioavailability and protein contents was found. - Abstract: A bioavailability study based on an in vitro dialyzability approach has been applied to assess the bio-available fractions of iodine and bromine species from edible seaweed. Iodide, iodate, 3-iodo-tyrosine (MIT), 3,5-diiodo-tyrosine (DIT), bromide and bromate were separated by anion exchange chromatography under a gradient elution mode (175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase, and flow rates within the 0.5–1.5 mL min −1 range). Inductively coupled plasma-mass spectrometry (ICP-MS) was used as a selective detector for iodine ( 127 I) and bromine ( 79 Br). Low dialyzability ratios (within the 2.0–18% range) were found for iodine species; whereas, moderate dialyzability percentages (from 9.0 to 40%) were obtained for bromine species. Iodide and bromide were the major species found in the dialyzates from seaweed, although MIT and bromate were also found in the dialyzates from most of the seaweed samples analysed. However, DIT was only found in dialyzates from Wakame, Kombu, and NIES 09 (Sargasso) certified reference material; whereas, iodate was not found in any dialyzate. Iodine dialyzability was found to be dependent on the protein content (negative correlation), and on the carbohydrate and dietary fibre levels (positive correlation). However, bromine dialyzability was only dependent on the protein amount in seaweed (negative correlation).

Laser ablation-inductively coupled plasma mass spectrometry for the characterization of pigments in prehistoric rock art.

Science.gov (United States)

Resano, Martin; García-Ruiz, Esperanza; Alloza, Ramiro; Marzo, Maria P; Vandenabeele, Peter; Vanhaecke, Frank

2007-12-01

In this work, several red-colored paintings of post-Paleolithic schematic style found in 10 different shelters in the vicinity of the Vero River (Huesca) were sampled and subjected to analysis by means of scanning electron microscopy-energy-dispersive X-ray spectrometry (SEM-EDX), Raman spectroscopy, and laser ablation-inductively coupled plasma mass spectrometry (LA-ICPMS). The goal of this research was to obtain meaningful information on the samples composition, in order to establish differences or similarities among them. The combined use of these techniques proved beneficial, as Raman data permitted structural information on the compounds present (hematite was identified as the main pigment, whereas calcite and gypsum are the main components of the substrate layer, as well as of the accretions that covered the pigments) to be obtained, while the quantitative values obtained by SEM were suitable for the use of Ca as internal reference during LA-ICPMS analysis. However, it was this latter technique that provided the most relevant data for fingerprinting purposes. The potential of this technique for obtaining spatially resolved information allowed the multielement quantitative analysis of the pigment layer, in spite of the presence of superficial accretions. The sensitivity of the technique permitted the determination of more than 40 elements present in a wide concentration range (from microgram per gram to 10% level) with minimum sample consumption (approximately 900 ng for each sample, corresponding to five replicates). Finally, in order to establish significant differences, only those elements showing a high correlation with Fe (As, Co, Mo, Sb, Tl, and Zr, in this case) were selected, as it is expected that these were truly present in the original pigment, while others could have migrated into the pigment layer throughout time. By using this information, it seems feasible to discriminate between various paint pots, as demonstrated for the samples under

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).

Critical comparison of performances of inductively coupled plasma atomic emission spectrometry and neutron activation analysis for the determination of elements in human lungs

International Nuclear Information System (INIS)

Alimonti, A.; Coni, E.; Caroli, S.; Sabbioni, E.; Nicolaou, G.E.; Pietra, R.

1989-01-01

A study was carried out to assess the performance of inductively coupled plasma atomic emission spectrometry (ICP-AES) and neutron activation analysis (NAA) techniques for determining reference values for Al, Cd, Cr, Cu, Mg, Mn, V and Zn in human lungs of urban non-smoking subjects. Experimental data were subjected to the usual basic statistical tests to evaluate the respective merits of the two basically different analytical techniques. Both approaches, if used under carefully optimised experimental conditions, can yield reliable results affected only minimally by systematic and random errors. On the other hand, on a more routine basis, particular attention should be paid to elements such as Al, Cd and V which may pose some problems with both techniques. (author)

On-line digestion in a focused microwave-assisted oven for elements determination in orange juice by inductively coupled plasma optical emission spectrometry

Directory of Open Access Journals (Sweden)

Fili Sabrina P.

2003-01-01

Full Text Available A flow injection system coupled to focused microwave-assisted oven was used for on-line orange juice sample digestion for determination of Ca, Cu, Fe, K, Mg, Mn, Na, P, and Zn by inductively coupled plasma optical emission spectrometry. The reactor coil was a PTFE tube (4.0 m long and 1.6 mm i.d. positioned into the commercial glass tube of the focused microwave oven. Aliquots of 500 muL of sample and 1000 muL of reagent (80% v/v HNO3 were mixed in a confluence and carried out to the reactor coil by air carrier. The relative standard deviation for five replicates of sample was lower than 5.0%. Good recoveries varying from 91 to 111% were obtained for added concentrations of the interest elements. The results obtained using the proposed digestion system are in agreement with those obtained for total digestion at the 95% confidence level. With this on-line digestion system was possible to carry out 12 samples h-1, minimizing contamination, saving consumption of samples and reagent and low residue generation.

Elemental ratios for characterization of quantum-dots populations in complex mixtures by asymmetrical flow field-flow fractionation on-line coupled to fluorescence and inductively coupled plasma mass spectrometry.

Science.gov (United States)

Menendez-Miranda, Mario; Fernandez-Arguelles, Maria T; Costa-Fernandez, Jose M; Encinar, Jorge Ruiz; Sanz-Medel, Alfredo

2014-08-11

Separation and identification of nanoparticles of different composition, with similar particle diameter, coexisting in heterogeneous suspensions of polymer-coated CdSe/ZnS quantum dots (QDs) have been thoroughly assessed by asymmetric flow field-flow fractionation (AF4) coupled on-line to fluorescence and inductively coupled plasma mass spectrometry (ICPMS) detectors. Chemical characterization of any previously on-line separated nanosized species was achieved by the measurement of the elemental molar ratios of every element involved in the synthesis of the QDs, using inorganic standards and external calibration by flow injection analysis (FIA). Such elemental molar ratios, strongly limited so far to pure single nanoparticles suspensions, have been achieved with adequate accuracy by coupling for the first time an ICP-QQQ instrument to an AF4 system. This hyphenation turned out to be instrumental to assess the chemical composition of the different populations of nanoparticles coexisting in the relatively complex mixtures, due to its capabilities to detect the hardly detectable elements involved in the synthesis. Interestingly such information, complementary to that obtained by fluorescence, was very valuable to detect and identify unexpected nanosized species, present at significant level, produced during QDs synthesis and hardly detectable by standard approaches. Copyright © 2014. Published by Elsevier B.V.

Development of anion-exchange/reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry methods for the speciation of bio-available iodine and bromine from edible seaweed.

Science.gov (United States)

Romarís-Hortas, Vanessa; Bermejo-Barrera, Pilar; Moreda-Piñeiro, Antonio

2012-05-04

Anion exchange high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry has been novelly applied to assess inorganic (iodide and iodate) and organic (3-iodotyrosine - MIT, and 3,5-diiodotyrosine - DIT) iodine species in a single chromatographic run. The optimized operating conditions (Dionex IonPac AS7, gradient elution with 175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase and flow rates within the 0.5-1.5 mL min(-1) range) have also been used to perform inorganic bromine speciation analysis (bromide and bromate). The developed method has been applied for determining the bio-available contents of iodine and bromine species in dialyzates from edible seaweed. Reverse phase high performance liquid chromatography (Zorbax Eclipse XDB-C8, gradient elution with 0.2% (m/m) acetic acid, and 0.2% (m/m) acetic acid in methanol, as mobile phases, and a constant flow rate of 0.75 mL min(-1)) also hyphenated with inductively coupled plasma-mass spectrometry was used to confirm the presence of organic iodine species (MIT and DIT) in the dialyzates. The verification of the presence of iodinated amino acids (MIT and DIT) in the extracts was also performed by reverse phase high performance liquid chromatography-electrospray ionization-mass spectrometry (LTQ Orbitrap). The developed methods have provided good repeatability (RSD values lower than 10% for both anion exchange and reverse phase separations) and analytical recoveries within the 90-105% range for all cases. The in vitro bio-availability method consisted of a simulated gastric and an intestinal digestion/dialysis (10 kDa molecular weight cut-off - MWCO) two-stage procedure. Iodide and MIT were the main bio-available species quantified, whereas bromide was the major bromine species found in the extracts. Copyright © 2012 Elsevier B.V. All rights reserved.

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.

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.

Determination of Cu, Mn, Ni and Sn in gasoline by electrothermal vaporization inductively coupled plasma mass spectrometry, and emulsion sample introduction

International Nuclear Information System (INIS)

Saint'Pierre, Tatiana D.; Dias, Lucia Felicidade; Pozebon, Dirce; Aucelio, Ricardo Q.; Curtius, Adilson J.; Welz, Bernhard

2002-01-01

Trace metals in fuels, except in the case of additives, are usually undesirable and normally they occur in very low concentrations in gasoline, requiring sensitive techniques for their determination. Coupling of electrothermal vaporization with inductively coupled plasma mass spectrometry minimizes the problems related to the introduction of organic solvents into the plasma. Furthermore, sample preparation as oil-in-water emulsions reduces problems related to gasoline analysis. In this work, a method for determination of Cu, Mn, Ni and Sn in gasoline is proposed. Samples were prepared by forming a 10-fold diluted emulsion with a surfactant (Triton X-100), after treatment with concentrated HNO 3 . The sample emulsion was pre-concentrated in the graphite tube by repeated pipetting and drying. External calibration was used with aqueous standards in a purified gasoline emulsion. Six samples from different gas stations were analyzed, and the analyte concentrations were found to be in the μg l -1 range or below. The limits of detection were 0.22, 0.02, 0.38 and 0.03 μg l -1 for Cu, Mn, Ni and Sn, respectively. The accuracy of the method was estimated using a recovery test

Mercury speciation in thawed out and refrozen fish samples by gas chromatography coupled to inductively coupled plasma mass spectrometry and atomic fluorescence spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Krystek, Petra; Ritsema, Rob [National Institute for Public Health and the Environment (RIVM), Laboratory for Analytical Chemistry, Bilthoven (Netherlands)

2005-01-01

Different sub-sampling procedures were applied for the determination of mercury species (as total mercury Hg, methylmercury MeHg{sup +} and inorganic mercury Hg{sup 2+}) in frozen fish meat. Analyses were carried out by two different techniques. After the sample material was pre-treated by microwave digestion, atomic fluorescence spectroscopy (AFS) was used for the determination of total Hg. Speciation analysis was performed according to the following procedure: dissolution of sample material in tetramethylammonium hydroxide (TMAH), derivatisation with sodium tetraethylborate (NaBEt{sub 4}), extraction into isooctane and measurement with gas chromatography inductively coupled plasma mass spectrometry (GC-ICPMS) for the identification and quantification of methylmercury (MeHg{sup +}) and inorganic mercury (Hg{sup 2+}). The concentration range of total Hg measured in the shark fillets is between 0.9 and 3.6 {mu}g g{sup -1} thawed out shark fillet. Speciation analysis leads to {>=}94% Hg present as MeHg{sup +}. Homogeneity, storage conditions and stability of analytical species and sample materials have great influence on analytical results. Sub-sampling of half-frozen/partly thawed out fish and analysis lead to significantly different concentrations, which are on average a factor of two lower. (orig.)

An evaluation of inductively coupled plasma optical emission spectrometry using electrothermal atomisation sample introduction and photographic plate detection

International Nuclear Information System (INIS)

Khathing, D.T.; Pickford, C.J.

1984-05-01

A photographic radiation measurement approach has been used with an inductively coupled plasma source to evaluate and tabulate the more prominent optical emission lines of 66 elements. Compared with the more common sample introduction technique using nebulisation, increased sensitivity for multielement analysis of small samples was achieved by using a simple graphite electrothermal atomisation system. This was constructed to serve as a dual purpose atomiser ie both for Atomic Absorption and for Inductively Coupled Plasma Emission spectroscopy. The system offers the advantage of a wide multi-elemental coverage, but sensitivities achieved with photographic detection are poorer than those obtained photoelectrically. (author)

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Oliveira Souza, Sidnei de; Silvério Lopes da Costa, Silvânio; Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges

2014-01-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg −1 for Mn to 77.3 mg kg −1 for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO 3 and H 2 O 2 ) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The ICP OES technique can be

Simultaneous determination of macronutrients, micronutrients and trace elements in mineral fertilizers by inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Oliveira Souza, Sidnei de [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Silvério Lopes da Costa, Silvânio [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); Coordenação de Química, Universidade Federal de Alagoas (UFAL), Campus Arapiraca, 57309-005, Arapiraca, AL (Brazil); Santos, Dayane Melo; Santos Pinto, Jéssica dos; Garcia, Carlos Alexandre Borges [Laboratório de Química Analítica Ambiental (LQA), Departamento de Química, Centro de Ciências Exatas e Tecnologia, Universidade Federal de Sergipe (UFS), 49100-000, São Cristovão, SE (Brazil); and others

2014-06-01

An analytical method for simultaneous determination of macronutrients (Ca, Mg, Na and P), micronutrients (Cu, Fe, Mn and Zn) and trace elements (Al, As, Cd, Pb and V) in mineral fertilizers was optimized. Two-level full factorial design was applied to evaluate the optimal proportions of reagents used in the sample digestion on hot plate. A Doehlert design for two variables was used to evaluate the operating conditions of the inductively coupled plasma optical emission spectrometer in order to accomplish the simultaneous determination of the analyte concentrations. The limits of quantification (LOQs) ranged from 2.0 mg kg{sup −1} for Mn to 77.3 mg kg{sup −1} for P. The accuracy and precision of the proposed method were evaluated by analysis of standard reference materials (SRMs) of Western phosphate rock (NIST 694), Florida phosphate rock (NIST 120C) and Trace elements in multi-nutrient fertilizer (NIST 695), considered to be adequate for simultaneous determination. Twenty-one samples of mineral fertilizers collected in Sergipe State, Brazil, were analyzed. For all samples, the As, Ca, Cd and Pb concentrations were below the LOQ values of the analytical method. For As, Cd and Pb the obtained LOQ values were below the maximum limit allowed by the Brazilian Ministry of Agriculture, Livestock and Food Supply (Ministério da Agricultura, Pecuária e Abastecimento — MAPA). The optimized method presented good accuracy and was effectively applied to quantitative simultaneous determination of the analytes in mineral fertilizers by inductively coupled plasma optical emission spectrometry (ICP OES). - Highlights: • Determination of inorganic constituents in mineral fertilizers was proposed. • Experimental design methodology was used to optimize analytical method. • The sample preparation procedure using diluted reagents (HNO{sub 3} and H{sub 2}O{sub 2}) was employed. • The analytical method was satisfactorily to the determination of thirteen elements. • The

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

Chemical characterization of materials by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Deb, S.B.; Nagar, B.K.; Saxena, M.K.; Ramakumar, K.L.

2009-11-01

An Inductively Coupled Plasma Mass Spectrometer was procured for trace elemental determination in diverse samples. Since its installation a number of analytical measurements have been carried out on different sample matrices. These include chemical quality control measurements of nuclear fuel and other materials such as uranium metal. Uranium peroxide, ADU, ThO 2 , UO 2 ; isotopic composition of B, Li; chemical characterization of simulated ThO 2 + 2%UO 2 fuel; sodium zirconium phosphate and trace metallic elements in zirconium; Antarctica rock samples and wet phosphoric acid. Necessary separation methodologies required for effective removal of matrix were indigenously developed. In addition, a rigorous analytical protocol, which includes various calibration methodologies such as mass calibration, response calibration, detector cross calibration and linearity check over the entire dynamic range of 109 required for quantitative determination of elements at trace and ultra trace level,, has been standardized. This report summarizes efforts of RACD that have been put in this direction for the application of ICP-MS for analytical measurements. (author)

[Determination of five arsenic species in rice by liquid chromatography-inductively coupled plasma-mass spectrometry].

Science.gov (United States)

Gong, Jiadi; Cao, Xiaolin; Cao, Zhaoyun; Bian, Yingfang; Yu, Shasha; Chen, Mingxue

2014-07-01

A method was developed for the simultaneous determination of arsenic acid [As (V)], arsenious acid [As (III)], arsenobetaine (AsB), monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA) in rice by liquid chromatography-inductively coupled plasma-mass spectrometry (LC-ICP-MS). The extraction reagent was 0.3 mol/L nitric acid with heat-assistant condition for 1.5 h at 95 degrees C. Then, the five arsenic species were separated by an anion exchange column (Dionex IonPac AS19, 250 mm x 4 mm) and detected by ICP-MS. Four kinds of extracted solutions were compared through the extraction efficiency. The concentration of nitric acid, the temperature and the extraction time were optimized. The recoveries of the five arsenic species spiked in rice at two levels ranged from 89.6% to 99.5% with the relative standard deviations (RSDs, n = 5) of 0.6% - 3.6%. The measured values of the arsenic species in standard rice materials were consistent with their standard values. The linear ranges were 0.05 - 200 microg/L for AsB and DMA, 0.10-400 microg/L for As (III) and MMA, 0.15-600 microg/L for As (V). The limits of detection for the five arsenic species were 0.15-0.45 microg/kg. The results showed that the method is much more precise for the risk assessment of the rice. This method is simple, accurate and durable for the determination of arsenic species in rice.

{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.

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.

Possibilities of High Resolution Inductively Coupled Plasma Optical Emission Spectrometry in the Determination of Trace Elements in Environmental Materials

Directory of Open Access Journals (Sweden)

Nikolaya Velitchkova

2013-01-01

Full Text Available This paper presents new quantitative data for the spectral interferences obtained by high resolution 40.68 MHz radial viewing inductively coupled plasma optical emission spectrometry (HR-ICP-OES in the determination of Zn, Cd, Sb, Cu, Mn, Pb, Sn, Cr, U, and Ba in environmental materials in the presence of a complex matrix, containing Al, Ca, Fe, Mg, and Ti. The -concept for quantification of spectral interferences was used. The optimum line selection for trace analysis of a variety of multicomponent matrices requires the choice of prominent lines, which are free or negligibly influenced by line interference problems. The versatility of -concept as basic methodology was experimentally demonstrated in the determination of trace of elements in soil and drinking water. The detection limits are lower in comparison with corresponding threshold concentration levels for soil and drinking water in accordance with environmental regulations. This paper shows the possibilities of present day ICP-OES equipment in the direct determination of trace elements (without preconcentration of impurities in environmental samples.

The matrix effect of biological concomitant element on the signal intensity of Ge, As, and Se in inductively coupled plasma/mass spectrometry

International Nuclear Information System (INIS)

Park, Kyung Su; Kim, Sun Tae; Kim, Young Man; Kim, Yun Je; Lee, Won

2002-01-01

The non-spectroscopic interference effects that occurred in inductively coupled plasma/mass spectrometry were studied for Ge, As and Se in human urine and serum. Many biological samples contain Na, K, Cl and organic compounds, which may cause the enhancement and depression on the analyte signal. The effect of 1% concomitant elements such as N, Cl, S, P, C, Na, and K on a 100 μg/L germanium, arsenic and selenium signal has been investigated by ICP/MS. The interference effects were not in the same direction. It appeared that concomitant elements such as Cl, S and C induce an enhancement effect, whereas N and P did not show any significant effect. And, Na and K caused a depression . We have found a link between the abundance of analytes and the ionization potential of concomitant elements (eV), except carbon and nitrogen

Development of inductively coupled plasma atomic emission spectrometry for palladium and Rhodium determination in platinum-based alloy

International Nuclear Information System (INIS)

Kovacevic, R.; Todorovic, M.; Manojlovic, D.; Mutic, J.

2008-01-01

Inductively coupled plasma atomic emission spectroscopy with internal standardization was applied for the analysis of an in-house reference platinum alloy containing palladium and rhodium (approximately 5% by weight). In order to compensate for variations in signal recovery due to matrix interferences, and therefore to improve the precision, platinum. the major component, was chosen as an internal standard. Quantitative analysis was based on calibration using a set of matrix-matched calibration standards with and without employing the internal standard. These results were compared with those obtained by X-ray fluorescence spectroscopy. The results for both techniques were in a good agreement, although the precision was slightly better in the inductively coupled plasma atomic emission spectroscopy technique, with or without the internal standard

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…

Magnetic immunoassay coupled with inductively coupled plasma mass spectrometry for simultaneous quantification of alpha-fetoprotein and carcinoembryonic antigen in human serum

Science.gov (United States)

Zhang, Xing; Chen, Beibei; He, Man; Zhang, Yiwen; Xiao, Guangyang; Hu, Bin

2015-04-01

The absolute quantification of glycoproteins in complex biological samples is a challenge and of great significance. Herein, 4-mercaptophenylboronic acid functionalized magnetic beads were prepared to selectively capture glycoproteins, while antibody conjugated gold and silver nanoparticles were synthesized as element tags to label two different glycoproteins. Based on that, a new approach of magnetic immunoassay-inductively coupled plasma mass spectrometry (ICP-MS) was established for simultaneous quantitative analysis of glycoproteins. Taking biomarkers of alpha-fetoprotein (AFP) and carcinoembryonic antigen (CEA) as two model glycoproteins, experimental parameters involved in the immunoassay procedure were carefully optimized and analytical performance of the proposed method was evaluated. The limits of detection (LODs) for AFP and CEA were 0.086 μg L- 1 and 0.054 μg L- 1 with the relative standard deviations (RSDs, n = 7, c = 5 μg L- 1) of 6.5% and 6.2% for AFP and CEA, respectively. Linear range for both AFP and CEA was 0.2-50 μg L- 1. To validate the applicability of the proposed method, human serum samples were analyzed, and the obtained results were in good agreement with that obtained by the clinical chemiluminescence immunoassay. The developed method exhibited good selectivity and sensitivity for the simultaneous determination of AFP and CEA, and extended the applicability of metal nanoparticle tags based on ICP-MS methodology in multiple glycoprotein quantifications.

ULTRASONIC NEBULIZATION AND ARSENIC VALENCE STATE CONSIDERATIONS PRIOR TO DETERMINATION VIA INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY

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An ultrasonic nebulizer (USN) was utilized as a sample introduction device for an inductively coupled plasma mass spectrometer in an attempt to increase the sensitivity for As. The USN produced a valence state response difference for As. The As response was suppressed approximate...

Liquid sample introduction in inductively coupled plasma atomic emission and mass spectrometry — Critical review

International Nuclear Information System (INIS)

Bings, N.H.; Orlandini von Niessen, J.O.; Schaper, J.N.

2014-01-01

Inductively coupled plasma optical emission spectroscopy (ICP-OES) and mass spectrometry (ICP-MS) can be considered as the most important tools in inorganic analytical chemistry. Huge progress has been made since the first analytical applications of the ICP. More stable RF generators, improved spectrometers and detection systems were designed along with the achievements gained from advanced microelectronics, leading to overall greatly improved analytical performance of such instruments. In contrast, for the vast majority of cases liquid sample introduction is still based on the pneumatic principle as described in the late 19th century. High flow pneumatic nebulizers typically demand the use of spray chambers as “aerosol filters” in order to match the prerequisites of an ICP. By this, only a small fraction of the nebulized sample actually contributes to the measured signal. Hence, the development of micronebulizers was brought forward. Those systems produce fine aerosols at low sample uptake rates, but they are even more prone for blocking or clogging than conventional systems in the case of solutions containing a significant amount of total dissolved solids (TDS). Despite the high number of publications devoted to liquid sample introduction, it is still considered the Achilles' heel of atomic spectrometry and it is well accepted, that the technology used for liquid sample introduction is still far from ideal, even when applying state-of-the-art systems. Therefore, this review is devoted to offer an update on developments in the field liquid sample introduction that had been reported until the year 2013. The most recent and noteworthy contributions to this field are discussed, trends are highlighted and future directions are outlined. The first part of this review provides a brief overview on theoretical considerations regarding conventional pneumatic nebulization, the fundamentals on aerosol generation and discusses characteristics of aerosols ideally

Liquid sample introduction in inductively coupled plasma atomic emission and mass spectrometry — Critical review

Energy Technology Data Exchange (ETDEWEB)

Bings, N.H., E-mail: bings@uni-mainz.de; Orlandini von Niessen, J.O.; Schaper, J.N.

2014-10-01

Inductively coupled plasma optical emission spectroscopy (ICP-OES) and mass spectrometry (ICP-MS) can be considered as the most important tools in inorganic analytical chemistry. Huge progress has been made since the first analytical applications of the ICP. More stable RF generators, improved spectrometers and detection systems were designed along with the achievements gained from advanced microelectronics, leading to overall greatly improved analytical performance of such instruments. In contrast, for the vast majority of cases liquid sample introduction is still based on the pneumatic principle as described in the late 19th century. High flow pneumatic nebulizers typically demand the use of spray chambers as “aerosol filters” in order to match the prerequisites of an ICP. By this, only a small fraction of the nebulized sample actually contributes to the measured signal. Hence, the development of micronebulizers was brought forward. Those systems produce fine aerosols at low sample uptake rates, but they are even more prone for blocking or clogging than conventional systems in the case of solutions containing a significant amount of total dissolved solids (TDS). Despite the high number of publications devoted to liquid sample introduction, it is still considered the Achilles' heel of atomic spectrometry and it is well accepted, that the technology used for liquid sample introduction is still far from ideal, even when applying state-of-the-art systems. Therefore, this review is devoted to offer an update on developments in the field liquid sample introduction that had been reported until the year 2013. The most recent and noteworthy contributions to this field are discussed, trends are highlighted and future directions are outlined. The first part of this review provides a brief overview on theoretical considerations regarding conventional pneumatic nebulization, the fundamentals on aerosol generation and discusses characteristics of aerosols ideally

The quick and ultrasensitive determination of K in NaI using inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Arnquist, Isaac J., E-mail: isaac.arnquist@pnnl.gov; Hoppe, Eric W.

2017-04-11

A highly sensitive, novel and quick assay method utilizing inductively coupled plasma mass spectrometry was developed for the determination of K in NaI powders and NaI(Tl) scintillator crystals for use in ultralow background applications. The determination of K (viz.{sup 40}K), as well as Th and U and their daughters, is important in ultralow background detector materials to ensure incorporation of materials of sufficiently high radiopurity. Through the use of improved instrumentation, cool plasma operating conditions, and meticulously clean sample preparations, detection limits of 11 fg {sup nat}K g{sup −1} (or 341 pBq {sup 40}K kg{sup −1}) was attained for K in pure water. Detection limits in the sample matrix (i.e., NaI) were 0.529 ng {sup nat}K g NaI{sup −1} (or 16.4 μBq {sup 40}K kg NaI{sup −1}). A number of different precursor NaI powder samples and NaI(Tl) scintillator crystals were assayed for their K content. Determinations ranged from 0.757 to 31.4 ng {sup nat}K g NaI{sup −1}. This method allows for the screening of materials to unprecedented levels in a fraction of the time compared to gamma ray counting techniques, providing a useful method for a more effective screening tool of K in ultralow background detector materials.

Levels of Essential Elements in Different Medicinal Plants Determined by Using Inductively Coupled Plasma Mass Spectrometry

Directory of Open Access Journals (Sweden)

Eid I. Brima

2018-01-01

Full Text Available The objective of this study was to investigate the content of essential elements in medicinal plants in the Kingdom of Saudi Arabia (KSA. Five different medical plants (mahareeb (Cymbopogon schoenanthus, sheeh (Artemisia vulgaris, harjal (Cynanchum argel delile, nabipoot (Equisetum arvense, and cafmariam (Vitex agnus-castus were collected from Madina city in the KSA. Five elements Fe, Mn, Zn, Cu, and Se were determined by using inductively coupled plasma mass spectrometry (ICP-MS. Fe levels were the highest and Se levels were the lowest in all plants. The range levels of all elements in all plants were as follows: Fe 193.4–1757.9, Mn 23.6–143.7, Zn 15.4–32.7, Se 0.13–0.92, and Cu 11.3–21.8 µg/g. Intakes of essential elements from the medical plants in infusion were calculated: Fe 4.6–13.4, Mn 6.7–123.2, Zn 7.0–42.7, Se 0.14–1.5, and Cu 1.5–5.0 µg/dose. The calculated intakes of essential elements for all plants did not exceed the daily intake set by the World Health Organization (WHO and European Food Safety Authority (EFSA. These medicinal plants may be useful sources of essential elements, which are vital for health.

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.

Comparison of ultra-violet and inductively coupled plasma-atomic emission spectrometry for the on-line quantification of selenium species after their separation by reversed-phase liquid chromatography

International Nuclear Information System (INIS)

Tsopelas, Fotios N.; Ochsenkuehn-Petropoulou, Maria Th.; Mergias, Ioannis G.; Tsakanika, Lambrini V.

2005-01-01

An analytical approach for selenium speciation using liquid chromatography (LC) coupled with ultra-violet (UV) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was developed. The separation of the investigated selenium species, selenites, selenates, selenomethionine, selenocystine, selenocystamine and dimethyldiselenide was accomplished in less than 6 min on a BIO Wide Pore RP-18 column using sodium salt of n-octanesulfonic acid as ion-pairing modifier. The on-line detection of the separated selenium species was performed using UV spectrometry at the optimum wavelength of 192 nm, obtained by the UV spectra of the investigated individual selenium species. ICP-AES was also used as element specific on-line detector, after its coupling with the chromatographic system. The UV and ICP-AES detectors were compared for their suitability, including sensitivity and detection limits, for the on-line quantification of the six selenium species. The developed LC-UV as well as LC-ICP-AES techniques were successfully applied to a selenized yeast candidate reference material, after its enzymatic extraction with protease XIV. It was found that the described LC-UV technique is suitable for the determination of selenomethionine, the main selenium compound in the yeast, with an accuracy of 5%, although the UV detector is not element specific and it is rarely used for selenium speciation. This finding can prove valuable for routine laboratories to perform selenium speciation in such materials

Imaging of elements in leaves of tobacco by solid sampling–electrothermal vaporization–inductively coupled plasma-optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Masson, Pierre, E-mail: masson@bordeaux.inra.fr

2014-12-01

Plants take up and store elements according to the environment in which they are growing. Because plants are at the base of the food chain, the determination of essential elements or toxic elements in plant materials is of importance. However, it is assumed that the element content determined on selected tissues may provide more specific information than that derived from the whole plant analysis. In this work, we assessed the feasibility of solid sampling–electrothermal vaporization–inductively coupled plasma-optical emission spectrometry analyses for quantitative imaging of Cd and Mg in plant leaves. Leaves of tobacco (Nicotiana tabacum) were selected to be used as samples. To produce a two dimensional image, sections cut from leaf samples were analyzed. Cellulose doped with multi-element solution standards was used as calibration samples. Two certified reference materials (NIST SRM 1547 Peach Leaves and NIST SRM 1573a Tomato leaves) were used to verify the accuracy of measurements with good agreement between the measured concentrations and the certified values. Quantitative imaging revealed the inhomogeneous distribution of the selected elements. Excess of Cd and Mg tended to be focused on peripheral regions and the tip of the leaf.

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.

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.

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.)

Mass cytometry: technique for real time single cell multitarget immunoassay based on inductively coupled plasma time-of-flight mass spectrometry.

Science.gov (United States)

Bandura, Dmitry R; Baranov, Vladimir I; Ornatsky, Olga I; Antonov, Alexei; Kinach, Robert; Lou, Xudong; Pavlov, Serguei; Vorobiev, Sergey; Dick, John E; Tanner, Scott D

2009-08-15

A novel instrument for real time analysis of individual biological cells or other microparticles is described. The instrument is based on inductively coupled plasma time-of-flight mass spectrometry and comprises a three-aperture plasma-vacuum interface, a dc quadrupole turning optics for decoupling ions from neutral components, an rf quadrupole ion guide discriminating against low-mass dominant plasma ions, a point-to-parallel focusing dc quadrupole doublet, an orthogonal acceleration reflectron analyzer, a discrete dynode fast ion detector, and an 8-bit 1 GHz digitizer. A high spectrum generation frequency of 76.8 kHz provides capability for collecting multiple spectra from each particle-induced transient ion cloud, typically of 200-300 micros duration. It is shown that the transients can be resolved and characterized individually at a peak frequency of 1100 particles per second. Design considerations and optimization data are presented. The figures of merit of the instrument are measured under standard inductively coupled plasma (ICP) operating conditions ( 900 for m/z = 159, the sensitivity with a standard sample introduction system of >1.4 x 10(8) ion counts per second per mg L(-1) of Tb and an abundance sensitivity of (6 x 10(-4))-(1.4 x 10(-3)) (trailing and leading masses, respectively) are shown. The mass range (m/z = 125-215) and abundance sensitivity are sufficient for elemental immunoassay with up to 60 distinct available elemental tags. When 500) can be used, which provides >2.4 x 10(8) cps per mg L(-1) of Tb, at (1.5 x 10(-3))-(5.0 x 10(-3)) abundance sensitivity. The real-time simultaneous detection of multiple isotopes from individual 1.8 microm polystyrene beads labeled with lanthanides is shown. A real time single cell 20 antigen expression assay of model cell lines and leukemia patient samples immuno-labeled with lanthanide-tagged antibodies is presented.

Determination of 90Sr and Pu isotopes in contaminated groundwater samples by inductively coupled plasma mass spectrometry

Science.gov (United States)

Zoriy, Miroslav V.; Ostapczuk, Peter; Halicz, Ludwik; Hille, Ralf; Becker, J. Sabine

2005-04-01

A sensitive analytical method for determining the artificial radionuclides 90Sr, 239Pu and 240Pu at the ultratrace level in groundwater samples from the Semipalatinsk Test Site area in Kazakhstan by double-focusing sector field inductively coupled plasma mass spectrometry (ICP-SFMS) was developed. In order to avoid possible isobaric interferences at m/z 90 for 90Sr determination (e.g. 90Zr+, 40Ar50Cr+, 36Ar54Fe+, 58Ni16O2+, 180Hf2+, etc.), the measurements were performed at medium mass resolution under cold plasma conditions. Pu was separated from uranium by means of extraction chromatography using Eichrom TEVA resin with a recovery of 83%. The limits of detection for 90Sr, 239Pu and 240Pu in water samples were determined as 11, 0.12 and 0.1 fg ml-1, respectively. Concentrations of 90Sr and 239Pu in contaminated groundwater samples ranged from 18 to 32 and from 28 to 856 fg ml-1, respectively. The 240Pu/239Pu isotopic ratio in groundwater samples was measured as 0.17. This isotope ratio indicates that the most probable source of contamination of the investigated groundwater samples was the nuclear weapons tests at the Semipalatinsk Test Site conducted by the USSR in the 1960s.

Quantitative characterization of gold nanoparticles by field-flow fractionation coupled online with light scattering detection and inductively coupled plasma mass spectrometry.

Science.gov (United States)

Schmidt, Bjørn; Loeschner, Katrin; Hadrup, Niels; Mortensen, Alicja; Sloth, Jens J; Koch, Christian Bender; Larsen, Erik H

2011-04-01

An analytical platform coupling asymmetric flow field-flow fractionation (AF(4)) with multiangle light scattering (MALS), dynamic light scattering (DLS), and inductively coupled plasma mass spectrometry (ICPMS) was established and used for separation and quantitative determination of size and mass concentration of nanoparticles (NPs) in aqueous suspension. Mixtures of three polystyrene (PS) NPs between 20 and 100 nm in diameter and mixtures of three gold (Au) NPs between 10 and 60 nm in diameter were separated by AF(4). The geometric diameters of the separated PS NPs and the hydrodynamic diameters of the Au and PS NPs were determined online by MALS and DLS, respectively. The three separated Au NPs were quantified by ICPMS and recovered at 50-95% of the injected masses, which ranged between approximately 8-80 ng of each nanoparticle size. Au NPs adhering to the membrane in the separation channel was found to be a major cause for incomplete recoveries. The lower limit of detection (LOD) ranged between 0.02 ng Au and 0.4 ng Au, with increasing LOD by increasing nanoparticle diameter. The analytical platform was applied to characterization of Au NPs in livers of rats, which were dosed with 10 nm, 60 nm, or a mixture of 10 and 60 nm nanoparticles by intravenous injection. The homogenized livers were solubilized in tetramethylammonium hydroxide (TMAH), and the recovery of Au NPs from the livers amounted to 86-123% of their total Au content. In spite of successful stabilization with bovine serum albumin even in alkaline medium, separation of the Au NPs by AF(4) was not possible due to association with undissolved remains of the alkali-treated liver tissues as demonstrated by electron microscopy images.

Evaluating the accuracy of uranium isotope amount ratio measurements performed by a quadrupole and a multi-collector magnetic sector inductively coupled plasma mass spectrometers for nuclear safeguards

International Nuclear Information System (INIS)

Pereira de Oliveira, O. Jr.; Sarkis, J.E.S.; Ponzevera, E.; Alonso, A.; De Bolle, W.; Quetel, C.

2008-01-01

The n(U 235 )/n(U 238 ) isotope amount ratio in a set of samples was measured using two modern analytical techniques: quadrupole inductively coupled plasma mass spectrometry (ICP-QMS) and multi-collector magnetic sector inductively coupled plasma mass spectrometry (MC-ICPMS). The measured ratios were compared to the certified ratios provided by the high accuracy gas source mass spectrometry (GSMS). The components of the uncertainty were identified and their contribution to the combined standard uncertainty was estimated using the recommendations of the ISO-GUM guide. The values of the measurement uncertainty and bias were determined and then compared to the International Target Values for Measurement Uncertainties in Safeguarding Nuclear Materials. It appears that only the measurements performed by MC-ICPMS can meet the stringent requirements of international nuclear safeguards. (authors)

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.

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.

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.

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.

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

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.; Bowles, C.J.; Farrar, Y.J.; Warner, I.M.

1990-01-01

Current Australian legislation specifies the maximum permitted levels of nine toxic elements in foods while the National Health and Medical Research Council (NH and NRC) 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 NRC 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 and radiochemical neutron activation analysis and inductively coupled plasma mass spectrometry. 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 NRC. (author). 11 refs, 22 figs, 17 tabs

A rapid monitoring method for inorganic arsenic in rice flour using reversed phase-high performance liquid chromatography-inductively coupled plasma mass spectrometry.

Science.gov (United States)

Narukawa, Tomohiro; Chiba, Koichi; Sinaviwat, Savarin; Feldmann, Jörg

2017-01-06

A new rapid monitoring method by means of high performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS) following the heat-assisted extraction was developed for measurement of total inorganic arsenic species in rice flour. As(III) and As(V) eluted at the same retention time and completely separated from organoarsenic species by an isocratic elution program on a reversed phase column. Therefore, neither ambiguous oxidation of arsenite to arsenate nor the integration of two peaks were necessary to determine directly the target analyte inorganic arsenic. Rapid injection allowed measuring 3 replicates within 6min and this combined with a quantitative extraction of all arsenic species from rice flour by a 15min HNO 3 -H 2 O 2 extraction makes this the fastest laboratory based method for inorganic arsenic in rice flour. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

Macro- and micro-element analysis in milk samples by inductively coupled plasma-optical emission spectrometry

Directory of Open Access Journals (Sweden)

Petrović Sanja M.

2016-01-01

Full Text Available The paper describes the determination of Ag, Al, B, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Na, Ni, Pb, Sr, Tl and Zn, as well as total fat content of milk samples, originated from different sources. The analyzed milk samples were: human milk, fresh cow milk, pasteurized cow milk from a local market, and reconstituted powder milk. The milk samples were obtained from Jablanica District (Serbia territory. Preparation of samples for macro- and micro-analyses was done by wet digestion. Concentrations of the elements after digestion were determined by inductively coupled plasma optical emission spectrometry (ICP-OES. Total fat content of milk samples was determinate by the Weibull and Stoldt method. The results showed that potassium and calcium concentrations were the highest in all samples: 1840.64 - 2993.26 mg/L and 456.05 - 1318.08 mg/L, respectively. Of all heavy metals from the examined milk samples (copper, zinc, manganese, nickel, cadmium, and lead, the most common were zinc and copper, with approximately similar content in the range of 5 - 12 mg/l, while cadmium nickel and manganese were not detected at all. Samples of fresh cow milk and human milk showed the highest fat content of 3.6 and 4.2 %, respectively. Results for total fat and macro- and micro-analyses showed that fresh cow milk has the highest contents of fat and calcium, making it the most nutritious. [Projekat Ministarstva nauke Republike Srbije, br. TR 34012

Standard test method for isotopic abundance analysis of uranium hexafluoride and uranyl nitrate solutions by multi-collector, inductively coupled plasma-mass spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2014-01-01

1.1 This test method covers the isotopic abundance analysis of 234U, 235U, 236U and 238U in samples of hydrolysed uranium hexafluoride (UF6) by inductively coupled plasma source, multicollector, mass spectrometry (ICP-MC-MS). The method applies to material with 235U abundance in the range of 0.2 to 6 % mass. This test method is also described in ASTM STP 1344. 1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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.

Effect of inter-tissue inductive coupling on multi-frequency imaging of intracranial hemorrhage by magnetic induction tomography

Science.gov (United States)

Xiao, Zhili; Tan, Chao; Dong, Feng

2017-08-01

Magnetic induction tomography (MIT) is a promising technique for continuous monitoring of intracranial hemorrhage due to its contactless nature, low cost and capacity to penetrate the high-resistivity skull. The inter-tissue inductive coupling increases with frequency, which may lead to errors in multi-frequency imaging at high frequency. The effect of inter-tissue inductive coupling was investigated to improve the multi-frequency imaging of hemorrhage. An analytical model of inter-tissue inductive coupling based on the equivalent circuit was established. A set of new multi-frequency decomposition equations separating the phase shift of hemorrhage from other brain tissues was derived by employing the coupling information to improve the multi-frequency imaging of intracranial hemorrhage. The decomposition error and imaging error are both decreased after considering the inter-tissue inductive coupling information. The study reveals that the introduction of inter-tissue inductive coupling can reduce the errors of multi-frequency imaging, promoting the development of intracranial hemorrhage monitoring by multi-frequency MIT.

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.

Determination of minor and trace elements in aromatic spices by micro-wave assisted digestion and inductively coupled plasma-mass spectrometry.

Science.gov (United States)

Khan, Naeem; Choi, Ji Yeon; Nho, Eun Yeong; Jamila, Nargis; Habte, Girum; Hong, Joon Ho; Hwang, In Min; Kim, Kyong Su

2014-09-01

This study aimed at analyzing the concentrations of 23 minor and trace elements in aromatic spices by inductively coupled plasma-mass spectrometry (ICP-MS), after wet digestion by microwave system. The analytical method was validated by linearity, detection limits, precision, accuracy and recovery experiments, obtaining satisfactory values in all cases. Results indicated the presence of variable amounts of both minor and trace elements in the selected aromatic spices. Manganese was high in cinnamon (879.8 μg/g) followed by cardamom (758.1 μg/g) and clove (649.9 μg/g), strontium and zinc were high in ajwain (489.9 μg/g and 84.95 μg/g, respectively), while copper was high in mango powder (77.68 μg/g). On the whole some of the minor and essential trace elements were found to have good nutritional contribution in accordance to RDA. The levels of toxic trace elements, including As, Cd, and Pb were very low and did not found to pose any threat to consumers. Copyright © 2014 Elsevier Ltd. All rights reserved.

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.

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

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.

Preconcentration of heavy metals on activated carbon and their determination in fruits by inductively coupled plasma optical emission spectrometry.

Science.gov (United States)

Feist, Barbara; Mikula, Barbara

2014-03-15

A method of separation and preconcentration of cadmium, cobalt, copper, nickel, lead, and zinc at trace level using activated carbon is proposed. Activated carbon with the adsorbed trace metals was mineralised using a high-pressure microwave mineraliser. The heavy metals were determined after preconcentration by inductively coupled plasma optical emission spectrometry (ICP-OES). The influence of several parameters, such as pH, sorbent mass, shaking time was examined. Moreover, effects of inorganic matrix on recovery of the determined elements were studied. The experiment shows that foreign ions did not influence recovery of the determined elements. The detection limits (DL) of Cd, Co, Cu, Ni, Pb, and Zn were 0.17, 0.19, 1.60, 2.60, 0.92 and 1.50 μg L(-)(1), respectively. The recovery of the method for the determined elements was better than 95% with relative standard deviation from 1.3% to 3.7%. The preconcentration factor was 80. The proposed method was applied for determination of Cd, Co, Cu, Ni, Pb, and Zn in fruits materials. Accuracy of the proposed method was verified using certified reference material (NCS ZC85006 Tomato). Copyright © 2013 Elsevier Ltd. All rights reserved.

High levels of heavy metal accumulation in dental calculus of smokers: a pilot inductively coupled plasma mass spectrometry study.

Science.gov (United States)

Yaprak, E; Yolcubal, I; Sinanoğlu, A; Doğrul-Demiray, A; Guzeldemir-Akcakanat, E; Marakoğlu, I

2017-02-01

Various trace elements, including toxic heavy metals, may exist in dental calculus. However, the effect of environmental factors on heavy metal composition of dental calculus is unknown. Smoking is a major environmental source for chronic toxic heavy metal exposition. The aim of this study is to compare toxic heavy metal accumulation levels in supragingival dental calculus of smokers and non-smokers. A total of 29 supragingival dental calculus samples were obtained from non-smoker (n = 14) and smoker (n = 15) individuals. Subjects with a probability of occupational exposure were excluded from the study. Samples were analyzed by inductively coupled plasma mass spectrometry in terms of 26 metals and metalloids, including toxic heavy metals. Toxic heavy metals, arsenic (p 0.05). Within the limitations of this study, it can be concluded that the elementary composition of dental calculus may be affected by environmental factors such as tobacco smoke. Therefore, dental calculus may be utilized as a non-invasive diagnostic biological material for monitoring chronic oral heavy metal exposition. However, further studies are required to evaluate its diagnostic potential. © 2016 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

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

International Nuclear Information System (INIS)

Krystek, P.; 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 system was chosen. The methodical set-up was optimized to achieve the best precision for both the isotope ratio and the total uranium concentration in the urine matrix.Three spiked urine samples from an European interlaboratory comparison were analyzed to determine the 235 U/ 238 U isotope ratio. The ratio was found to be in the range 0.002116 to 0.007222, the latter being the natural uranium isotope ratio. The first ratio indicates the abundance of depleted uranium.The effect of storage conditions and the stability for the matrix urine were investigated by using ''real-life'' urine samples from unexposed persons in the Netherlands. For samples stored under refrigeration and acidified the results (range 0.8 to 5.3 ng L -1 U) were in the normal fluctuation range whereas a decrease in uranium concentration was observed for samples stored at room temperature without acidification. (orig.)

Determination of the elemental composition of ferromanganese formations certified reference materials by mass-spectrometry with inductively coupled plasma

Directory of Open Access Journals (Sweden)

N. V. Zarubina

2014-01-01

Full Text Available Contents of 41 elements in the Russian standard samples of ferromanganese nodules OOPE 601, OOPE 602, OOPE 603 and ore crust OOPE 604 were identified by mass-spectrometry with inductively-coupled plasma. Content of W was firstly presented in the sample OOPE-603. Relative standard deviation for most elements was in the range of 3-10%. A description of ICP-MS technique including sample preparation procedure and other instrumental parameters were given as well as analysis of ferromanganese nodules standard samples NOD-A-1 and NOD-P-1 of U.S. Geological Survey was demonstrated for validation. Normalized to chondrite distribution curves of REE in the studied samples were shown as an indicator of the internal consistency offound concentrations. The available literature data on the content of a wide range of elements and its comparison with the matter obtained by us was produced. Measured contents of elements in the established CRM may be useful in the analytical practice to evaluate precision of results. There is a lack of relevant information on a variety of geochemically important elements in the Russian standard samples of OOPE series and the new data can be taken into account in their certification.

Elemental ratios for characterization of quantum-dots populations in complex mixtures by asymmetrical flow field-flow fractionation on-line coupled to fluorescence and inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Menendez-Miranda, Mario; Fernandez-Arguelles, Maria T.; Costa-Fernandez, Jose M.; Encinar, Jorge Ruiz; Sanz-Medel, Alfredo

2014-01-01

Highlights: • The hyphenated system allows unequivocal identification of nanoparticle populations. • AF4 separation permitted detection of unexpected nanosized species in a sample. • ICP-QQQ provides elemental ratios with adequate accuracy in every nanoparticle. • Purity and chemical composition of different quantum dot samples were assessed. - Abstract: Separation and identification of nanoparticles of different composition, with similar particle diameter, coexisting in heterogeneous suspensions of polymer-coated CdSe/ZnS quantum dots (QDs) have been thoroughly assessed by asymmetric flow field-flow fractionation (AF4) coupled on-line to fluorescence and inductively coupled plasma mass spectrometry (ICPMS) detectors. Chemical characterization of any previously on-line separated nanosized species was achieved by the measurement of the elemental molar ratios of every element involved in the synthesis of the QDs, using inorganic standards and external calibration by flow injection analysis (FIA). Such elemental molar ratios, strongly limited so far to pure single nanoparticles suspensions, have been achieved with adequate accuracy by coupling for the first time an ICP-QQQ instrument to an AF4 system. This hyphenation turned out to be instrumental to assess the chemical composition of the different populations of nanoparticles coexisting in the relatively complex mixtures, due to its capabilities to detect the hardly detectable elements involved in the synthesis. Interestingly such information, complementary to that obtained by fluorescence, was very valuable to detect and identify unexpected nanosized species, present at significant level, produced during QDs synthesis and hardly detectable by standard approaches

Uranium analysis in urine by inductively coupled plasma dynamic reaction cell mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ejnik, John W. [Northern Michigan University, Chemistry Department, Marquette, MI (United States); Todorov, Todor I.; Mullick, Florabel G.; Centeno, Jose A. [Armed Forces Institute of Pathology (AFIP), Division of Biophysical Toxicology, Washington, DC (United States); Squibb, Katherine; McDiarmid, Melissa A. [University of Maryland, School of Medicine, Baltimore, MD (United States)

2005-05-01

Urine uranium concentrations are the best biological indicator for identifying exposure to depleted uranium (DU). Internal exposure to DU causes an increased amount of urine uranium and a decreased ratio of {sup 235}U/{sup 238}U in urine samples, resulting in measurements that vary between 0.00725 and 0.002 (i.e., natural and depleted uranium's {sup 235}U/{sup 238}U ratios, respectively). A method based on inductively coupled plasma dynamic reaction cell mass spectrometry (ICP-DRC-MS) was utilized to identify DU in urine by measuring the quantity of total U and the {sup 235}U/{sup 238}U ratio. The quantitative analysis was achieved using {sup 233}U as an internal standard. The analysis was performed both with and without the reaction gas oxygen. The reaction gas converted ionized {sup 235}U{sup +} and {sup 238}U{sup +} into {sup 235}UO{sub 2}{sup +} (m/z=267) and {sup 238}UO{sub 2}{sup +} (m/z=270). This conversion was determined to be over 90% efficient. A polyatomic interference at m/z 234.8 was successfully removed from the {sup 235}U signal under either DRC operating conditions (with or without oxygen as a reaction gas). The method was validated with 15 urine samples of known uranium compositions. The method detection limit for quantification was determined to be 0.1 pg U mL{sup -1} urine and an average coefficient of variation (CV) of 1-2% within the sample measurements. The method detection limit for determining {sup 235}U/{sup 238}U ratio was 3.0 pg U mL{sup -1} urine. An additional 21 patient samples were analyzed with no information about medical history. The measured {sup 235}U/{sup 238}U ratio within the urine samples correctly identified the presence or absence of internal DU exposure in all 21 patients. (orig.)

Internal standardization in atomic-emission spectrometry using inductively coupled plasma

International Nuclear Information System (INIS)

Moore, G.L.

1985-01-01

The principle of internal standardization has been used in quantitative analytical emission spectroscopy since 1925 to minimize the errors arising from fluctuations in sample preparation, excitation-source conditions, and detection parameters. Although modern spectroscopic excitation sources are far more stable and electronic detection methods are more precise than before, the system for the introduction of the sample in spectrometric analysis using inductively coupled plasma (ICP) introduces significant errors, and internal standardization can still play a useful role in improving the overall precision of the analytical results. The criteria for the selection of the elements to be used as internal standards in arc and spark spectrographic analysis apply to a much lesser extent in ICP-spectrometric analysis. Internal standardization is recommended for use in routine ICP-simultaneous spectrometric analysis to improve its accuracy and precision and to provide a monitor for the reassurance of the analyst. However, the selection of an unsuitable reference element can result in misuse of the principle of internal standardization and, although internal standardization can be applied when a sequential monochromator is used, the main sources of error will not be minimized

Electrochemical Dissolution of Iridium and Iridium Oxide Particles in Acidic Media: Transmission Electron Microscopy, Electrochemical Flow Cell Coupled to Inductively Coupled Plasma Mass Spectrometry, and X-ray Absorption Spectroscopy Study.

Science.gov (United States)

Jovanovič, Primož; Hodnik, Nejc; Ruiz-Zepeda, Francisco; Arčon, Iztok; Jozinović, Barbara; Zorko, Milena; Bele, Marjan; Šala, Martin; Šelih, Vid Simon; Hočevar, Samo; Gaberšček, Miran

2017-09-13

Iridium-based particles, regarded as the most promising proton exchange membrane electrolyzer electrocatalysts, were investigated by transmission electron microscopy and by coupling of an electrochemical flow cell (EFC) with online inductively coupled plasma mass spectrometry. Additionally, studies using a thin-film rotating disc electrode, identical location transmission and scanning electron microscopy, as well as X-ray absorption spectroscopy have been performed. Extremely sensitive online time-and potential-resolved electrochemical dissolution profiles revealed that Ir particles dissolve well below oxygen evolution reaction (OER) potentials, presumably induced by Ir surface oxidation and reduction processes, also referred to as transient dissolution. Overall, thermally prepared rutile-type IrO 2 particles are substantially more stable and less active in comparison to as-prepared metallic and electrochemically pretreated (E-Ir) analogues. Interestingly, under OER-relevant conditions, E-Ir particles exhibit superior stability and activity owing to the altered corrosion mechanism, where the formation of unstable Ir(>IV) species is hindered. Due to the enhanced and lasting OER performance, electrochemically pre-oxidized E-Ir particles may be considered as the electrocatalyst of choice for an improved low-temperature electrochemical hydrogen production device, namely a proton exchange membrane electrolyzer.

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.

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.

Determination of Pb in river water samples by inductively coupled plasma optical emission spectrometry after ultrasound-assisted co-precipitation with manganese dioxide

International Nuclear Information System (INIS)

Sousa Bispo, Marcia; Santos da Boa Morte, Elane; Korn das Gracas Andrade, Maria; Sena Gomes Teixeira, Leonardo; Korn, Mauro; Costa, Antonio Celso Spinola

2005-01-01

A simple and efficient procedure for separation and pre-concentration using ultrasound-assisted co-precipitation with manganese dioxide was developed for Pb determination by inductively coupled plasma optical emission spectrometry (ICP OES). The optimization process was carried out using a two-level factorial design and a Doehlert matrix. Three variables (i.e. concentration of oxidizing solution-KMnO 4 , concentration of MnSO 4 solution and time of ultrasonic irradiation) were used as factors in the optimization. The recoveries, based on the analysis of spiked samples, were between 90% and 105%, and the precision was ≤ 5%. The detection limit and quantification limit for Pb determination were 3.2 and 10.7 μg L -1 , respectively. The proposed method was applied for the determination of Pb in water samples from a river heavily polluted by industrial effluents. The recovery measured by analyte addition technique showed that the proposed pre-concentration method had good accuracy

Curve resolution and figures of merit estimation for determination of trace elements in geological materials by inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Lorber, A.; Harel, A.; Goldbart, Z.; Brenner, I.B.

1987-01-01

In geochemical analysis using inductively coupled plasma atomic emission spectrometry (ICP-AES), spectral interferences and background enhancement in response to sample concomitants are the main cause of deterioration of the limit of detection (LOD) and inaccuracy of the determination at the trace and minor element levels. In this account, the authors describe the chemometric procedure of curve resolution for compensating for these sources of error. A newly developed method for calculating figures of merit is used to evaluate the correction procedure, test the statistical significance of the determined concentration, and determine LODs for each sample. The technique involves scanning the vicinity of the spectral line of the analyte. With prior knowledge of potential spectral interferences, deconvolution of the overlapped response is possible. Analytical data for a wide range of geological standard reference materials demonstrate the effectiveness of the chemometric techniques. Separation of 0.002 nm spectral coincidence, employing a 0.02 nm resolution spectrometer, is demonstrated

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.

Application of direct solid sample analysis for the determination of chlorine in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Santos de Gois, Jefferson; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); Welz, Bernhard [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil); Borges, Daniel L.G., E-mail: daniel.borges@ufsc.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil)

2015-03-01

This work describes a methodology developed to carry out Cl determination in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry and direct solid sample analysis. The solid samples were directly weighed into graphite ‘cups’ and inserted into the graphite furnace. The RF power and the carrier gas flow rate were optimized at 1300 W and 0.7 L min{sup −1}, respectively. Calibration could be carried out using aqueous standard solutions with pre-dried modifiers (Pd + Nd or Pd + Ca) or using solid certified reference materials with the same pre-dried modifiers or without the use of modifiers. The limit of quantification was determined as 5 μg g{sup −1} under optimized conditions and the Cl concentration was determined in five certified reference materials with certified concentrations for Cl, in addition to three certified reference materials, for which certified values for Cl were unavailable; in the latter case, the results were compared with those obtained using high-resolution continuum source molecular absorption spectrometry. Good agreement at a 95% statistical confidence level was achieved between determined and certified or reference values. - Highlights: • Direct determination of chlorine in solid biological materials is described for the first time using ICP-MS. • Calibration against aqueous standards is feasible. • The method is accurate and sensitive, regardless of the composition of the solid sample.

Analysis of Trace Elements in Rat Bronchoalveolar Lavage Fluid by Inductively Coupled Plasma Mass Spectrometry.

Science.gov (United States)

Qamar, Wajhul; Al-Ghadeer, Abdul Rahman; Ali, Raisuddin; Abuelizz, Hatem A

2017-08-01

The main objective was to determine the elemental profile of the lung lining fluid of rats which are used as model animals in various experiments. Lung lining fluid elemental constitution obtained after bronchoalveolar lavage fluid (BALF) was analyzed by inductively coupled plasma mass spectrometry (ICP-MS) to determine the biological trace elements along with calcium and magnesium. BALF was collected from healthy rats using a tracheal cannula. However, cells in BALF were counted to monitor any underlying inflammatory lung condition. Cell free BALF samples were processed and analyzed for the elements including magnesium (Mg), calcium (Ca), chromium (Cr), manganese (Mn), iron (Fe), nickel (Ni), copper (Cu), zinc (Zn), selenium (Se), bromine (Br), and iodine (I). In view of this, calcium concentration was the highest (6318.08 ± 3094.3 μg/L) and copper concentration was the lowest (0.89 ± 0.21 μg/L). The detected elements, from high to low concentration, include Ca > Mg > Fe > Br > I > Cr > Ni > Zn > Mn > Se > Cu. Pearson's correlation analysis revealed no significant correlation between cell count and concentration of any of the element detected in BALF. Correlation analysis also revealed significant positive correlation among Fe, I, Cr, Ni, and Mn. Ca was found to be correlated negatively with Cu and positively with Se. Br and Mg found to be positively correlated with each other. Zn remained the only element that was not found to be correlated with any of the elements in the rat BALF.

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.

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)

Styrene and methyl methacrylate copolymer synthesized by RF inductively coupled plasma

Energy Technology Data Exchange (ETDEWEB)

Li, Z; Gillon, X; Diallo, M; Houssiau, L; Pireaux, J-J, E-mail: zhiling.li@fundp.ac.be [University of Namur (FUNDP) Research Centre in Physics of Matter and Radiation (PMR), 61, Rue de Bruxelles, 5000 Namur (Belgium)

2011-01-01

A series of random copolymers of styrene and methyl methacrylate was prepared on a silicon substrate by RF pulsed inductively coupled plasma. The plasma gas phase was investigated by optical emission spectroscopy (OES). The physico-chemical characteristics of the deposited copolymer films were analyzed by several surface techniques: X-ray photoelectron spectroscopy (XPS), Fourier-Transform infrared absorption (FT-IR), Time-of-flight secondary ion mass spectrometry (ToF-SIMS), etc. OES of the plasma and FT-IR spectra of the films are predictive: plasma emitting a higher relative benzyl radical signal results in the deposition of a more aromatic plasma polymer. The functional thin films can be deposited by selection of the co-monomers.

Laser-induced breakdown spectroscopy and inductively coupled plasma-mass spectrometry for determination of Cr in soils from Brits District, South Africa

Directory of Open Access Journals (Sweden)

A. A. Ambushe

2015-10-01

Full Text Available Laser-induced breakdown spectroscopy (LIBS is an emerging analytical technique, which can be used to perform elemental analysis of any material, irrespective of its physical state. In this study, the LIBS technique has been applied for quantification of total Cr in soil samples collected from polluted areas of Brits, North West Province, South Africa. A Q-switched neodymium-yttrium aluminium garnet (Nd-YAG laser (10 Hz, λ = 1064 nm was employed for generation of a laser-induced plasma on the surface of the soil sample. The atomic emission lines were recorded using an Andor Shamrock SR-303i spectrometer, fitted with an intensified charge-coupled device (ICCD camera. Detailed investigation of experimental parameters such as gate delay time, gate width and laser pulse energy was conducted. Soil samples were dried, finely ground, sieved and thereafter pelletized before LIBS analysis. Calibration curve for the quantification of Cr was constructed using certified reference materials of soils and sediments. The concentrations of Cr in soil samples varied from 111 to 3180 mg/kg. In order to test the validity of the LIBS results, inductively coupled plasma-mass spectrometry (ICP-MS was also employed for determination of Cr. The results obtained using LIBS were found to be in good agreement with those of ICP-MS.DOI: http://dx.doi.org/10.4314/bcse.v29i3.3

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

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.

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

A simple method using on-line continuous leaching and ion exchange chromatography coupled to inductively coupled plasma mass spectrometry for the speciation analysis of bio-accessible arsenic in rice.

Science.gov (United States)

Horner, Nolan S; Beauchemin, Diane

2012-03-02

A simple method for the speciation analysis of bio-accessible arsenic (As) in rice was developed using a continuous on-line leaching method to release the bio-accessible fraction. The continuous on-line leaching method has several advantages over commonly used batch methods including quicker and easier sample preparation, reduced risk of contamination and access to real time leaching data. The bio-accessibility of As in the samples was monitored using inductively coupled plasma mass spectrometry (ICP-MS). Results from a certified reference material as well as cooked and uncooked white rice showed that the majority of As was leached by saliva. Results obtained using the continuous on-line leaching method were comparable to those obtained using a batch method. Speciation analysis of the saliva leachate was performed using ion exchange chromatography coupled to ICP-MS. The four most toxic forms of As (As(III), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and As(V)) were clearly separated within 5 min in a single chromatographic run. Over 92% of bio-accessible As in the certified reference material and uncooked white rice sample was in the form of DMA and As(V), whereas it was present as DMA and As(III) in the cooked white rice. Copyright © 2011 Elsevier B.V. All rights reserved.

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

Analysis of cobalt, tantalum, titanium, vanadium and chromium in tungsten carbide by inductively coupled plasma-optical emission spectrometry

CSIR Research Space (South Africa)

Archer, M

2003-12-01

Full Text Available Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used to measure the concentrations of cobalt, tantalum, titanium, vanadium and chromium in solutions of tungsten carbide. The main advantage of the method described here lies...

Ultra-trace determination of gold nanoparticles in environmental water by surfactant assisted dispersive liquid liquid microextraction coupled with electrothermal vaporization-inductively coupled plasma-mass spectrometry

Science.gov (United States)

Liu, Ying; He, Man; Chen, Beibei; Hu, Bin

2016-08-01

A new method by coupling surfactant assisted dispersive liquid liquid microextraction (SA-DLLME) with electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) was proposed for the analysis of gold nanoparticles (AuNPs) in environmental water samples. Effective separation of AuNPs from ionic gold species was achieved by using sodium thiosulphate as a complexing agent. Various experimental parameters affecting SA-DLLME of AuNPs, such as the organic solvent, organic solvent volume, pH of the sample, the kind of surfactant, surfactant concentration, vortex time, speed of centrifugation, centrifugation time, and different coating as well as sizes of AuNPs were investigated carefully. Furthermore, the interference of coexisting ions, dissolved organic matter (DOM) and other metal nanoparticles (NPs) were studied. Under the optimal conditions, a detection limit of 2.2 ng L- 1 and an enrichment factor of 152-fold was achieved for AuNPs, and the original morphology of the AuNPs could be maintained during the extraction process. The developed method was successfully applied for the analysis of AuNPs in environmental water samples, including tap water, the East Lake water, and the Yangtze River water, with recoveries in the range of 89.6-102%. Compared with the established methods for metal NPs analysis, the proposed method has the merits of simple and fast operation, low detection limit, high selectivity, good tolerance to the sample matrix and no digestion or dilution required. It provides an efficient quantification methodology for monitoring AuNPs' pollution in the environmental water and evaluating its toxicity.

Determination of Tributyltin in Seafood Based on Magnetic Molecularly Imprinted Polymers Coupled with High-Performance Liquid Chromatography-Inductively Coupled Plasma Mass Spectrometry

Directory of Open Access Journals (Sweden)

Hua Yang

2017-01-01

Full Text Available In this study, Fe3O4 was adopted as a carrier for surface molecular imprinting with two-stage polymerization. First, the functional monomer (methacrylic acid, MAA was modified on the surface of Fe3O4, which was then polymerized with the template molecule (tributyltin, TBT, cross linking agent (ethylene glycol dimethacrylate, EGDMA, and porogen (acetonitrile, hereby successfully preparing Fe3O4@MIPs prone to specifically identify TBT. The physical properties of Fe3O4@MIPs were then characterized, and adsorption and selection capacities were also assessed. Compared with conventional imprinting polymers, this magnetic molecular imprinting polymer (MIP displayed significantly increased and more specific adsorption. Meanwhile, its pretreatment was simpler and faster due to magnetic separation characteristics. Using magnetic MIPs as adsorbents for enrichment and separation, detection limit, recovery rate, and linear range were 1.0 ng g−1, 79.74–95.72%, and 5 ng g−1~1000 ng g−1, respectively, for a number of seafood samples. High-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS was used to analyze Tegillarca granosa, mussels, large yellow croaker, and other specimens, with recovery rates of 79.74–95.72% and RSD of 1.3%–4.7%. Overall, this method has a shorter total analysis time, lower detection limit, and wider linear range and can be more effectively applied to determine MAA in seawater and seafood.

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

Determination of lead in bone tissues by axially viewed inductively coupled plasma multichannel-based emission spectrometry.

Science.gov (United States)

Grotti, Marco; Abelmoschi, Maria Luisa; Dalla Riva, Simona; Soggia, Francesco; Frache, Roberto

2005-04-01

A new procedure for determining low levels of lead in bone tissues has been developed. After wet acid digestion in a pressurized microwave-heated system, the solution was analyzed by inductively coupled plasma multichannel-based emission spectrometry. Internal standardization using the Co 228.615 nm reference line was chosen as the optimal method to compensate for the matrix effects from the presence of calcium and nitric acid at high concentration levels. The detection limit of the procedure was 0.11 microg Pb g(-1) dry mass. Instrumental precision at the analytical concentration of approximately 10 microg l(-1) ranged from 6.1 to 9.4%. Precision of the sample preparation step was 5.4%. The concentration of lead in SRM 1486 (1.32+/-0.04 microg g(-1)) found using the new procedure was in excellent agreement with the certified level (1.335+/-0.014 microg g(-1)). Finally, the method was applied to determine the lead in various fish bone tissues, and the analytical results were found to be in good agreement with those obtained through differential pulse anodic stripping voltammetry. The method is therefore suitable for the reliable determination of lead at concentration levels of below 1 microg g(-1) in bone samples. Moreover, the multi-element capability of the technique allows us to simultaneously determine other major or trace elements in order to investigate inter-element correlation and to compute enrichment factors, making the proposed procedure particularly useful for investigating lead occurrence and pathways in fish bone tissues in order to find suitable biomarkers for the Antarctic marine environment.

Accurate determination and certification of bromine in plastic by isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Ohata, Masaki; Miura, Tsutomu

2014-01-01

Highlights: • Accurate analytical method of Br in plastic was studied by isotope dilution ICPMS. • A microwave acid digestion using quartz vessel was suitable for Br analysis. • Sample dilution by NH 3 solution could remove memory effect for ICPMS measurement. • The analytical result of the ID-ICPMS showed consistency with that of INAA. • The ID-ICPMS developed could apply to certification of Br in candidate plastic CRM. - Abstract: The accurate analytical method of bromine (Br) in plastic was developed by an isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). The figures of merit of microwave acid digestion procedures using polytetrafluoroethylene (PTFE) or quartz vessels were studied and the latter one was suitable for Br analysis since its material was free from Br contamination. The sample dilution procedures using Milli-Q water or ammonium (NH 3 ) solution were also studied to remove memory effect for ICPMS measurement. Although severe memory effect was observed on Milli-Q water dilution, NH 3 solution could remove it successfully. The accuracy of the ID-ICPMS was validated by a certified reference material (CRM) as well as the comparison with the analytical result obtained by an instrumental neutron activation analysis (INAA) as different analytical method. From these results, the ID-ICPMS developed in the present study could be evaluated as accurate analytical method of Br in plastic materials and it could apply to certification of Br in candidate plastic CRM with respect to such regulations related to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive

Extraction inductively coupled plasma-optical emission spectrometry (ICP-OES). Determination of traces of phosphorus in tungsten

International Nuclear Information System (INIS)

Bauer, G.; Wegscheider, W.; Mueller, K.

1989-01-01

A method for the separation and preconcentration of traces of phosphorus from tungsten was developed. Solid phase extraction of the phosphovanadomolybdate complex performed on a micro-column was applied. Phosphorus was determined by optical emission spectroscopy (OES) with inductively coupled plasma (ICP) excitation. A limit of detection of 0,4 μg/g P with respect to the solid phase is obtained. By directly coupling the extraction/elution step to the ICP instrument a detection limit of 0,06 μg/g P in W was achieved. Besides, the complexity of spectral evaluation in ICP-OES determinations of traces in spectralline-rich matrices is discussed. (Authors)

Comparative oxidation state specific analysis of arsenic species by high-performance liquid chromatography-inductively coupled-mass spectrometry and hydride generation-cryotrapping-atomic absorption spectrometry

Science.gov (United States)

The formation of methylarsonous acid (MAsIII) and dimethylarsinous acid (DMAsIII) in the course of inorganic arsenic (iAs) metabolism plays an important role in the adverse effects of chronic exposure to iAs. High-performance liquid chromatography-inductively coupled plasma-mass ...

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

Standard test method for analysis of urine for uranium-235 and uranium-238 isotopes by inductively coupled plasma-mass spectrometry

CERN Document Server

American Society for Testing and Materials. Philadelphia

2010-01-01

1.1 This test method covers the determination of the concentration of uranium-235 and uranium-238 in urine using Inductively Coupled Plasma-Mass Spectrometry. This test method can be used to support uranium facility bioassay programs. 1.2 This method detection limits for 235U and 238U are 6 ng/L. To meet the requirements of ANSI N13.30, the minimum detectable activity (MDA) of each radionuclide measured must be at least 0.1 pCi/L (0.0037 Bq/L). The MDA translates to 47 ng/L for 235U and 300 ng/L for 238U. Uranium– 234 cannot be determined at the MDA with this test method because of its low mass concentration level equivalent to 0.1 pCi/L. 1.3 The digestion and anion separation of urine may not be necessary when uranium concentrations of more than 100 ng/L are present. 1.4 Units—The values stated in picoCurie per liter units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard. 1....

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.

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)

Diagnostic studies of ion beam formation in inductively coupled plasma

Energy Technology Data Exchange (ETDEWEB)

Jacobs, Jenee L. [Iowa State Univ., Ames, IA (United States)

2015-01-01

This dissertation describes a variety of studies focused on the plasma and the ion beam in inductively coupled plasma mass spectrometry (ICP-MS). The ability to use ICP-MS for measurements of trace elements in samples requires the analytes to be efficiently ionized. Updated ionization efficiency tables are discussed for ionization temperatures of 6500 K and 7000 K with an electron density of 1 x 10¹⁵ cm^-3. These values are reflective of the current operating parameters of ICP-MS instruments. Calculations are also discussed for doubly charged (M²⁺) ion formation, neutral metal oxide (MO) ionization, and metal oxide (MO⁺) ion dissociation for similar plasma temperature values. Ionization efficiency results for neutral MO molecules in the ICP have not been reported previously.

High-precision measurement of variations in calcium isotope ratios in urine by multiple collector inductively coupled plasma mass spectrometry

Science.gov (United States)

Morgan, J.L.L.; Gordon, G.W.; Arrua, R.C.; Skulan, J.L.; Anbar, A.D.; Bullen, T.D.

2011-01-01

We describe a new chemical separation method to isolate Ca from other matrix elements in biological samples, developed with the long-term goal of making high-precision measurement of natural stable Ca isotope variations a clinically applicable tool to assess bone mineral balance. A new two-column procedure utilizing HBr achieves the purity required to accurately and precisely measure two Ca isotope ratios (44Ca/42Ca and 44Ca/43Ca) on a Neptune multiple collector inductively coupled plasma mass spectrometer (MC-ICPMS) in urine. Purification requirements for Sr, Ti, and K (Ca/Sr > 10000; Ca/Ti > 10000000; and Ca/K > 10) were determined by addition of these elements to Ca standards of known isotopic composition. Accuracy was determined by (1) comparing Ca isotope results for samples and standards to published data obtained using thermal ionization mass spectrometry (TIMS), (2) adding a Ca standard of known isotopic composition to a urine sample purified of Ca, and (3) analyzing mixtures of urine samples and standards in varying proportions. The accuracy and precision of δ44/42Ca measurements of purified samples containing 25 μg of Ca can be determined with typical errors less than ±0.2‰ (2σ).

Inductively coupled plasma emission spectrometric detection of simulated high performance liquid chromatographic peaks

International Nuclear Information System (INIS)

Fraley, D.M.; Yates, D.; Manahan, S.E.

1979-01-01

Because of its multielement capability, element-specificity, and low detection limits, inductively coupled plasma optical emission spectrometry (ICP) is a very promising technique for the detection of specific elemental species separated by high performance liquid chromatography (HPLC). This paper evaluated ICP as a detector for HPLC peaks containing specific elements. Detection limits for a number of elements have been evaluated in terms of the minimum detectable concentration of the element at the chromatographic peak maximum. The elements studies were Al, As, B, Ba, Ca, Cd, Co, Cr, Cu, Fe, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Sb, Se, Sr, Ti, V, and Zn. In addition, ICP was compared with atomic absorption spectrometry for the detection of HPLC peaks composed of EDTA and NTA chelates of copper. Furthermore, ICP was compared to uv solution absorption for the detection of copper chelates. 6 figures, 4 tables

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

Determination of uranium from nuclear fuel in environmental samples using inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

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

2000-01-01

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. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on inductively coupled plasma quadrupole mass spectrometry with a hexapole collision cell (HEX-ICP-QMS). The figures of merit of the HEX-ICP-QMS were studied with a plasma-shielded torch using different nebulizers (such as an ultrasonic nebulizer (USN) and Meinhard nebulizer) for solution introduction. A 238 U + ion intensity of up to 27000 MHz/ppm in HEX-ICP-QMS with USN was observed by introducing helium into the hexapole collision cell as the collision gas at a flow rate of 10 ml min -1 . The formation rate of uranium hydride ions UH + /U + of 2 x 10 -6 was obtained by using USN with a membrane desolvator. The limit of 236 U/ 238 U ratio determination in 10 μg 1 -1 uranium solution was 3 x 10 -7 corresponding to the detection limit for 236 U of 3 pg 1 -1 . The precision of uranium isotopic ratio measurements in 10 μg 1 -1 laboratory uranium isotopic standard solution was 0.13% ( 235 U/ 238 U) and 0.33% ( 236 U/ 238 U) using a Meinhard nebulizer and 0.45% ( 235 U/ 238 U) and 0.88% ( 236 U/ 238 U) using a USN. 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 . (orig.)

Trace element determination using static high-sensitivity inductively coupled plasma optical emission spectrometry (SHIP-OES).

Science.gov (United States)

Engelhard, Carsten; Scheffer, Andy; Nowak, Sascha; Vielhaber, Torsten; Buscher, Wolfgang

2007-02-05

A low-flow air-cooled inductively coupled plasma (ICP) design for optical emission spectrometry (OES) with axial plasma viewing is described and an evaluation of its analytical capabilities in trace element determinations is presented. Main advantage is a total argon consumption of 0.6 L min(-1) in contrast to 15 L min(-1) using conventional ICP sources. The torch was evaluated in trace element determinations and studied in direct comparison with a conventional torch under the same conditions with the same OES system, ultrasonic nebulization (USN) and single-element optimization. A variety of parameters (x-y-position of the torch, rf power, external air cooling, gas flow rates and USN operation parameters) was optimized to achieve limits of detection (LOD) which are competitive to those of a conventional plasma source. Ionic to atomic line intensity ratios for magnesium were studied at different radio frequency (rf) power conditions and different sample carrier gas flows to characterize the robustness of the excitation source. A linear dynamic range of three to five orders of magnitude was determined under compromise conditions in multi-element mode. The accuracy of the system was investigated by the determination of Co, Cr, Mn, Zn in two certified reference materials (CRM): CRM 075c (Copper with added impurities), and CRM 281 (Trace elements in rye grass). With standard addition values of 2.44+/-0.04 and 3.19+/-0.21 microg g(-1) for Co and Mn in the CRM 075c and 2.32+/-0.09, 81.8+/-0.4, 32.2+/-3.9 for Cr, Mn and Zn, respectively, were determined in the samples and found to be in good agreement with the reported values; recovery rates in the 98-108% range were obtained. No influence on the analysis by the matrix load in the sample was observed.

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

Methodology for monitoring gold nanoparticles and dissolved gold species in culture medium and cells used for nanotoxicity tests by liquid chromatography hyphenated to inductively coupled plasma-mass spectrometry.

Science.gov (United States)

López-Sanz, Sara; Fariñas, Nuria Rodríguez; Vargas, Rosario Serrano; Martín-Doimeadios, Rosa Del Carmen Rodríguez; Ríos, Ángel

2017-03-01

An analytical methodology based on coupling reversed-phase liquid chromatography (HPLC) to an inductively coupled plasma mass spectrometry (ICP-MS) has been developed for the characterization and identification of gold nanoparticles (AuNPs) and gold dissolved species (Au 3+ ) in culture medium (Dulbecco's Modified Eagle Medium, DMEM) and HeLa cells (a human cervical adenocarcinoma cell line) used in nanotoxicity tests. The influence of the culture medium was also studied and the method applied for nanotoxicity tests. It was also observed that AuNPs can undergo an oxidation process in the supernatants and only a small amount of AuNPs and dissolved Au 3+ was associated with cells. To evaluate the biological impact of AuNPs, a classical viability assay onto HeLa cells was performed using cellular media DMEM in the presence of increasing dosage of 10nm AuNPs. The results showed that 10nm AuNPs exhibit a slight toxic effect. Copyright © 2016 Elsevier B.V. All rights reserved.

Bayesian Integration and Classification of Composition C-4 Plastic Explosives Based on Time-of-Flight-Secondary Ion Mass Spectrometry and Laser Ablation-Inductively Coupled Plasma Mass Spectrometry.

Science.gov (United States)

Mahoney, Christine M; Kelly, Ryan T; Alexander, Liz; Newburn, Matt; Bader, Sydney; Ewing, Robert G; Fahey, Albert J; Atkinson, David A; Beagley, Nathaniel

2016-04-05

Time-of-flight-secondary ion mass spectrometry (TOF-SIMS) and laser ablation-inductively coupled plasma mass spectrometry (LA-ICPMS) were used for characterization and identification of unique signatures from a series of 18 Composition C-4 plastic explosives. The samples were obtained from various commercial and military sources around the country. Positive and negative ion TOF-SIMS data were acquired directly from the C-4 residue on Si surfaces, where the positive ion mass spectra obtained were consistent with the major composition of organic additives, and the negative ion mass spectra were more consistent with explosive content in the C-4 samples. Each series of mass spectra was subjected to partial least squares-discriminant analysis (PLS-DA), a multivariate statistical analysis approach which serves to first find the areas of maximum variance within different classes of C-4 and subsequently to classify unknown samples based on correlations between the unknown data set and the original data set (often referred to as a training data set). This method was able to successfully classify test samples of C-4, though with a limited degree of certainty. The classification accuracy of the method was further improved by integrating the positive and negative ion data using a Bayesian approach. The TOF-SIMS data was combined with a second analytical method, LA-ICPMS, which was used to analyze elemental signatures in the C-4. The integrated data were able to classify test samples with a high degree of certainty. Results indicate that this Bayesian integrated approach constitutes a robust classification method that should be employable even in dirty samples collected in the field.

Direct analysis of ultra-trace semiconductor gas by inductively coupled plasma mass spectrometry coupled with gas to particle conversion-gas exchange technique.

Science.gov (United States)

Ohata, Masaki; Sakurai, Hiromu; Nishiguchi, Kohei; Utani, Keisuke; Günther, Detlef

2015-09-03

An inductively coupled plasma mass spectrometry (ICPMS) coupled with gas to particle conversion-gas exchange technique was applied to the direct analysis of ultra-trace semiconductor gas in ambient air. The ultra-trace semiconductor gases such as arsine (AsH3) and phosphine (PH3) were converted to particles by reaction with ozone (O3) and ammonia (NH3) gases within a gas to particle conversion device (GPD). The converted particles were directly introduced and measured by ICPMS through a gas exchange device (GED), which could penetrate the particles as well as exchange to Ar from either non-reacted gases such as an air or remaining gases of O3 and NH3. The particle size distribution of converted particles was measured by scanning mobility particle sizer (SMPS) and the results supported the elucidation of particle agglomeration between the particle converted from semiconductor gas and the particle of ammonium nitrate (NH4NO3) which was produced as major particle in GPD. Stable time-resolved signals from AsH3 and PH3 in air were obtained by GPD-GED-ICPMS with continuous gas introduction; however, the slightly larger fluctuation, which could be due to the ionization fluctuation of particles in ICP, was observed compared to that of metal carbonyl gas in Ar introduced directly into ICPMS. The linear regression lines were obtained and the limits of detection (LODs) of 1.5 pL L(-1) and 2.4 nL L(-1) for AsH3 and PH3, respectively, were estimated. Since these LODs revealed sufficiently lower values than the measurement concentrations required from semiconductor industry such as 0.5 nL L(-1) and 30 nL L(-1) for AsH3 and PH3, respectively, the GPD-GED-ICPMS could be useful for direct and high sensitive analysis of ultra-trace semiconductor gas in air. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysis of a rhenium-osmium solid-solution spike by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Richardson, J.M.; Dickin, A.P.; McNutt, R.H.; McAndrew, J.I.; Beneteau, S.B.

1989-01-01

The rhenium-osmium decay scheme ( 187 Re → 187 Os) offers a unique opportunity to investigate the genesis of, and directly date, ultramafic rock, sulphide and platinum ore deposits. Inductively coupled plasma mass spectrometry (ICP-MS) is a viable method for Os isotopic analysis as it provides the high temperatures necessary to ionise Os. The sample can be introduced into the ICP mass spectrometer either by conventional nebulisation or by distillation using an Os ''generator''. Generator-mode analysis is superior to nebulisation because (i) the total number of counts is two orders of magnitude higher for a given sample size and (ii) Os oxidises readily to volatile OsO 4 , which has a boiling-point lower than most Re compounds, so that Os can be efficiently separated from 187 Re. The importance of Os loss during sample preparation was minimised by combining the sample powder with a powdered Re-Os isotopic spike prior to any chemical treatment. The spike is in a nickel sulphide matrix and was made by a thioacetamide co-precipitation of Os, Re and Ni followed by a fire assay. The 190 Os/ 192 Os ratio in this preparation is 51.5 ± 0.9, the 187 Os 188 Os ratio is 0.063 ± 0.006 and the 185 Re/ 187 Re ratio is 17.04 - + 0.41. These values are within the error limits quoted by the Oak Ridge National Laboratory and Techsnabexport, the suppliers of the metallic spikes. Parameters that significantly influence the Os analyses include the oxidising agent and the run temperature. The oxidising agent H 5 IO 6 is preferred to H 2 O 2 or HNO 3 as it has the highest electrode potential, provides a prolonged, consistent reaction and is more stable when stored. Chilling the sample and the H 5 IO 6 , initially retards uncontrolled OsO 4 emission. Heat applied later in the run releases OsO 4 and helps maintain a high count rate. Thus, OsO 4 can be generated in a steady, controllable and reproducible manner. (author)

[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.

Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Jia Xiaoyu; Han Yi; Liu Xinli; Duan Taicheng; Chen Hangting

2011-01-01

The dispersive liquid-liquid microextraction (DLLME) combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of mercury in water samples was described. Firstly methylmercury (MeHg + ) and mercury (Hg 2+ ) were complexed with sodium diethyldithiocarbamate, and then the complexes were extracted into carbon tetrachloride by using DLLME. Under the optimized conditions, the enrichment factors of 138 and 350 for MeHg + and Hg 2+ were obtained from only 5.00 mL sample solution. The detection limits of the analytes (as Hg) were 0.0076 ng mL -1 for MeHg + and 0.0014 ng mL -1 for Hg 2+ , respectively. The relative standard deviations for ten replicate measurements of 0.5 ng mL -1 MeHg + and Hg 2+ were 6.9% and 4.4%, respectively. Standard reference material of seawater (GBW(E)080042) was analyzed to verify the accuracy of the method and the results were in good agreement with the certified values. Finally, the developed method was successfully applied for the speciation of mercury in three environmental water samples.

Accurate Determination of Platinum, Palladium, and Rhodium in Ryegrass using Collision Cell Inductively Coupled Plasma Mass Spectrometry with Xenon as Collision Gas

International Nuclear Information System (INIS)

Amr, M.A.

2011-01-01

Inductively coupled plasma mass spectrometry with an octupole collision cell was used for determination of Pt, Pd and Rh in ryegrass (Lolium multiflorum) which was grown hydroponically. Xenon was used as a collision gas to reduce serious polyatomic interferences formed by combination of matrix elements such as CI, Cu, Hf, Sr, Zn, Zr, Y and REE with O, N, C, and Ar. The detection limits for Pt, Pd and Rh in spiked ryegrass are 1.8, 4.2, and 0.8 ppt, respectively. The results for Pt, Pd and Rh in reference materials (NIST SRM 2557, recycled monolith auto catalyst) are in agreement with the certified values. The bioaccumulation of Pt, Pd and Rh by ryegrass grown hydroponically with nutrient solutions containing Pt, Pd and Rh was studied. The obtained results showed that most of the studied metals were accumulated in roots, and only a small fraction was metabolized and transported to leaves. The highest bioaccumulation factors were obtained for Pd and Rh in roots and for Pt in leaves

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)

Determination of tetrabromobisphenol-A/S and their main derivatives in water samples by high performance liquid chromatography coupled with inductively coupled plasma tandem mass spectrometry.

Science.gov (United States)

Liu, Lihong; Liu, Aifeng; Zhang, Qinghua; Shi, Jianbo; He, Bin; Yun, Zhaojun; Jiang, Guibin

2017-05-12

As the most widely used brominated flame retardants (BFRs), Tetrabromobisphenol-A (TBBPA) as well as its alternative Tetrabromobisphenol-S (TBBPS) and their derivatives have raised wide concerns due to their adverse effects on human health and hence the sensitive detection of those BFRs was urgently needed. Herein, a novel analytical method based on high-performance liquid chromatography (HPLC) coupled with inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) has been developed for the determination of TBBPA/S and their derivatives, including TBBPA-bis(2-hydroxyethyl ether) (TBBPA-BHEE), TBBPA-bis(allylether) (TBBPA-BAE), TBBPA-bis(glycidyl ether) (TBBPA-BGE), TBBPA-bis(2,3-dibromopropyl ether) (TBBPA-BDBPE) and TBBPS-bis(2,3-dibromopropyl ether) (TBBPS-BDBPE) in water samples. After optimization, the TBBPA/S and their derivatives, especially the TBBPA-BAE and TBBPA-BDBPE were simultaneously and sensitively quantified by determination of bromine (m/z=79) by using the ICP-MS. The instrument limits of detection (LODs) for the TBBPA, TBBPA-BHEE, TBBPA-BGE, TBBPA-BAE, TBBPA-BDBPE, TBBPS and TBBPS-BDBPE were determined to be 0.12, 0.14, 0.19, 0.14, 0.12, 0.17 and 0.13μgL -1 , respectively, which was close to or much better than the reported methods. The relative standard deviations (RSDs, n=5) of peak area and retention time were better than 2.2% and 0.2% for intra-day analysis, indicating good repeatability and high precision. The proposed method had been successfully applied for the analysis of TBBPA/S and their derivatives in water samples with satisfactory recoveries (67.7%-113%). Copyright © 2017 Elsevier B.V. All rights reserved.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of whole-water recoverable arsenic, boron, and vanadium using inductively coupled plasma-mass spectrometry

Science.gov (United States)

Garbarino, John R.

2000-01-01

Analysis of in-bottle digestate by using the inductively coupled plasma?mass spectrometric (ICP?MS) method has been expanded to include arsenic, boron, and vanadium. Whole-water samples are digested by using either the hydrochloric acid in-bottle digestion procedure or the nitric acid in-bottle digestion procedure. When the hydrochloric acid in-bottle digestion procedure is used, chloride must be removed from the digestate by subboiling evaporation before arsenic and vanadium can be accurately determined. Method detection limits for these elements are now 10 to 100 times lower than U.S. Geological Survey (USGS) methods using hydride generation? atomic absorption spectrophotometry (HG? AAS) and inductively coupled plasma? atomic emission spectrometry (ICP?AES), thus providing lower variability at ambient concentrations. The bias and variability of the methods were determined by using results from spike recoveries, standard reference materials, and validation samples. Spike recoveries in reagent-water, surface-water, ground-water, and whole-water recoverable matrices averaged 90 percent for seven replicates; spike recoveries were biased from 25 to 35 percent low for the ground-water matrix because of the abnormally high iron concentration. Results for reference material were within one standard deviation of the most probable value. There was no significant difference between the results from ICP?MS and HG?AAS or ICP?AES methods for the natural whole-water samples that were analyzed.

Accurate determination and certification of bromine in plastic by isotope dilution inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ohata, Masaki, E-mail: m-oohata@aist.go.jp; Miura, Tsutomu

2014-07-21

Highlights: • Accurate analytical method of Br in plastic was studied by isotope dilution ICPMS. • A microwave acid digestion using quartz vessel was suitable for Br analysis. • Sample dilution by NH{sub 3} solution could remove memory effect for ICPMS measurement. • The analytical result of the ID-ICPMS showed consistency with that of INAA. • The ID-ICPMS developed could apply to certification of Br in candidate plastic CRM. - Abstract: The accurate analytical method of bromine (Br) in plastic was developed by an isotope dilution inductively coupled plasma mass spectrometry (ID-ICPMS). The figures of merit of microwave acid digestion procedures using polytetrafluoroethylene (PTFE) or quartz vessels were studied and the latter one was suitable for Br analysis since its material was free from Br contamination. The sample dilution procedures using Milli-Q water or ammonium (NH{sub 3}) solution were also studied to remove memory effect for ICPMS measurement. Although severe memory effect was observed on Milli-Q water dilution, NH{sub 3} solution could remove it successfully. The accuracy of the ID-ICPMS was validated by a certified reference material (CRM) as well as the comparison with the analytical result obtained by an instrumental neutron activation analysis (INAA) as different analytical method. From these results, the ID-ICPMS developed in the present study could be evaluated as accurate analytical method of Br in plastic materials and it could apply to certification of Br in candidate plastic CRM with respect to such regulations related to RoHS (restriction of the use of hazardous substances in electrical and electronics equipment) directive.

Discrimination of side-window glass of Korean autos by laser ablation inductively coupled plasma mass spectrometry.

Science.gov (United States)

Lee, Sin-Woo; Ryu, Jong-Sik; Min, Ji-Sook; Choi, Man-Yong; Lee, Kwang-Sik; Shin, Woo-Jin

2016-07-15

Fragments of glass from cars are often found at crime scenes and can be crucial evidence for solving the crime. The glass fragments are important as trace evidence at crime scenes related to car accidents and burgled homes. By identifying the origin of glass fragments, it is possible to infer the identity of a suspect. Our results represent a promising approach to a thorough forensic investigation of car glass. Thirty-five samples from the side windows of cars produced and used in South Korea were collected from the official agencies of five car manufacturers and from two glassmakers. In addition, 120 samples from side mirrors were collected from the same suppliers as well as from small businesses. Their chemical compositions (including Pb isotopes) were analyzed using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and linear discriminant analysis (LDA) was performed. The percentages of major elements (Si, Ca, and Fe) in side-window glass varied within narrow ranges (30.0 ± 2.36%, 5.93 ± 0.52%, and 0.33 ± 0.05%, respectively), while the differences among Pb isotope ratios were not significant. In contrast, light rare earth elements (LREEs) were different from each glassmaker. From the LDA, the types of side-window glass were successfully discriminated according to car manufacturer, glassmaker, and even glass thickness. However, glass from side mirrors cannot be used for good forensic identifiers. Discrimination techniques for side-window glass, although not for side mirrors, using chemical compositions combined with multivariate statistical analyses provide evidence for forensic investigations. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Determination of mercury in coal by isotope dilution cold-vapor generation inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Long, S.E.; Kelly, W.R.

2002-04-01

A method based on isotope dilution cold-vapor inductively coupled plasma mass spectrometry (ID-CV-ICPMS) has been developed for high-accuracy determinations of mercury in bituminous and sub-bituminous coals. A closed-system digestion process employing a Carius tube is used to completely oxidize the coal matrix and chemically equilibrate the mercury in the sample with a Hg-201 isotopic spike. The digestates are diluted with high-purity quartz-distilled water, and the mercury is released as a vapor by reduction with tin chloride. Measurements of Hg-201/Hg-202 isotope ratios are made using a quadrupole ICPMS system in time-resolved analysis mode. The new method has some significant advantages over existing methods. The instrument detection limit is less than 1 pg/mL. The average blank (n = 17) is 30 pg, which is roughly 1 order of magnitude lower than the equivalent microwave digestion procedure. The detection limit in coal is blank limited and is similar to 40 pg/g. Memory effects are very low. The relative reproducibility of the analytical measurements is similar to 0.5% for mercury concentrations in the range 10-150 ng/g. The method has been used to measure mercury concentrations in six coal reference materials, SRM 1632b (77.4 ng/g), SRM 1632c (94.3 ng/g), BCR 40 (433.2 ng/g), BCR 180 (125.0 ng/g), BCR 181 (135.8 ng/g), and SARM 20 (252.6 ng/g), as well as a coal fly ash, SRM 1633b (143.1 ng/g). The method is equally applicable to other types of fossil fuels including both crude and refined oils.

Simultaneous determination of arsenic and mercury species in rice by ion-pairing reversed phase chromatography with inductively coupled plasma mass spectrometry.

Science.gov (United States)

Fang, Yong; Pan, Yushi; Li, Peng; Xue, Mei; Pei, Fei; Yang, Wenjian; Ma, Ning; Hu, Qiuhui

2016-12-15

An analytical method using reversed phase chromatography-inductively coupled plasma mass spectrometry for arsenic and mercury speciation analysis was described. The effect of ion-pairing reagent on simultaneous separation of four arsenic (arsenite, arsenate, monomethlyarsonate and dimethylarsinate) and three mercury species (inorganic mercury (Hg(II)), methylmecury and ethylmercury) was investigated. Parameters including concentrations and pH of the mobile phase were optimized. The separation and re-equilibration time was attained within 20min. Meanwhile, a sequential extraction method for arsenic and mercury in rice was tested. Subsequently, 1% HNO3 microwave-assisted extraction was chosen. Calibration curves based on peak area measurements were linear with correlation coefficient greater than 0.9958 for each species in the range studied. The detection limits of the species were in the range of 0.84-2.41μg/L for arsenic and 0.01-0.04μg/L for mercury, respectively. The proposed method was then successfully applied for the simultaneous determination of arsenic and mercury species in rice flour standard material and two kinds of rice from local markets. Copyright © 2016 Elsevier Ltd. All rights reserved.

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)

A novel method for the determination of mercury and selenium in shark tissue using high-resolution inductively coupled plasma-mass spectrometry

International Nuclear Information System (INIS)

Paul, Mitchell C.; Toia, Robert F.; Nagy-Felsobuki, Ellak I. von

2003-01-01

A method for measuring Hg and Se in shark tissue by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) has been developed. Using a matrix of 4% (v/v) aqueous methanol, the spray chamber and transfer tubing memory effects of Hg were significantly reduced. The methanol matrix was able to effectively wash out Hg (10 ppb) and return the signal to blank level in approximately 5 min. This enabled accurate and concomitant measurements of Hg and Se with detection limits (3σ blank signal, n=10) of 26 and 4 ppt, respectively. The recoveries of Hg and Se based on the CRM were 88 and 83%, respectively. The concentrations of Hg and Se in the (liver, muscle, kidney) of a hammerhead shark (dry weight) were (2.65±0.85, 7.09±1.32, 4.43±1.36) and (17.3±4.1, 1.28±0.29, 24.1±5.2) mg kg -1 (where the expanded uncertainty uses a k=2 value) respectively. Multi-elemental semi-quantitative analysis of a hammerhead shark liver, muscle and kidney revealed high levels of Cd, Zn and As

A comparison of continuous pneumatic nebulization and flow injection-direct injection nebulization for sample introduction in inductively coupled plasma-mass spectrometry

International Nuclear Information System (INIS)

Crain, J.S.; Kiely, J.T.

1995-08-01

Dilute nitric acid blanks and solutions containing Ni, Cd, Pb, and U (including two laboratory waste samples) were analyzed eighteen times over a two-month period using inductively coupled plasma-mass spectrometry (ICP-MS). Two different sample introduction techniques were employed: flow injection-direct injection nebulization (FI-DIN) and continuous pneumatic nebulization (CPN). Using comparable instrumental measurement procedures, FI-DIN analyses were 33% faster and generated 52% less waste than CPN analyses. Instrumental limits of detection obtained with FI-DIN and CPN were comparable but not equivalent (except in the case of Pb) because of nebulizer-related differences in sensitivity (i.e., signal per unit analyte concentration) and background. Substantial and statistically significant differences were found between FI-DIN and CPN Ni determinations, and in the case of the laboratory waste samples, there were also small but statistically significant differences between Cd determinations. These small (2 to 3%) differences were not related to polyatomic ion interference (e.g., 95 Mo 16 O + ), but in light of the time savings and waste reduction to be realized, they should not preclude the use of FI-DIN in place of CPN for determination of Cd, Pb, U and chemically

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.

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

Ultracentrifugation and inductively coupled plasma mass spectrometry for metal-protein equilibrium studies

Energy Technology Data Exchange (ETDEWEB)

Arnquist, Isaac J.; Holcombe, James A., E-mail: holcombe@mail.utexas.edu

2012-10-15

The coupling of separation by preparative ultracentrifugation and metal detection by inductively coupled plasma mass spectrometry (ICP-MS) has been explored for metal-protein equilibrium determinations. This study characterizes the stoichiometry as well as apparent (K{sub app}) and intrinsic (K{sub int}) binding affinities of the metal-protein association for a model protein. In particular, the affinity of Cu{sup 2+} for the high affinity binding site in bovine serum albumin (BSA) is determined. Once equilibrium is established between Cu{sup 2+} and BSA, preparative ultracentrifugation moves the metalloprotein away from the meniscus, leaving unbound equilibrium copper in the protein free solution. Since the initial (total) concentrations of purified BSA and Cu{sup 2+} can be determined, the free copper concentration at equilibrium can also be determined by taking a small aliquot above the sedimenting boundary for analysis using ICP-MS. This analysis allows for the determination of free Cu{sup 2+} ion, which is identical to the equilibrium concentration prior to ultracentrifugation. From these data K{sub app} and K{sub int} were determined at two different conditions, 100 mM Tris(hydroxymethyl)aminomethane (Tris) at pH 9.53 and pH 7.93. log K{sub app} values of 17.6 and 14.6 were determined at pH 9.53 and pH 7.93, respectively. Furthermore, pH-independent log K{sub int} values of - 1.43 and - 1.04 were determined at pH 9.53 and 7.93, respectively. While the log K{sub int} at pH 9.53 was in good agreement with literature values obtained from alternative methods, K{sub int} at pH 7.93 was about 2.5 Multiplication-Sign larger than previously reported. BSA undergoes a structural rearrangement between pH 7-9, and the generally accepted pH-dependency of protein tertiary structure may be responsible for the variations in the 'intrinsic' binding constant. The Cu-BSA binding affinity was also monitored in 100 mM Tris 0.1% sodium dodecyl sulfate (SDS) solution at p

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

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.

Inductively coupled plasma-atomic emission spectrometry: analytical assessment of the technique at the beginning of the 90's

International Nuclear Information System (INIS)

Sanz-Medel, A.

1991-01-01

The main application of the inductively coupled plasma (ICP) today is in atomic emission spectroscopy (AES), as an excitation spectrochemical source, although uses of an ICP for fluorescence as just an atomizer, and specially for mass spectrometry, as an ionization source, are rocketing in the last few years. Since its inception, only a quarter of a century ago, ICP-AES has rapidly evolved to one of the preferred routine analytical techniques for convenient determination of many elements with high speed, at low levels and in the most varied samples. Perhaps its comparatively high kinetic temperature (capable of atomizing virtually every compound of any sample), its high excitation and ionization temperatures, and its favourable spatial structure at the core of the ICP success. By now, the ICP-AES can be considered as having achieved maturity in that a huge amount of analytical problems can be tackled with this technique, while no major or fundamental changes have been adopted for several years. Despite this fact, important driving forces are still in operation to further improve the ICP-AES sensitivity, selectivity, precision, sample throughput, etc. Moreover, proposals to extend the scope of the technique to traditionally elusive fields (e.g. non-metals and organic compound analysis) are also appearing in the recent literature. In this paper the 'state of the art', the last developments and the expectations in trying to circumvent the limitations of the ICP-AES (on the light of literature data and personal experience) are reviewed. (author)

A rugged and transferable method for determining blood cadmium, mercury, and lead with inductively coupled plasma-mass spectrometry

International Nuclear Information System (INIS)

McShane, William J.; Pappas, R. Steven; Wilson-McElprang, Veronica; Paschal, Dan

2008-01-01

A simple, high-throughput method for determining total cadmium, mercury, and lead in blood in cases of suspected exposure, using inductively coupled plasma-mass spectrometry (ICP-MS), has been developed and validated. One part matrix-matched standards, blanks, or aliquots of blood specimens were diluted with 49 parts of a solution containing 0.25% (w/w) tetramethylammonium hydroxide; 0.05% v/v Triton X-100 (blood cell membranes and protein solubilization); 0.01% (w/v) ammonium pyrolidinedithiocarbamate (mercury memory effect prevention and oxidation state stabilization, solubilization by complexation of all three metals); 1% v/v isopropanol (signal enhancement); and 10 μg/L iridium (internal standard). Thus the final dilution factor is 1 + 49. The method provides the basis for the determination of total cadmium, mercury, and lead for assessment of environmental, occupational, accidental ingestion or elevated exposures from other means. Approximately 80 specimens, including blanks, calibration standards, and quality control materials can be processed in an 8-h day. The method has been evaluated by examining reference materials from the National Institute of Standards and Technology, as well as by participation in six rounds of proficiency testing intercomparisons led by the Wadsworth Center of the New York State Department of Health. This method was developed for the purpose of increasing U.S. emergency response laboratory capacity. To this end, 33 U.S. state, and 1 district health department laboratories have validated this method in their own laboratories

A rugged and transferable method for determining blood cadmium, mercury, and lead with inductively coupled plasma-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

McShane, William J. [Battelle-Centers for Disease Control and Prevention, Division of Laboratory Sciences, Emergency Response and Air Toxicants Branch, 4770 Buford Highway, MS F-44, Atlanta, GA 30341 (United States)], E-mail: WMcShane@cdc.gov; Pappas, R. Steven [Centers for Disease Control and Prevention, Division of Laboratory Sciences, Emergency Response and Air Toxicants, 4770 Buford Highway, MS F-44, Atlanta, GA 30341 (United States)], E-mail: RPappas@cdc.gov; Wilson-McElprang, Veronica [Battelle-Centers for Disease Control and Prevention, Division of Laboratory Sciences, Emergency Response and Air Toxicants Branch, 4770 Buford Highway, MS F-44, Atlanta, GA 30341 (United States)], E-mail: VWilsonMcelprang@cdc.gov; Paschal, Dan [Centers for Disease Control and Prevention, Division of Laboratory Sciences, Emergency Response and Air Toxicants, 4770 Buford Highway, MS F-44, Atlanta, GA 30341 (United States)], E-mail: DPaschal@cdc.gov

2008-06-15

A simple, high-throughput method for determining total cadmium, mercury, and lead in blood in cases of suspected exposure, using inductively coupled plasma-mass spectrometry (ICP-MS), has been developed and validated. One part matrix-matched standards, blanks, or aliquots of blood specimens were diluted with 49 parts of a solution containing 0.25% (w/w) tetramethylammonium hydroxide; 0.05% v/v Triton X-100 (blood cell membranes and protein solubilization); 0.01% (w/v) ammonium pyrolidinedithiocarbamate (mercury memory effect prevention and oxidation state stabilization, solubilization by complexation of all three metals); 1% v/v isopropanol (signal enhancement); and 10 {mu}g/L iridium (internal standard). Thus the final dilution factor is 1 + 49. The method provides the basis for the determination of total cadmium, mercury, and lead for assessment of environmental, occupational, accidental ingestion or elevated exposures from other means. Approximately 80 specimens, including blanks, calibration standards, and quality control materials can be processed in an 8-h day. The method has been evaluated by examining reference materials from the National Institute of Standards and Technology, as well as by participation in six rounds of proficiency testing intercomparisons led by the Wadsworth Center of the New York State Department of Health. This method was developed for the purpose of increasing U.S. emergency response laboratory capacity. To this end, 33 U.S. state, and 1 district health department laboratories have validated this method in their own laboratories.

Investigations on the direct introduction of cigarette smoke for trace elements analysis by inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Chang, Michael J.; Naworal, John D.; Walker, Kathleen; Connell, Chris T.

2003-01-01

Direct introduction of mainstream cigarette smoke into an inductively coupled plasma mass spectrometry (ICP-MS) has been investigated with respect to its feasibility for on-line analysis of trace elements. An automated apparatus was designed and built interfacing a smoking machine with an ICP-MS for smoke generation, collection, injection and analysis. Major and minor elements present in the particulate phase and the gas phase of mainstream cigarette smoke of 2R4F reference cigarettes have been qualitatively identified by examination of their full mass spectra. This method provides a rapid-screening analysis of the transfer of trace elements into mainstream smoke during cigarette combustion. A full suite of elements present in the whole cigarette smoke has been identified, including As, B, Ba, Br, Cd, Cl, Cs, Cu, Hg, I, K, Li, Mn, Na, Pb, Rb, Sb, Sn, Tl and Zn. Of these elements, the major portions of B, Ba, Cs, Cu, K, Li, Mn, Na, Pb, Rb, Sn, Tl and Zn are present in the particulate phase, whereas the major portion of Hg is present in the gas phase. As, Br, Cd, Cl, I and Sb exist in a distribution between the gas phase and the particulate phase. Depending on the element, the precision of measurement ranges from 5 to 25% in terms of relative standard deviation of peak height and peak area, based on the fourth puff of 2R4F mainstream cigarette smoke analyzed in five smoking replicates

Inorganic mass spectrometry of solid samples

International Nuclear Information System (INIS)

Adams, F.; Vertes, A.

1990-01-01

In this review some recent developments in the field of inorganic mass spectrometry of solids are described with special emphasis on the actual state of understanding of the ionization processes. It concentrates on the common characteristics of methods such as spark source-, laser-, secondary ion-, inductively coupled plasma- and glow discharge mass spectrometry. (orig.)

Use of gradient dilution to flag and overcome matrix interferences in axial-viewing inductively coupled plasma-atomic emission spectrometry

International Nuclear Information System (INIS)

Cheung, Yan; Schwartz, Andrew J.; Hieftje, Gary M.

2014-01-01

Despite the undisputed power of inductively coupled plasma-atomic emission spectrometry (ICP-AES), its users still face serious challenges in obtaining accurate analytical results. Matrix interference is perhaps the most important challenge. Dilution of a matrix-containing sample is a common practice to reduce matrix interference. However, determining the optimal dilution factor requires tedious and time-consuming offline sample preparation, since emission lines and the effect of matrix interferences are affected differently by the dilution. The current study exploits this difference by employing a high-performance liquid chromatography gradient pump prior to the nebulizer to perform on-line mixing of a sample solution and diluent. Linear gradient dilution is performed on both the calibration standard and the matrix-containing sample. By ratioing the signals from two emission lines (from the same or different elements) as a function of dilution factor, the analyst can not only identify the presence of a matrix interference, but also determine the optimal dilution factor needed to overcome the interference. A ratio that does not change with dilution signals the absence of a matrix interference, whereas a changing ratio indicates the presence of an interference. The point on the dilution profile where the ratio stabilizes indicates the optimal dilution factor to correct the interference. The current study was performed on axial-viewing ICP-AES with o-xylene as the solvent

On-line double isotope dilution laser ablation inductively coupled plasma mass spectrometry for the quantitative analysis of solid materials.

Science.gov (United States)

Fernández, Beatriz; Rodríguez-González, Pablo; García Alonso, J Ignacio; Malherbe, Julien; García-Fonseca, Sergio; Pereiro, Rosario; Sanz-Medel, Alfredo

2014-12-03

We report on the determination of trace elements in solid samples by the combination of on-line double isotope dilution and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The proposed method requires the sequential analysis of the sample and a certified natural abundance standard by on-line IDMS using the same isotopically-enriched spike solution. In this way, the mass fraction of the analyte in the sample can be directly referred to the certified standard so the previous characterization of the spike solution is not required. To validate the procedure, Sr, Rb and Pb were determined in certified reference materials with different matrices, including silicate glasses (SRM 610, 612 and 614) and powdered samples (PACS-2, SRM 2710a, SRM 1944, SRM 2702 and SRM 2780). The analysis of powdered samples was carried out both by the preparation of pressed pellets and by lithium borate fusion. Experimental results for the analysis of powdered samples were in agreement with the certified values for all materials. Relative standard deviations in the range of 6-21% for pressed pellets and 3-21% for fused solids were obtained from n=3 independent measurements. Minimal sample preparation, data treatment and consumption of the isotopically-enriched isotopes are the main advantages of the method over previously reported approaches. Copyright © 2014 Elsevier B.V. All rights reserved.

Evaluation of liquid chromatography inductively coupled plasma mass spectrometry for arsenic speciation in water from industrial treatment of shale

Energy Technology Data Exchange (ETDEWEB)

Duarte, Fabio Andrei; Fagundes Pereira, Juliana Severo; Mesko, Marcia Foster; Goldschmidt, Fabiane; Moraes Flores, Erico Marlon de; Dressler, Valderi Luiz, E-mail: valdres@quimica.ufsm.br

2007-09-15

This work describes an arsenic speciation analysis in aqueous effluent from a shale industrial plant using liquid chromatography coupled to inductively coupled plasma mass spectrometry (LC-ICP-MS). Arsenic species have been separated through an anion-exchange column and several parameters investigated, such as retention time, pH, flow rate and concentration of the mobile phase (ammonium carbonate), chloride interference and column conditioning time. The best conditions have been found by fixing the pH of the mobile phase at 8.7. Keeping the mobile phase flow rate at 1.5 ml min{sup -1}, arsenic species were separated by varying the concentration of the mobile phase and the time of elution, as follow: 1.5 mmol l{sup -1} for 10 min, 12 mmol l{sup -1} for 10 min and 20 mmol l{sup -1} for 10 min, respectively. Up to 13 As species present in the samples were separated under these conditions and the following species could be identified and quantified: arsenite [As(III)], dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and arsenate [As(V)]. The limits of detection of the LC-ICP-MS method were 0.02, 0.06, 0.04 and 0.10 {mu}g l{sup -1} of As(III), DMA, MMA, and As(V), respectively. The concentration of these species in the samples were from 3.7 to 6.4 {mu}g l{sup -1}, 6.9 to 13.2 {mu}g l{sup -1}, 100 to 142 {mu}g l{sup -1} and 808 to 1363 {mu}g l{sup -1} for As(III), DMA, MMA and As(V), respectively. The accuracy, evaluated by recovery tests, varied from 94 to 105% and the precision, evaluated by the relative standard deviation was typically lower than 10%.

Determination of rare earth elements, thorium and uranium by inductively coupled plasma mass spectrometry and strontium isotopes by thermal ionization mass spectrometry in soil samples of Bryansk region contaminated due to Chernobyl accident

International Nuclear Information System (INIS)

Sahoo, S.K.; Yonehara, H.; Kurotaki, K.; Shiraishi, K.; Ramzaev, V.; Barkovski, A.

2001-01-01

Inductively coupled plasma mass spectrometric (ICP-MS) determination of rare earth elements (REEs), thorium and uranium in forest, pasture, field and kitchen garden soils from a Russian territory and in certified reference materials (JLK-1, JSD-2 and BCR-1) is described. In addition to concentration data, strontium isotopic composition of the soil samples were measured by thermal ionization mass spectrometry. The measurements contributed to the understanding of the background levels of these elements in an area contaminated due to Chernobyl accident. There was not a significant variation in the concentration of REEs at different depth levels in forest soil samples, however, the ratio of Th/U varied from 3.32 to 3.60. Though concentration of U and Th varied to some extent, the ratio did not show much variation. The value of 87 Sr/ 86 Sr ratio, was in the top layer soil sample relatively higher than in the lower layers. (author)

Magnetic immunoassay coupled with inductively coupled plasma mass spectrometry for simultaneous quantification of alpha-fetoprotein and carcinoembryonic antigen in human serum

Energy Technology Data Exchange (ETDEWEB)

Zhang, Xing; Chen, Beibei; He, Man; Zhang, Yiwen; Xiao, Guangyang; Hu, Bin, E-mail: binhu@whu.edu.cn

2015-04-01

The absolute quantification of glycoproteins in complex biological samples is a challenge and of great significance. Herein, 4-mercaptophenylboronic acid functionalized magnetic beads were prepared to selectively capture glycoproteins, while antibody conjugated gold and silver nanoparticles were synthesized as element tags to label two different glycoproteins. Based on that, a new approach of magnetic immunoassay-inductively coupled plasma mass spectrometry (ICP-MS) was established for simultaneous quantitative analysis of glycoproteins. Taking biomarkers of alpha-fetoprotein (AFP) and carcinoembryonic antigen (CEA) as two model glycoproteins, experimental parameters involved in the immunoassay procedure were carefully optimized and analytical performance of the proposed method was evaluated. The limits of detection (LODs) for AFP and CEA were 0.086 μg L{sup −1} and 0.054 μg L{sup −1} with the relative standard deviations (RSDs, n = 7, c = 5 μg L{sup −1}) of 6.5% and 6.2% for AFP and CEA, respectively. Linear range for both AFP and CEA was 0.2–50 μg L{sup −1}. To validate the applicability of the proposed method, human serum samples were analyzed, and the obtained results were in good agreement with that obtained by the clinical chemiluminescence immunoassay. The developed method exhibited good selectivity and sensitivity for the simultaneous determination of AFP and CEA, and extended the applicability of metal nanoparticle tags based on ICP-MS methodology in multiple glycoprotein quantifications. - Highlights: • 4-Mercaptophenylboronic acid functionalized magnetic beads were prepared and characterized. • ICP-MS based magnetic immunoassay approach was developed for quantification of glycoproteins. • AFP and CEA were quantified simultaneously with Au and Ag NPs as element tags. • The developed method exhibited good selectivity and sensitivity for target glycoproteins.

Determination of rare earth elements in environmental matrices by sector-field inductively coupled plasma mass spectrometry.

Science.gov (United States)

Riondato, J; Vanhaecke, F; Moens, L; Dams, R

2001-07-01

In the framework of an international certification campaign, sector-field inductively coupled plasma mass spectrometry (sector-field ICP-MS) was used for the accurate determination of the rare earth elements in five candidate reference materials: aquatic plant, calcareous soil, mussel tissue, river sediment, and tuna muscle. All samples were taken into solution by use of microwave-assisted or mixed microwave-assisted / open beaker acid digestion. Subsequently, the samples were appropriately diluted and subjected to ICP-MS analysis. Except for Sc, all the elements involved were determined at low mass resolution (R = 300). For Sc, application of a higher resolution setting (R = 3,000) was required to separate the analyte signal from those of several molecular ions which gave rise to spectral overlap at low mass resolution. Some of the heavier REE can also suffer from spectral overlap attributed to the occurrence of oxide ions (MO+) of the lighter REE and Ba. This spectral overlap could be successfully overcome by mathematical correction. Matrix effects were overcome by use of two carefully selected internal standards, such that external calibration could be used. On each occasion, a geological reference material was analyzed as a quality-control sample and the reliability of all results obtained was additionally checked by means of chondrite normalization. For tuna muscle the content of all REE was below the limit of detection. For calcareous soil and river sediment, low to sub microg g(-1) values were observed, whereas the REE content of aquatic plant and mussel tissue was considerably lower (low to sub ng g(-1)). Overall, the results obtained were in excellent agreement with the average values, calculated on the basis of all "accepted" values, obtained in different laboratories using different techniques.

Assessing oral bioaccessibility of trace elements in soils under worst-case scenarios by automated in-line dynamic extraction as a front end to inductively coupled plasma atomic emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Rosende, María [FI-TRACE group, Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa, km 7.5, Palma de Mallorca, Illes Balears E-07122 (Spain); Magalhães, Luis M.; Segundo, Marcela A. [REQUIMTE, Department of Chemistry, Faculty of Pharmacy, University of Porto, R. de Jorge Viterbo Ferreira, 228, Porto 4050-313 (Portugal); Miró, Manuel, E-mail: manuel.miro@uib.es [FI-TRACE group, Department of Chemistry, University of the Balearic Islands, Carretera de Valldemossa, km 7.5, Palma de Mallorca, Illes Balears E-07122 (Spain)

2014-09-09

Highlights: • Automatic oral bioaccessibility tests of trace metals under worst-case scenarios. • Use of intricate and realistic digestive fluids (UBM method). • Analysis of large amounts of soils (≥400 mg) in a flow-based configuration. • Smart interface to inductively coupled plasma atomic emission spectrometry. • Comparison of distinct flow systems mimicking physiological conditions. - Abstract: A novel biomimetic extraction procedure that allows for the in-line handing of ≥400 mg solid substrates is herein proposed for automatic ascertainment of trace element (TE) bioaccessibility in soils under worst-case conditions as per recommendations of ISO norms. A unified bioaccessibility/BARGE method (UBM)-like physiological-based extraction test is evaluated for the first time in a dynamic format for accurate assessment of in-vitro bioaccessibility of Cr, Cu, Ni, Pb and Zn in forest and residential-garden soils by on-line coupling of a hybrid flow set-up to inductively coupled plasma atomic emission spectrometry. Three biologically relevant operational extraction modes mimicking: (i) gastric juice extraction alone; (ii) saliva and gastric juice composite in unidirectional flow extraction format and (iii) saliva and gastric juice composite in a recirculation mode were thoroughly investigated. The extraction profiles of the three configurations using digestive fluids were proven to fit a first order reaction kinetic model for estimating the maximum TE bioaccessibility, that is, the actual worst-case scenario in human risk assessment protocols. A full factorial design, in which the sample amount (400–800 mg), the extractant flow rate (0.5–1.5 mL min{sup −1}) and the extraction temperature (27–37 °C) were selected as variables for the multivariate optimization studies in order to obtain the maximum TE extractability. Two soils of varied physicochemical properties were analysed and no significant differences were found at the 0.05 significance level

Assessing oral bioaccessibility of trace elements in soils under worst-case scenarios by automated in-line dynamic extraction as a front end to inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Rosende, María; Magalhães, Luis M.; Segundo, Marcela A.; Miró, Manuel

2014-01-01

Highlights: • Automatic oral bioaccessibility tests of trace metals under worst-case scenarios. • Use of intricate and realistic digestive fluids (UBM method). • Analysis of large amounts of soils (≥400 mg) in a flow-based configuration. • Smart interface to inductively coupled plasma atomic emission spectrometry. • Comparison of distinct flow systems mimicking physiological conditions. - Abstract: A novel biomimetic extraction procedure that allows for the in-line handing of ≥400 mg solid substrates is herein proposed for automatic ascertainment of trace element (TE) bioaccessibility in soils under worst-case conditions as per recommendations of ISO norms. A unified bioaccessibility/BARGE method (UBM)-like physiological-based extraction test is evaluated for the first time in a dynamic format for accurate assessment of in-vitro bioaccessibility of Cr, Cu, Ni, Pb and Zn in forest and residential-garden soils by on-line coupling of a hybrid flow set-up to inductively coupled plasma atomic emission spectrometry. Three biologically relevant operational extraction modes mimicking: (i) gastric juice extraction alone; (ii) saliva and gastric juice composite in unidirectional flow extraction format and (iii) saliva and gastric juice composite in a recirculation mode were thoroughly investigated. The extraction profiles of the three configurations using digestive fluids were proven to fit a first order reaction kinetic model for estimating the maximum TE bioaccessibility, that is, the actual worst-case scenario in human risk assessment protocols. A full factorial design, in which the sample amount (400–800 mg), the extractant flow rate (0.5–1.5 mL min −1 ) and the extraction temperature (27–37 °C) were selected as variables for the multivariate optimization studies in order to obtain the maximum TE extractability. Two soils of varied physicochemical properties were analysed and no significant differences were found at the 0.05 significance level

Multidimensional chromatography coupled to mass spectrometry in analysing complex proteomics samples

NARCIS (Netherlands)

Horvatovich, Peter; Hoekman, Berend; Govorukhina, Natalia; Bischoff, Rainer

Multidimensional chromatography coupled to mass spectrometry (LC(n)-MS) provides more separation power and an extended measured dynamic concentration range to analyse complex proteomics samples than one dimensional liquid chromatography coupled to mass spectrometry (1D-LC-MS). This review gives an

Low wireless power transfer using inductive coupling for mobile phone charger

International Nuclear Information System (INIS)

Fareq, M; Fitra, M; Irwanto, M; Hasan, Syafruddin; Arinal, M

2014-01-01

A wireless power transfer (WPT) using inductive coupling for mobile phone charger is studied. The project is offer to study and fabricate WPT using inductive coupling for mobile phone charger that will give more information about distance is effect for WPT performance and WPT is not much influenced by the presence of hands, books and types of plastics. The components used to build wireless power transfer can be divided into 3 parts components, the transceiver for power transmission, the inductive coils in this case as the antenna, receiver and the rectifier which act convert AC to DC. Experiments have been conducted and the wireless power transfer using inductive coupling is suitable to be implemented for mobile phone charger.

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

Determination of Cu, Zn, Pb and Cd by atomic emission spectrometry with inductively coupled plasma in waters and sediments from San Juan Ecosystem, Santiago de Cuba

International Nuclear Information System (INIS)

Argota Perez, George; Argota Coello, Humberto; Fernandez-Heredia, Angel

2014-01-01

In this paper the levels of concentration of copper, zinc, lead and cadmium in waters and sediments from the ecosystem San Juan in the Santiago of Cuba province were evaluated. Two sampling of the ecosystem in two stations belonging to the high and middle part of the river, in rainy and little rainy periods were carried out. The conservation and treatment of the samples were developed according to established standards and the determinations of the elements were realized using atomic emission spectrometry with inductively coupled plasma. The concentrations intervals of the studied elements were established so much in the superficial waters like in the sediments and it was demonstrated that exists statistical significant differences for the factors station, period and type of sample, being the middle part of the river, the little rainy period and the sediments, where the grater concentrations of the pollutants appear

Speciation of mercury in water samples by dispersive liquid-liquid microextraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Jia Xiaoyu; Han Yi; Liu Xinli [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China); Graduate School of Chinese Academy of Sciences, Beijing 100039 (China); Duan Taicheng, E-mail: tcduan@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China); Chen Hangting, E-mail: htchen@ciac.jl.cn [State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry, Chinese Academy of Science, Changchun 130022 (China)

2011-01-15

The dispersive liquid-liquid microextraction (DLLME) combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of mercury in water samples was described. Firstly methylmercury (MeHg{sup +}) and mercury (Hg{sup 2+}) were complexed with sodium diethyldithiocarbamate, and then the complexes were extracted into carbon tetrachloride by using DLLME. Under the optimized conditions, the enrichment factors of 138 and 350 for MeHg{sup +} and Hg{sup 2+} were obtained from only 5.00 mL sample solution. The detection limits of the analytes (as Hg) were 0.0076 ng mL{sup -1} for MeHg{sup +} and 0.0014 ng mL{sup -1} for Hg{sup 2+}, respectively. The relative standard deviations for ten replicate measurements of 0.5 ng mL{sup -1} MeHg{sup +} and Hg{sup 2+} were 6.9% and 4.4%, respectively. Standard reference material of seawater (GBW(E)080042) was analyzed to verify the accuracy of the method and the results were in good agreement with the certified values. Finally, the developed method was successfully applied for the speciation of mercury in three environmental water samples.

Certification measurement of the cadmium, copper and lead contents in rice using isotope dilution inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Vassileva, Emilia; Quetel, Christophe R.

2004-01-01

This paper describes the certification of the Cd, Cu and Pb amount contents in a rice material, that were used as reference values for round 19 of the international measurement evaluation programme (IMEP). The protocol developed in this study was based on isotope dilution associated to inductively coupled plasma mass spectrometry (ID-ICP-MS). A multiple spiking approach was applied to reduce significantly the number of analytical steps. For the decomposition of the sample, three different microwave assisted digestion procedures were tested and compared. The use of hydrofluoric acid was found necessary to ensure full solubilisation and complete isotopic equilibration. Estimation of the combined uncertainty attached to the measurement results was performed according to the ISO guidelines. Contributions from the correction for moisture content, sample homogeneity, procedural blank, spike impurities, spectral interferences, instrumental background and dead-time effects were evaluated. SI-traceable values with less than 2% combined uncertainty (k = 2) were obtained for Cd, Cu and Pb, respectively, (14.39 ± 0.21) x 10 -6 mol kg -1 , (44.31 ± 0.42) x 10 -6 mol kg -1 and (2.034 ± 0.034) x 10 -6 mol kg -1 . The rice powder was observed to be highly hygroscopic and a second series of isotope dilution mass spectrometry measurements was carried out on samples in equilibrium with the ambient moisture conditions ('saturated' samples). The Comite Consultatif pour la Quantite de Matiere (CCQM) requested this approach for the participation to the key comparison 24 on the same rice test material. The excellent agreement for Cd between the IMEP-19 reference value, the value submitted by the institute for reference materials and measurements (IRMM) to CCQM-K24 and the corresponding reference value obtained as the arithmetic mean from the results of the 11 participating National Measurement Institutes (less than 0.27% difference) further validated this work. Eventually, this series

Determination of uranium from nuclear fuel in environmental samples using inductively coupled plasma mass spectrometry

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

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. A rapid and sensitive analytical procedure was developed for uranium isotopic ratio measurement in environmental samples based on inductively coupled plasma quadrupole mass spectrometry with a hexapole collision cell (HEX-ICP-QMS). The figures of merit of the HEX-ICP-QMS were studied with a plasma-shielded torch using different nebulizers (such as an ultrasonic nebulizer (USN) and Meinhard nebulizer) for solution introduction. A {sup 238}U{sup +} ion intensity of up to 27000 MHz/ppm in HEX-ICP-QMS with USN was observed by introducing helium into the hexapole collision cell as the collision gas at a flow rate of 10 ml min{sup -1}. The formation rate of uranium hydride ions UH{sup +}/U{sup +} of 2 x 10{sup -6} was obtained by using USN with a membrane desolvator. The limit of {sup 236}U/{sup 238}U ratio determination in 10 {mu}g 1{sup -1} uranium solution was 3 x 10{sup -7} corresponding to the detection limit for {sup 236}U of 3 pg 1{sup -1}. The precision of uranium isotopic ratio measurements in 10 {mu}g 1{sup -1} laboratory uranium isotopic standard solution was 0.13% ({sup 235}U/{sup 238}U) and 0.33% ({sup 236}U/{sup 238}U) using a Meinhard nebulizer and 0.45% ({sup 235}U/{sup 238}U) and 0.88% ({sup 236}U/{sup 238}U) using a USN. 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}. (orig.)

Parallel path nebulizer: Critical parameters for use with microseparation techniques combined with inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Yanes, Enrique G.; Miller-Ihli, Nancy J.

2005-01-01

Four different, low flow parallel path Mira Mist CE nebulizers were evaluated and compared in support of an ongoing project related to the use of microseparation techniques interfaced to inductively coupled plasma mass spectrometry for the quantification of cobalamin species (Vitamin B12). For the characterization of the different Mira Mist CE nebulizers, the nebulizer orientation as well as the effect of methanol on analytical response was the focus of the study. The position of the gas outlet on the nebulizer which consistently provided the maximum signal was when it was rotated to the 11 o'clock position when the nebulizer is viewed end-on. With this orientation the increased signal may be explained by the fact that the cone angle of the aerosol is such that the largest percentage of the aerosol is directed to the center of the spray chamber and consequently into the plasma. To characterize the nebulizer's performance, the signal response of a multielement solution containing elements with a variety of ionization potentials was used. The selection of elements with varying ionization energies and degrees of ionization was essential for a better understanding of observed increases in signal enhancement when methanol was used. Two different phenomena contribute to signal enhancement when using methanol: the first is improved transport efficiency and the second is the 'carbon enhancement effect'. The net result was that as much as a 30-fold increase in signal was observed for As and Mg when using a make-up solution of 20% methanol at a 15 μL/min flow rate which is equivalent to a net volume of 3 μL/min of pure methanol

Microwave assisted extraction of iodine and bromine from edible seaweed for inductively coupled plasma-mass spectrometry determination.

Science.gov (United States)

Romarís-Hortas, Vanessa; Moreda-Piñeiro, Antonio; Bermejo-Barrera, Pilar

2009-08-15

The feasibility of microwave energy to assist the solubilisation of edible seaweed samples by tetramethylammonium hydroxide (TMAH) has been investigated to extract iodine and bromine. Inductively coupled plasma-mass spectrometry (ICP-MS) has been used as a multi-element detector. Variables affecting the microwave assisted extraction/solubilisation (temperature, TMAH volume, ramp time and hold time) were firstly screened by applying a fractional factorial design (2(5-1)+2), resolution V and 2 centre points. When extracting both halogens, results showed statistical significance (confidence interval of 95%) for TMAH volume and temperature, and also for the two order interaction between both variables. Therefore, these two variables were finally optimized by a 2(2)+star orthogonal central composite design with 5 centre points and 2 replicates, and optimum values of 200 degrees C and 10 mL for temperature and TMAH volume, respectively, were found. The extraction time (ramp and hold times) was found statistically non-significant, and values of 10 and 5 min were chosen for the ramp time and the hold time, respectively. This means a fast microwave heating cycle. Repeatability of the over-all procedure has been found to be 6% for both elements, while iodine and bromine concentrations of 24.6 and 19.9 ng g(-1), respectively, were established for the limit of detection. Accuracy of the method was assessed by analyzing the NIES-09 (Sargasso, Sargassum fulvellum) certified reference material (CRM) and the iodine and bromine concentrations found have been in good agreement with the indicative values for this CRM. Finally, the method was applied to several edible dried and canned seaweed samples.

Analytical procedure for characterization of medieval wall-paintings by X-ray fluorescence spectrometry, laser ablation inductively coupled plasma mass spectrometry and Raman spectroscopy

International Nuclear Information System (INIS)

Syta, Olga; Rozum, Karol; Choińska, Marta; Zielińska, Dobrochna; Żukowska, Grażyna Zofia; Kijowska, Agnieszka; Wagner, Barbara

2014-01-01

Analytical procedure for the comprehensive chemical characterization of samples from medieval Nubian wall-paintings by means of portable X-ray fluorescence (pXRF), laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) and Raman spectroscopy (RS) was proposed in this work. The procedure was used for elemental and molecular investigations of samples from archeological excavations in Nubia (modern southern Egypt and northern Sudan). Numerous remains of churches with painted decorations dated back to the 7th–14th century were excavated in the region of medieval kingdoms of Nubia but many aspects of this art and its technology are still unknown. Samples from the selected archeological sites (Faras, Old Dongola and Banganarti) were analyzed in the form of transfers (n = 26), small fragments collected during the excavations (n = 35) and cross sections (n = 15). XRF was used to collect data about elemental composition, LA-ICPMS allowed mapping of selected elements, while RS was used to get the molecular information about the samples. The preliminary results indicated the usefulness of the proposed analytical procedure for distinguishing the substances, from both the surface and sub-surface domains of the wall-paintings. The possibility to identify raw materials from the wall-paintings will be used in the further systematic, archeometric studies devoted to the detailed comparison of various historic Nubian centers. - Highlights: • The analytical procedure for examination of unique wall paintings was proposed. • Identification of pigments and supporting layers of wall-paintings was obtained. • Heterogeneous samples were mapped with the use of LA-ICPMS. • Anatase in the sub-surface regions of samples was detected by Raman spectroscopy

Analytical procedure for characterization of medieval wall-paintings by X-ray fluorescence spectrometry, laser ablation inductively coupled plasma mass spectrometry and Raman spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Syta, Olga; Rozum, Karol; Choińska, Marta [Faculty of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warsaw (Poland); Zielińska, Dobrochna [Institute of Archaeology, University of Warsaw, Krakowskie Przedmieście 26/28, 00-927 Warsaw (Poland); Żukowska, Grażyna Zofia [Chemical Faculty, Warsaw University of Technology, Noakowskiego 3, 00-664 Warsaw (Poland); Kijowska, Agnieszka [National Museum in Warsaw, Aleje Jerozolimskie 3, 00-495 Warsaw (Poland); Wagner, Barbara, E-mail: barbog@chem.uw.edu.pl [Faculty of Chemistry, University of Warsaw, Pasteura 1, 02-093 Warsaw (Poland)

2014-11-01

Analytical procedure for the comprehensive chemical characterization of samples from medieval Nubian wall-paintings by means of portable X-ray fluorescence (pXRF), laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS) and Raman spectroscopy (RS) was proposed in this work. The procedure was used for elemental and molecular investigations of samples from archeological excavations in Nubia (modern southern Egypt and northern Sudan). Numerous remains of churches with painted decorations dated back to the 7th–14th century were excavated in the region of medieval kingdoms of Nubia but many aspects of this art and its technology are still unknown. Samples from the selected archeological sites (Faras, Old Dongola and Banganarti) were analyzed in the form of transfers (n = 26), small fragments collected during the excavations (n = 35) and cross sections (n = 15). XRF was used to collect data about elemental composition, LA-ICPMS allowed mapping of selected elements, while RS was used to get the molecular information about the samples. The preliminary results indicated the usefulness of the proposed analytical procedure for distinguishing the substances, from both the surface and sub-surface domains of the wall-paintings. The possibility to identify raw materials from the wall-paintings will be used in the further systematic, archeometric studies devoted to the detailed comparison of various historic Nubian centers. - Highlights: • The analytical procedure for examination of unique wall paintings was proposed. • Identification of pigments and supporting layers of wall-paintings was obtained. • Heterogeneous samples were mapped with the use of LA-ICPMS. • Anatase in the sub-surface regions of samples was detected by Raman spectroscopy.

Speciation analysis of inorganic arsenic by magnetic solid phase extraction on-line with inductively coupled mass spectrometry determination.

Science.gov (United States)

Montoro Leal, P; Vereda Alonso, E; López Guerrero, M M; Cordero, M T Siles; Cano Pavón, J M; García de Torres, A

2018-07-01

Arsenic, one of the main environmental pollutants and potent natural poison, is a chemical element that is spread throughout the Earth's crust. It is well known that the toxicity of arsenic is highly dependent on its chemical forms. Generally, the inorganic species are more toxic than its organics forms, and As(III) is 60 times more toxic than As(V). In environmental waters, arsenic exists predominantly in two chemical forms: As(III) and As(V). In view of these facts, fast, sensitive, accurate and simple analytical methods for the speciation of inorganic arsenic in environmental waters are required. In this work, a new magnetic solid phase extraction with a hydride generation system was coupled on line with inductively coupled plasma mass spectrometry (MSPE-HG-ICP-MS). The new system was based on the retention of As(III) and As(V) in two knotted reactors filled with (Fe 3 O 4 ) magnetic nanoparticles functionalized with [1,5-bis (2-pyridyl) 3-sulfophenylmethylene] thiocarbonohydrazide (PSTH-MNPs). As(III) and total inorganic As were sequentially eluted in different reduction conditions. The concentration of As(V) was obtained by subtracting As(III) from total As. The system runs in a fully automated way and the method has proved to have a wide linear range and to be precise, sensitive and fast. The detection limits found were 2.7 and 3.2 ng/L for As(III) and total As, respectively; with relative standard deviations (RSDs) of 2.5% and 2.7% and a sample throughput of 14.4 h -1 . In order to validate the developed method, several certified reference samples of environmental waters including sea water, were analyzed and the determined values were in good agreement with the certified values. The proposed method was successfully applied to the speciation analysis of inorganic arsenic in well-water and sea water. Copyright © 2018 Elsevier B.V. All rights reserved.

Simplified sample preparation in the simultaneous measurement of whole blood antimony, bismuth, manganese, and zinc by inductively coupled plasma mass spectrometry.

Science.gov (United States)

Haglock-Adler, Carrie J; Strathmann, Frederick G

2015-02-01

We developed and validated a simplified sample preparation for the analysis of antimony (Sb), bismuth (Bi), manganese (Mn), and zinc (Zn) in whole blood. This simplification included a reduction in sample volume, removal of a lengthy acidic digestion, and optimization of the internal standard. Measurement of Sb, Bi, Mn and Zn in whole blood was conducted using inductively coupled-plasma mass spectrometry. Method performance characteristics, including intra- and inter-assay imprecision, accuracy, linearity, AMR, sensitivity, carryover, sample stability and assay stability were determined in accordance with clinical laboratory standards. In addition, analytical and clinical recoveries were assessed to investigate comparability between goat blood matrix and pooled patient blood. Established assay performance characteristics included inter- and intra-assay imprecision samples, proficiency testing samples, and comparison to an outside reference laboratory. This method overcomes the laborious acidic heat digestion previously used and replaces it with a simplified sample preparation involving an alkaline dilution. The method requires minimal sample preparation with the dilution of alkaline diluent and is validated to quantify Sb and Bi from 1 to 25 μg/L, Mn from 1 to 80 μg/L, and Zn from 50 to 1500 μg/dL in whole blood. Copyright © 2014 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved.

Analysis of rare earth elements in coal fly ash using laser ablation inductively coupled plasma mass spectrometry and scanning electron microscopy

Science.gov (United States)

Thompson, Robert L.; Bank, Tracy; Montross, Scott; Roth, Elliot; Howard, Bret; Verba, Circe; Granite, Evan

2018-05-01

Reference standard NIST SRM 1633b and FA 345, a fly ash sample from an eastern U.S. coal power plant, were analyzed to determine and quantify the mineralogical association of rare earth elements (REE). These analyses were completed using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and a scanning electron microscope, equipped with an energy-dispersive X-ray spectrometer (SEM-EDS). Internal standardization was avoided by quantifying elemental concentrations by normalizing to 100% oxides. Mineral grains containing elevated REE concentrations were found in diverse chemical environments, but were most commonly found in regions where Al and Si were predominant. Dividing the spot analyses into time segments yielded plots that showed the REE content changing over time as individual mineral grains were being ablated. SEM-EDS images of FA 345 confirmed the trends that were found in the LA-ICP-MS results. Small grains of apatite, monazite, or zircon were frequently observed as free mineral grains or embedded in amorphous aluminosilicate glass and were not associated with ferrous particles. This finding is consistent with previous reports that magnetic enrichment may be an effective way of concentrating non-magnetic REE phases. Furthermore, aggressive mechanical and chemical-based separation schemes will be required to separate and recover REE from aluminosilicate glass.

Speciation analysis of tellurium by solid-phase extraction in the presence of ammonium pyrrolidine dithiocarbamate and inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Yu, Chunhai; Cai, Qiantao; Guo, Zhong-Xian; Yang, Zhaoguang [Centre for Advanced Water Technology, Innovation Centre (NTU), Singapore (Singapore); Khoo, Soo Beng [Department of Chemistry, National University of Singapore (Singapore)

2003-05-01

Under acidic conditions tellurium(IV) formed a complex with ammonium pyrrolidine dithiocarbamate (APDC). The tellurium(IV) complex was completely retained on a non-polar Isolute silica-based octadecyl (C{sub 18}) sorbent-containing solid-phase extraction (SPE) cartridge, while the uncomplexed Te(VI) passed through the cartridge and remained as a free species in the solution. Only partial Te(IV) was retained on the SPE cartridge for samples without addition of APDC. On the basis of different retention behaviours of the complexed Te(IV) and uncomplexed Te(VI), a simple and highly sensitive method is proposed for the determination of total tellurium and Te(VI) by SPE separation and inductively coupled plasma mass spectrometry (ICP-MS) detection. The Te(IV) concentration was calculated as the difference between total tellurium and Te(VI) concentrations. The detection limit (3{sigma}) is 3 ng L{sup -1} tellurium. Factors affecting the separation and detection of tellurium species were investigated. Coexisting ions did not show significant interferences with the Te(IV)-APDC complex retention and the subsequent ICP-MS detection of Te. The method has been successfully applied to the tellurium speciation analysis in waters with spiked recoveries for Te(IV) and Te(VI) of 86.0-108% and 87.1-97.4%, respectively. (orig.)

Determination of Se at low concentration in coal by collision/reaction cell technology inductively coupled plasma mass spectrometry

Science.gov (United States)

Henn, Alessandra S.; Rondan, Filipe S.; Mesko, Marcia F.; Mello, Paola A.; Perez, Magali; Armstrong, Joseph; Bullock, Liam A.; Parnell, John; Feldmann, Joerg; Flores, Erico M. M.

2018-05-01

A method is proposed for the determination of selenium at low concentration in coal by collision/reaction cell technology inductively coupled plasma mass spectrometry (CRC-ICP-MS). Samples were decomposed by high pressure microwave-assisted wet digestion (MAWD) using 250 mg of coal, a mixture of 5 mL of 14.4 mol L-1 HNO3 and 1 mL of 40% HF and 70 min of heating program (200 °C and 40 bar). Hydrogen gas used in the collision/reaction cell was investigated to minimize the argon-based interferences at m/z 77, 78 and 80. The rejection parameter (RPq) and the H2 gas flow rate were set to 0.45 and 4.8 mL min-1, respectively. The use of H2 in the cell resulted in other polyatomic interferences, such as 76Ge1H+, 79Br1H+ and 81Br1H+, which impaired Se determination using 77Se, 80Se and 82Se isotopes, thus Se determination was carried out by monitoring only 78Se isotope. Selenium was determined in certified reference materials of coal (NIST 1635 and SARM 20) and an agreement better than 95% was observed between the results obtained by CRC-ICP-MS and the certified values. Under optimized conditions, the instrumental limit of detection was 0.01 μg L-1 and the method limit of detection was 0.01 μg g-1, which was suitable for Se determination at very low concentration in coal.

Direct multielement trace analyses of silicon carbide powders by spark ablation simultaneous inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Kiera, Arne F.; Schmidt-Lehr, Sebastian; Song, Ming; Bings, Nicolas H.; Broekaert, Jose A.C.

2008-01-01

A procedure for the direct analysis of silicon carbide powders (SiC) by simultaneous detection inductively coupled plasma optical emission spectrometry using a Spectro-CIROS TM spectrometer (CCD-ICP-OES) and a novel spark ablation system Spectro-SASSy (SA) as sample introduction technique is described. The sample preparation procedure for SA of non-conducting material is based on mixing the sample powders with a conducting matrix, in this case copper and briquetting pellets. Pressing time, pressure and mixing ratio are shown to be important parameters of the pelleting technique with respect to their mechanical stability for the reliability of the analysis results. A mixing ratio of 0.2 g +0.6 g for SiC and Cu, a pressure of 10 t cm -2 and a pressing time of 8 min have been found optimum. It has also been shown that the spark parameters selected are crucial for uniform volatilization. Electron probe micrographs of the burning spots and the analytical signal magnitude showed that a rather hard spark at 100 Hz was optimum. The determination of trace elements in silicon carbide powders is demonstrated using a calibration based on the addition of standard solutions. For Al, Ti, V, Mn and Fe detection limits in the lower μg g -1 range can be achieved. Internal standardization with Y in combination with the addition of standard solutions allows relative standard deviations in the range of 4 to 24% for concentration levels of the order of 3 to 350 μg g -1

Direct multielement trace analyses of silicon carbide powders by spark ablation simultaneous inductively coupled plasma optical emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Kiera, Arne F.; Schmidt-Lehr, Sebastian; Song, Ming [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany); Bings, Nicolas H. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)], E-mail: bings@chemie.uni-hamburg.de; Broekaert, Jose A.C. [Institute for Inorganic and Applied Chemistry, University of Hamburg, Martin-Luther-King-Platz 6, D-20146 Hamburg (Germany)

2008-02-15

A procedure for the direct analysis of silicon carbide powders (SiC) by simultaneous detection inductively coupled plasma optical emission spectrometry using a Spectro-CIROS{sup TM} spectrometer (CCD-ICP-OES) and a novel spark ablation system Spectro-SASSy (SA) as sample introduction technique is described. The sample preparation procedure for SA of non-conducting material is based on mixing the sample powders with a conducting matrix, in this case copper and briquetting pellets. Pressing time, pressure and mixing ratio are shown to be important parameters of the pelleting technique with respect to their mechanical stability for the reliability of the analysis results. A mixing ratio of 0.2 g +0.6 g for SiC and Cu, a pressure of 10 t cm{sup -2} and a pressing time of 8 min have been found optimum. It has also been shown that the spark parameters selected are crucial for uniform volatilization. Electron probe micrographs of the burning spots and the analytical signal magnitude showed that a rather hard spark at 100 Hz was optimum. The determination of trace elements in silicon carbide powders is demonstrated using a calibration based on the addition of standard solutions. For Al, Ti, V, Mn and Fe detection limits in the lower {mu}g g{sup -1} range can be achieved. Internal standardization with Y in combination with the addition of standard solutions allows relative standard deviations in the range of 4 to 24% for concentration levels of the order of 3 to 350 {mu}g g{sup -1}.

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

A Facile Droplet-Chip-Time-Resolved Inductively Coupled Plasma Mass Spectrometry Online System for Determination of Zinc in Single Cell.

Science.gov (United States)

Wang, Han; Chen, Beibei; He, Man; Hu, Bin

2017-05-02

Single cell analysis is a significant research field in recent years reflecting the heterogeneity of cells in a biological system. In this work, a facile droplet chip was fabricated and online combined with time-resolved inductively coupled plasma mass spectrometry (ICPMS) via a microflow nebulizer for the determination of zinc in single HepG2 cells. On the focusing geometric designed PDMS microfluidic chip, the aqueous cell suspension was ejected and divided by hexanol to generate droplets. The droplets encapsulated single cells remain intact during the transportation into ICP for subsequent detection. Under the optimized conditions, the frequency of droplet generation is 3-6 × 10 6 min -1 , and the injected cell number is 2500 min -1 , which can ensure the single cell encapsulation. ZnO nanoparticles (NPs) were used for the quantification of zinc in single cells, and the accuracy was validated by conventional acid digestion-ICPMS method. The ZnO NPs incubated HepG2 cells were analyzed as model samples, and the results exhibit the heterogeneity of HepG2 cells in the uptake/adsorption of ZnO NPs. The developed online droplet-chip-ICPMS analysis system achieves stable single cell encapsulation and has high throughput for single cell analysis. It has the potential in monitoring the content as well as distribution of trace elements/NPs at the single cell level.

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.

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

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.

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.

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.)

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.)

Spatially and time-resolved element-specific in situ corrosion investigations with an online hyphenated microcapillary flow injection inductively coupled plasma mass spectrometry set-up

International Nuclear Information System (INIS)

Homazava, N.; Ulrich, A.; Kraehenbuehl, U.

2008-01-01

A novel technique for in situ spatial, time-resolved element-specific investigations of corrosion processes is developed. The technique is based on an online hyphenation of a specially designed microflow-capillary set-up to inductively coupled plasma mass spectrometry (ICP-MS) using flow injection sample introduction. Detailed aspects of the method development, optimization of the sample microflow introduction and flow injection characteristics for the localized corrosion analysis are described. Moreover, specific challenges of the ICP-MS analysis as applied to the analysis of corrosion sample probes, e.g. high matrix load and limited sample volume, are discussed. The efficiency of the developed technique is proved by corrosion susceptibility analysis of a commercial Al alloy. Results of the corrosion experiments of the aluminum alloy AA 6111 are presented to demonstrate the influence of various factors such as exposure time and pH value of the corrosive medium on the element-specific dissolution rates of the alloy. This novel technique provides new aspects in corrosion science and sheds new light on corrosion mechanisms

Relationship between the induction frequency and LTE in inductively coupled plasmas

International Nuclear Information System (INIS)

Mostaghimi, J.; Boulos, M.I.

1990-01-01

In this paper, the effect of the induction frequency on the local thermodynamic equilibrium (LTE) conditions in an inductively coupled plasma is investigated. Using generators with frequencies ranging from 5 to 56 MHz, a previous study investigated demonstrated the importance of this effect. Their measurements of the excitation temperatures of the iron atomic lines showed a sharp decrease in this temperature as a result of the increase in frequency. Another conclusion was that, all other parameters constant, increase in frequency will help the promotion of non-LTE effects

Major constituent quantitative determination in uranium alloys by coupled plasma atomic emission spectrometry and X ray fluorescence wavelength dispersive spectrometry

International Nuclear Information System (INIS)

Oliveira, Luis Claudio de; Silva, Adriana Mascarenhas Martins da; Gomide, Ricardo Goncalves; Silva, Ieda de Souza

2013-01-01

A wavelength-dispersive X-ray fluorescence (WD-XRF) spectrometric method for determination of major constituents elements (Zr, Nb, Mo) in Uranium/Zirconium/Niobium and Uranium/Molybdenum alloy samples were developed. The methods use samples taken in the form of chips that were dissolved in hot nitric acid and precipitate particles melted with lithium tetraborate and dissolved in hot nitric acid and finally analyzed as a solution. Studies on the determination by inductively coupled plasma optic emission spectrometry (ICP OES) using matched matrix in calibration curve were developed. The same samples solution were analyzed in both methods. The limits of detection (LOD), linearity of the calibrations curves, recovery study, accuracy and precision of the both techniques were carried out. The results were compared. (author)

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

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

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.

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

Application of laser ablation inductivly coupled plasma mass spectrometry for characterization of U-7Mo/Al-55i dispersion fuels

Energy Technology Data Exchange (ETDEWEB)

Lee, Jeong Mook; Park, Jai Il; Youn, Young Sang; Ha, Yeong Keong; Kim, Jong Yun [Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2017-04-15

This technical note demonstrates the feasibility of using laser ablation inductively coupled plasma mass spectrometry for the characterization of U–7Mo/Al–5Si dispersion fuel. Our measurements show 5.0% Relative Standard Deviation (RSD) for the reproducibility of measured {sup 98}Mo/{sup 238}U ratios in fuel particles from spot analysis, and 3.4% RSD for {sup 98}Mo/{sup 238}U ratios in a NIST-SRM 612 glass standard. Line scanning allows for the distinction of U–7Mo fuel particles from the Al–5Si matrix. Each mass spectrum peak indicates the presence of U–7Mo fuel particles, and the time width of each peak corresponds to the size of that fuel particle. The size of the fuel particles is estimated from the time width of the mass spectrum peak for {sup 98}Mo by considering the scan rate used during the line scan. This preliminary application clearly demonstrates that laser ablation inductively coupled plasma mass spectrometry can directly identify isotope ratios and sizes of the fuel particles in U–Mo/Al dispersion fuel. Once optimized further, this instrument will be a powerful tool for investigating irradiated dispersion fuels in terms of fission product distributions in fuel matrices, and the changes in fuel particle size or shape after irradiation.

The inductively coupled plasma as a source for the measurement of fundamental spectroscopic constants

International Nuclear Information System (INIS)

Farnsworth, P.B.

1993-01-01

Inductively coupled plasmas (ICPs) are stable, robust sources for the generation of spectra from neutral and singly ionized atoms. They are used extensively for analytical spectrometry, but have seen limited use for the measurement of fundamental spectroscopic constants. Several properties of the ICP affect its suitability for such fundamental measurements. They include: spatial structure, spectral background, noise characteristics, electron densities and temperatures, and the state of equilibrium in the plasma. These properties are particularly sensitive to the means by which foreign atoms are introduced into the plasma. With some departures from the operating procedures normally used in analytical measurements, the ICP promise to be a useful source for the measurement of fundamental atomic constants. (orig.)

Arsenic species determination in human scalp hair by pressurized hot water extraction and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

Science.gov (United States)

Morado Piñeiro, Andrés; Moreda-Piñeiro, Jorge; Alonso-Rodríguez, Elia; López-Mahía, Purificación; Muniategui-Lorenzo, Soledad; Prada-Rodríguez, Darío

2013-02-15

Analytical methods for the determination of total arsenic and arsenic species (mainly As(III) and As(V)) in human scalp hair have been developed. Inductively coupled plasma-mass spectrometry (ICP-MS) and high performance liquid chromatography (HPLC) coupled to ICP-MS have been used for total arsenic and arsenic species determination, respectively. The proposed methods include a "green", fast, high efficient and automated species leaching procedure by pressurized hot water extraction (PHWE). The operating parameters for PHWE including modifier concentration, extraction temperature, static time, extraction steps, pressure, mean particle size, diatomaceous earth (DE) mass/sample mass ratio and flush volume were studied using design of experiments (Plackett-Burman design PBD). Optimum condition implies a modifier concentration (acetic acid) of 150 mM and powdered hair samples fully mixed with diatomaceous earth (DE) as a dispersing agent at a DE mass/sample mass ratio of 5. The extraction has been carried out at 100°C and at an extraction pressure of 1500 psi for 5 min in four extraction step. Under optimised conditions, limits of quantification of 7.0, 6.3 and 50.3 ng g(-1) for total As, As(III) and As(V), respectively were achieved. Repeatability of the overall procedure (4.4, 7.2 and 2.1% for total As, As(III) and As(V), respectively) was achieved. The analysis of GBW-07601 (human hair) certified reference material was used for validation. The optimised method has been finally applied to several human scalp hair samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Parameters assessment of the inductively-coupled circuit for wireless power transfer

Science.gov (United States)

Isaev, Yu N.; Vasileva, O. V.; Budko, A. A.; Lefebvre, S.

2017-02-01

In this paper, a wireless power transfer model through the example of inductively-coupled coils of irregular shape in software package COMSOL Multiphysics is studied. Circuit parameters, such as inductance, coil resistance and self-capacitance were defined through electromagnetic energy by the finite-element method. The study was carried out according to Helmholtz equation. Spatial distribution of current per unit depending on frequency and the coupling coefficient for analysis of resonant frequency and spatial distribution of the vector magnetic potential at different distances between coils were presented. The resulting algorithm allows simulating the wireless power transfer between the inductively coupled coils of irregular shape with the assessment of the optimal parameters.

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.

Dispersive liquid-liquid microextraction for simultaneous determination of cadmium, cobalt, lead and nickel in water samples by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Dos Santos Silva, E.; Correia, L.O.; Dos Santos, L.O.; Dos Santos Vieira, E.V.; Lemos, V.A.

2012-01-01

We report on a new method for the dispersive liquid-liquid microextraction of Cd(II), Co(II), Pb(II) and Ni (II) from water samples prior to their simultaneous determination by inductively coupled plasma optical emission spectrometry (ICP-OES). The procedure is based on the injection of a ternary solvent system composed of appropriate quantities of extraction solvent (trichloroethylene), dispersive solvent (ethanol), and the chelating reagent 2-(2'-benzothiazolylazo)-p-cresol into the sample solution. The solution turns turbid immediately after injection, and the analytes are extracted into the droplets of the organic phase which was dried and dissolved in a mixture of Triton X-114, nitric acid, and ethanol. The metal ions in this mixture were quantified by ICP-OES. The detection limits under optimized conditions are 0.2, 0.3, 0.2 and 0.7 μg L -1 for Cd(II), Co(II), Pb(II) and Ni(II), respectively. The enrichment factors were also calculated for Cd (13), Co (11), Pb (11) and Ni (8). The procedure was applied to the determination of cadmium, cobalt, lead and nickel in certified reference material (waterway sediment) and water samples. (author)

Precise determination of sodium in serum by simulated isotope dilution method of inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Yan Ying; Zhang Chuanbao; Zhao Haijian; Chen Wenxiang; Shen Ziyu; Wang Xiaoru; Chen Dengyun

2007-01-01

A new precise and accurate method for the determination of sodium in serum by inductively coupled plasma mass spectrometry (ICP-MS) was developed. Since 23 Na is the single isotope element, 27 Al is selected as simulated isotope of Na. Al is spiked into serum samples and Na standard solution. 23 Na/ 27 Al ratio in the Na standard solution is determined to assume the natural Na isotope ratio. The serums samples are digested by purified HNO 3 /H 2 O 2 and diluted to get about 0.6 μg·g -1 Al solutions, and the 23 Na/ 27 Al ratios of the serum samples are obtained to calculate the accurate Na concentrations basing on the isotope dilution method. When the simulated isotope dilution method of ICP-MS is applied and Al is selected as the simulated isotope of Na, the precise and accurate Na concentrations in the serums are determined. The inter-day precision of CV<0.13% for one same serum sample is obtained during 3 days 4 measurements. The spike recoveries are between 99.69% and 100.60% for 4 different serum samples and 3 days multi-measurements. The results of measuring standard reference materials of serum sodium are agree with the certified value. The relative difference between 3 days is 0.22%-0.65%, and the relative difference in one bottle is 0.15%-0.44%. The ICP-MS and Al simulated isotope dilution method is proved to be not only precise and accurate, but also quick and convenient for measuring Na in serum. It is promising to be a reference method for precise determination of Na in serum. Since Al is a low cost isotope dilution reagent, the method is possible to be widely applied for serum Na determination. (authors)

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

Determination of picomolar beryllium levels in seawater with inductively coupled plasma mass spectrometry following silica-gel preconcentration

Energy Technology Data Exchange (ETDEWEB)

Tazoe, Hirofumi, E-mail: tazoe@cc.hirosaki-u.ac.jp [Department of Radiation Chemistry, Institute of Radiation Emergency Mediation, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori 036-8564 (Japan); College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan); Yamagata, Takeyasu [College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan); Obata, Hajime [Atmosphere and Ocean Research Institute, The Tokyo University, 5-1-5 Kashiwanoha, Kashiwa-shi, Chiba 277-8564 (Japan); Nagai, Hisao [College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan)

2014-12-10

Highlights: • We developesd the simplest and robust SPE method for ultra low picomolar level beryllium in seawater. • Just silica gel column can quantitatively adsorb beryllium in neutral pH condition containing natural seawater. • EDTA solution can eliminate seawater matrixes retaining Be in the column, which optimize to ICP-MS detemination. • Accurate and precise Be data have been obtained for natural seawater from North Pacific Ocean. - Abstract: A robust and rapid method for the determination of natural levels of beryllium (Be) in seawater was developed to facilitate mapping Be concentrations in the ocean. A solid-phase extraction method using a silica gel column was applied for preconcentration and purification of Be in seawater prior to determination of Be concentrations with inductively coupled plasma mass spectrometry (ICP-MS). Be was quantitatively adsorbed onto silica gel from solutions with pH values ranging from 6.3 to 9, including natural seawater. The chelating agent ethylenediamine tetraacetic acid was used to remove other ions in the seawater matrix (Na, Mg, and Ca) that interfere with the ICP-MS analysis. The reproducibility of the method was 3% based on triplicate analyses of natural seawater samples, and the detection limit was 0.4 pmol kg{sup −1} for 250 mL of seawater, which is sufficient for the analysis of seawater in the open ocean. The method was then used to determine the vertical profile of Be in the eastern North Pacific Ocean, which was found to be a recycled-type profile in which the Be concentration increased with depth from the surface (7.2 pmol kg{sup −1} at <200 m) to deep water (29.2 pmol kg{sup −1} from 3500 m to the bottom)

Determination of picomolar beryllium levels in seawater with inductively coupled plasma mass spectrometry following silica-gel preconcentration

International Nuclear Information System (INIS)

Tazoe, Hirofumi; Yamagata, Takeyasu; Obata, Hajime; Nagai, Hisao

2014-01-01

Highlights: • We developesd the simplest and robust SPE method for ultra low picomolar level beryllium in seawater. • Just silica gel column can quantitatively adsorb beryllium in neutral pH condition containing natural seawater. • EDTA solution can eliminate seawater matrixes retaining Be in the column, which optimize to ICP-MS detemination. • Accurate and precise Be data have been obtained for natural seawater from North Pacific Ocean. - Abstract: A robust and rapid method for the determination of natural levels of beryllium (Be) in seawater was developed to facilitate mapping Be concentrations in the ocean. A solid-phase extraction method using a silica gel column was applied for preconcentration and purification of Be in seawater prior to determination of Be concentrations with inductively coupled plasma mass spectrometry (ICP-MS). Be was quantitatively adsorbed onto silica gel from solutions with pH values ranging from 6.3 to 9, including natural seawater. The chelating agent ethylenediamine tetraacetic acid was used to remove other ions in the seawater matrix (Na, Mg, and Ca) that interfere with the ICP-MS analysis. The reproducibility of the method was 3% based on triplicate analyses of natural seawater samples, and the detection limit was 0.4 pmol kg −1 for 250 mL of seawater, which is sufficient for the analysis of seawater in the open ocean. The method was then used to determine the vertical profile of Be in the eastern North Pacific Ocean, which was found to be a recycled-type profile in which the Be concentration increased with depth from the surface (7.2 pmol kg −1 at <200 m) to deep water (29.2 pmol kg −1 from 3500 m to the bottom)

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

High resolution studies of the origins of polyatomic ions in inductively coupled plasma-mass spectrometry, Part I. Identification methods and effects of neutral gas density assumptions, extraction voltage, and cone material

International Nuclear Information System (INIS)

Ferguson, Jill Wisnewski; Houk, R.S.

2006-01-01

Common polyatomic ions (ArO + , NO + , H 2 O + , H 3 O + , Ar 2 + , ArN + , OH + , ArH + , O 2 + ) in inductively coupled plasma-mass spectrometry (ICP-MS) are identified using high mass resolution and studied using kinetic gas temperatures (T gas ) determined from a dissociation reaction approach. Methods for making accurate mass measurements, confirming ion identifications, and correcting for mass bias are discussed. The effects of sampler and skimmer cone composition and extraction voltage on polyatomic ion formation are also explored. Neutral species densities at several locations in the extraction interface are estimated and the corresponding effects of the T gas value are calculated. The results provide information about the origins of background ions and indicate possible locations for their formation or removal

A new HF-resistant tandem spray chamber for improved determination of trace elements and Pb isotopes using inductively coupled plasma-mass spectrometry

International Nuclear Information System (INIS)

Krachler, Michael; Rausch, Nicole; Feuerbacher, Helmut; Klemens, Patrick

2005-01-01

The use of a new HF-resistant tandem spray chamber arrangement consisting of a cyclonic spray chamber and a Scott-type spray chamber made from PFA and PEEK provides a straightforward approach for improving the performance of inductively coupled-mass spectrometry (ICP-MS). The characteristics of the tandem spray chamber were critically evaluated against a PEEK cyclonic and a PFA Scott-type spray chamber, respectively. Sensitivity across the entire mass range was increased by about three times compared to the conventional setup utilizing only one spray chamber. Precision of the results, especially at low signal intensities, improved by 160% and 31% compared to the cyclonic and Scott-type spray chamber, respectively. Using the tandem spray chamber, the oxide formation rate was lowered by about 50%. Signals as low as 30 counts could be determined under routine measurement conditions with a RSD of 2.4% thus allowing to precisely quantify small concentration differences at the ng l -1 concentration level. The excellent precision (0.02-0.07%) of 206 Pb / 207 Pb and 206 Pb / 208 Pb ratios determined in pore water samples was rather limited by the instrumental capabilities of the single collector ICP-MS instrument than by the performance of the tandem spray chamber

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

Design And Construction Of Wireless Charging System Using Inductive Coupling

Directory of Open Access Journals (Sweden)

Do Lam Mung

2015-06-01

Full Text Available Abstract Wireless charging system described by using the method of inductive coupling. In this project oscillation circuit converts DC energy to AC energytransmitter coil to transmit magnetic field by passing frequency and then induce the receiver coil. The properties of Induction coupling are wavemagnetic field-wideband rangevery shortcm efficiencyhight and operation frequencyLF-bandseveral handred kHz.The project shows as a small charging for 5V battery of phone in this method. The system bases on coupling magnetic field then designed and constructed as two parts. There are transmitter part and receiver part. The transmitter coil transmitter part transmits coupling magnetic field to receiver coil receiver part by passing frequency at about 1.67MHz. The Amperes law Biot-Savart law and Faraday law are used to calculate the inductive coupling between the transmitter coil and the receiver coil. The calculation of this law shows how many power transfer in receiver part when how many distance between the transmitter coil and the receiver coil. The system is safe for users and neighbouring electronic devices. To get more accurate wireless charging system it needs to change the design of the following keywords.

Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

Hola, Marketa; Otruba, Vitezslav; Kanicky, Viktor

2006-01-01

Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP-OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm 3 ) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between ± 3% and ± 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA-ICP-OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed. The

Influence of binders on infrared laser ablation of powdered tungsten carbide pressed pellets in comparison with sintered tungsten carbide hardmetals studied by inductively coupled plasma atomic emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Hola, Marketa [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic); Otruba, Vitezslav [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic); Kanicky, Viktor [Research Centre for Environmental Chemistry and Ecotoxicology and Laboratory of Atomic Spectrochemistry, Faculty of Science, Masaryk University in Brno, Kotlarska 2, CZ 611 37 Brno (Czech Republic)]. E-mail: viktork@chemi.muni.cz

2006-05-15

Laser ablation (LA) was studied as a sample introduction technique for the analysis of powdered and sintered tungsten carbides (WC/Co) by inductively coupled plasma optical emission spectrometry (ICP-OES). The possibility to work with powdered and compact materials with close chemical composition provided the opportunity to compare LA sampling of similar substances in different forms that require different preparation procedures. Powdered WC/Co precursors of sintered hardmetals were prepared for the ablation as pressed pellets with and without powdered silver as a binder, while sintered hardmetal blocks were embedded into a resin to obtain discs, which were then smoothed and polished. A Q-switched Nd:YAG laser operated at its fundamental wavelength of 1064 nm with a pulse frequency of 10 Hz and maximum pulse energy of 220 mJ was used. A single lens was used for the laser beam focusing. An ablation cell (14 cm{sup 3}) mounted on a PC-controlled XY-translator was connected to an ICP spectrometer Jobin Yvon 170 Ultrace (laterally viewed ICP, mono- and polychromator) using a 1.5-m tubing (4 mm i.d.). Ablation was performed in a circular motion (2 mm diameter). Close attention was paid to the study of the crater parametres depending on hardness, cohesion and Ag binder presence in WC/Co samples. The influence of the Co content on the depth and structure of the ablation craters of the binderless pellets was also studied. Linear calibration plots of Nb, Ta and Ti were obtained for cemented WC/Co samples, binderless and binder-containing pellets. Relative widths of uncertainty intervals about the centroids vary between {+-} 3% and {+-} 7%, and exceptionally reach a value above 10%. The lowest determinable quantities (LDQ) of Nb, Ta and Ti calculated from the calibration lines were less than 0.5% (m/m). To evaluate the possibility of quantitative elemental analysis by LA-ICP-OES, two real sintered WC/Co samples and two real samples of powdered WC/Co materials were analysed

Preconcentration of uranium, thorium, zirconium, titanium, molybdenum and vanadium with oxine supported on microcrystalline naphthalene and their determinations by inductively coupled plasma atomic emission spectrometry

International Nuclear Information System (INIS)

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

2013-01-01

A sensitive and rapid method for the determination of uranium, thorium, zirconium, titanium, molybdenum and vanadium by inductively coupled plasma atomic emission spectrometry (ICP-AES) after solid-liquid extraction with microcrystalline naphthalene is developed. Analytes were quantitatively adsorbed as their oxinate complexes on naphthalene and determined by ICP-AES after stripping with 2 M HCl. The effect of various experimental parameters such as pH, reagent amounts, naphthalene amount and stripping conditions on the determination of these elements was investigated in detail. Under the optimized experimental conditions, the detection limits of this method for U (VI), Th (IV), Zr (IV), Ti (IV), Mo (VI) and V (V) were 20.0 ng mL -1 and the relative standard deviations obtained for three replicate determinations at a concentration of 1.0 µg mL -1 were 1.5-3.0%. The proposed method has been applied in the analysis of SY-2, SY-3 and pre-analysed samples for U, Th, Zr, Ti, Mo and V the analytical results are in good agreement with recommended values. (author)

Arsenic Species in Edible Seaweeds Using In Vitro Biomimetic Digestion Determined by High-Performance Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry

Directory of Open Access Journals (Sweden)

Yan-Fang Zhao

2014-01-01

Full Text Available Arsenite [As (III], arsenate [As (V], methylarsonate (MMA, and dimethylarsinate (DMA in five edible seaweeds (the brown algae Laminaria japonica, red algae Porphyra yezoensis, brown algae Undaria pinnatifida, brown algae Hizikia fusiformis, and green algae Enteromorpha prolifera were analyzed using in vitro digestion method determined by high-performance liquid chromatography inductively coupled plasma mass spectrometry. The results showed that DMA was found in the water extracts of all samples; As (III were detected in L. japonica and U. pinnatifida and about 23.0 and 0.15 mg/kg of As (V were found in H. fusiformis and E. prolifera respectively. However, after the gastrointestinal digestion, As (V was not detected in any of the five seaweeds. About 0.19 and 1.47 mg/kg of As (III was detected in the gastric extracts of L. japonica and H. fusiformis, respectively, and about 0.31 and 0.10 mg/kg of As (III were extracted from the intestinal extracts of Porphyra yezoensis and U. pinnatifida, respectively. The present results successfully reveal the differences of As species and levels in the water and biomimetic extracts of five edible seaweeds. The risk assessment of the inorganic arsenic in the five edible seaweeds based on present data showed almost no hazards to human health.

Microwave-assisted versus conventional decomposition procedures applied to a ceramic potsherd standard reference material by inductively coupled plasma atomic emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Papadopoulou, D.N.; Zachariadis, G.A.; Anthemidis, A.N.; Tsirliganis, N.C.; Stratis, J.A

2004-03-03

Inductively coupled plasma atomic emission spectrometry (ICP-AES) is a powerful, sensitive analytical technique with numerous applications in chemical characterization including that of ancient pottery, mainly due to its multi-element character, and the relatively short time required for the analysis. A critical step in characterization studies of ancient pottery is the selection of a suitable decomposition procedure for the ceramic matrix. The current work presents the results of a comparative study of six decomposition procedures applied on a standard ceramic potsherd reference material, SARM 69. The investigated decomposition procedures included three microwave-assisted decomposition procedures, one wet decomposition (WD) procedure by conventional heating, one combined microwave-assisted and conventional heating WD procedure, and one fusion procedure. Chemical analysis was carried out by ICP-AES. Five major (Si, Al, Fe, Ca, Mg), three minor (Mn, Ba, Ti) and two trace (Cu, Co) elements were determined and compared with their certified values. Quantitation was performed at two different spectral lines for each element and multi-element matrix-matched calibration standards were used. The recovery values for the six decomposition procedures ranged between 75 and 110% with a few notable exceptions. Data were processed statistically in order to evaluate the investigated decomposition procedures in terms of recovery, accuracy and precision, and eventually select the most appropriate one for ancient pottery analysis.

Extraction and analysis of silver and gold nanoparticles from biological tissues using single particle inductively coupled plasma mass spectrometry.

Science.gov (United States)

Gray, Evan P; Coleman, Jessica G; Bednar, Anthony J; Kennedy, Alan J; Ranville, James F; Higgins, Christopher P

2013-12-17

Expanded use of engineered nanoparticles (ENPs) in consumer products increases the potential for environmental release and unintended biological exposures. As a result, measurement techniques are needed to accurately quantify ENP size, mass, and particle number distributions in biological matrices. This work combines single particle inductively coupled plasma mass spectrometry (spICPMS) with tissue extraction to quantify and characterize metallic ENPs in environmentally relevant biological tissues for the first time. ENPs were extracted from tissues via alkaline digestion using tetramethylammonium hydroxide (TMAH). Method development was performed using ground beef and was verified in Daphnia magna and Lumbriculus variegatus . ENPs investigated include 100 and 60 nm Au and Ag stabilized by polyvynylpyrrolidone (PVP). Mass- and number-based recovery of spiked Au and Ag ENPs was high (83-121%) from all tissues tested. Additional experiments suggested ENP mixtures (60 and 100 nm Ag ENPs) could be extracted and quantitatively analyzed. Biological exposures were also conducted to verify the applicability of the method for aquatic organisms. Size distributions and particle number concentrations were determined for ENPs extracted from D. magna exposed to 98 μg/L 100 nm Au and 4.8 μg/L 100 nm Ag ENPs. The D. magna nanoparticulate body burden for Au ENP uptake was 613 ± 230 μg/kgww, while the measured nanoparticulate body burden for D. magna exposed to Ag ENPs was 59 ± 52 μg/kgww. Notably, the particle size distributions determined from D. magna tissues suggested minimal shifts in the size distributions of ENPs accumulated, as compared to the exposure media.

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.

Application of a microwave-based desolvation system for multi-elemental analysis of wine by inductively coupled plasma based techniques

Energy Technology Data Exchange (ETDEWEB)

Grindlay, Guillermo [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, P.O. Box 99, 03080 Alicante (Spain)], E-mail: guillermo.grindlay@ua.es; Mora, Juan; Maestre, Salvador; Gras, Luis [Department of Analytical Chemistry, Nutrition and Food Sciences, University of Alicante, P.O. Box 99, 03080 Alicante (Spain)

2008-11-23

Elemental wine analysis is often required from a nutritional, toxicological, origin and authenticity point of view. Inductively coupled plasma based techniques are usually employed for this analysis because of their multi-elemental capabilities and good limits of detection. However, the accurate analysis of wine samples strongly depends on their matrix composition (i.e. salts, ethanol, organic acids) since they lead to both spectral and non-spectral interferences. To mitigate ethanol (up to 10% w/w) related matrix effects in inductively coupled plasma atomic emission spectrometry (ICP-AES), a microwave-based desolvation system (MWDS) can be successfully employed. This finding suggests that the MWDS could be employed for elemental wine analysis. The goal of this work is to evaluate the applicability of the MWDS for elemental wine analysis in ICP-AES and inductively coupled plasma mass spectrometry (ICP-MS). For the sake of comparison a conventional sample introduction system (i.e. pneumatic nebulizer attached to a spray chamber) was employed. Matrix effects, precision, accuracy and analysis throughput have been selected as comparison criteria. For ICP-AES measurements, wine samples can be directly analyzed without any sample treatment (i.e. sample dilution or digestion) using pure aqueous standards although internal standardization (IS) (i.e. Sc) is required. The behaviour of the MWDS operating with organic solutions in ICP-MS has been characterized for the first time. In this technique the MWDS has shown its efficiency to mitigate ethanol related matrix effects up to concentrations of 1% (w/w). Therefore, wine samples must be diluted to reduce the ethanol concentration up to this value. The results obtained have shown that the MWDS is a powerful device for the elemental analysis of wine samples in both ICP-AES and ICP-MS. In general, the MWDS has some attractive advantages for elemental wine analysis when compared to a conventional sample introduction system such

Application of a microwave-based desolvation system for multi-elemental analysis of wine by inductively coupled plasma based techniques

International Nuclear Information System (INIS)

Grindlay, Guillermo; Mora, Juan; Maestre, Salvador; Gras, Luis

2008-01-01

Elemental wine analysis is often required from a nutritional, toxicological, origin and authenticity point of view. Inductively coupled plasma based techniques are usually employed for this analysis because of their multi-elemental capabilities and good limits of detection. However, the accurate analysis of wine samples strongly depends on their matrix composition (i.e. salts, ethanol, organic acids) since they lead to both spectral and non-spectral interferences. To mitigate ethanol (up to 10% w/w) related matrix effects in inductively coupled plasma atomic emission spectrometry (ICP-AES), a microwave-based desolvation system (MWDS) can be successfully employed. This finding suggests that the MWDS could be employed for elemental wine analysis. The goal of this work is to evaluate the applicability of the MWDS for elemental wine analysis in ICP-AES and inductively coupled plasma mass spectrometry (ICP-MS). For the sake of comparison a conventional sample introduction system (i.e. pneumatic nebulizer attached to a spray chamber) was employed. Matrix effects, precision, accuracy and analysis throughput have been selected as comparison criteria. For ICP-AES measurements, wine samples can be directly analyzed without any sample treatment (i.e. sample dilution or digestion) using pure aqueous standards although internal standardization (IS) (i.e. Sc) is required. The behaviour of the MWDS operating with organic solutions in ICP-MS has been characterized for the first time. In this technique the MWDS has shown its efficiency to mitigate ethanol related matrix effects up to concentrations of 1% (w/w). Therefore, wine samples must be diluted to reduce the ethanol concentration up to this value. The results obtained have shown that the MWDS is a powerful device for the elemental analysis of wine samples in both ICP-AES and ICP-MS. In general, the MWDS has some attractive advantages for elemental wine analysis when compared to a conventional sample introduction system such

A rapid method for simultaneous determination of arsenic, cadmium and lead in drinking water by inductively coupled plasma mass spectrometry

Directory of Open Access Journals (Sweden)

Joshua Rey P. Torres

Full Text Available The raw water source of drinking water in most areas in the Philippines is typically river water and in some cases groundwater. These sources are prone to elevated levels of metals and metalloids that may cause exposure of the general population when the treatment of the water is inadequate. This work presents a simple method based on EPA Method 200.8 for the determination of total concentrations of arsenic (As, cadmium (Cd and lead (Pb in drinking water using inductively coupled plasma-mass spectrometry (ICP-MS as the element-selective detector. This was applied in the determination of these elements in the water supply in Metro Manila, Philippines. The method detection limits were 0.095 μg L-1, 0.043 μg L-1, and 0.114 μg L-1 for total As, Cd and Pb, respectively.The method was validated using National Institute of Standards and Technology (NIST 1643e certified reference material for trace elements in water and determined values were 60.4 ± 0.5 μg L-1, 6.7 ± 0.1 μg L-1, and 19.6 ± 0.5 μg L-1 for As, Cd and Pb, respectively. These determined values were in good agreement with the certified values in the reference material. Analysis of actual drinking water samples showed that most samples did not exceed the limit of the Philippine drinking water standard for the elements.

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

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.

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.

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)

Coupled heat-electromagnetic simulation of inductive charging stations for electric vehicles

NARCIS (Netherlands)

Kaufmann, C.; Günther, M.; Klagges, D.; Richwin, M.; Schöps, S.; Maten, ter E.J.W.

2012-01-01

Coupled electromagnetic-heat problems have been studied for induction or inductive heating, for dielectric heating, for testing of corrosion, for detection of cracks, for hardening of steel, and more recently for inductive charging of electric vehicles. In nearly all cases a simple co-simulation is

Coupled heat-electromagnetic simulation of inductive charging stations for electric vehicles

NARCIS (Netherlands)

Kaufmann, C.; Günther, M.; Klagges, D.; Richwin, M.; Schöps, S.; Maten, ter E.J.W.; Fontes, M.; Günther, M.; Marheineke, N.

2014-01-01

Coupled electromagnetic-heat problems have been studied for induction or inductive heating, for dielectric heating, for testing of corrosion, for detection of cracks, for hardening of steel, and more recently for inductive charging of electric vehicles. In nearly all cases a simple co-simulation is

Ultra-wide bandwidth improvement of piezoelectric energy harvesters through electrical inductance coupling

Science.gov (United States)

Abdelmoula, H.; Abdelkefi, A.

2015-11-01

The design and analysis of innovative ultra-wide bandwidth piezoelectric energy harvesters are deeply investigated. An electrical inductance is considered in the harvester's circuit to be connected in series or parallel to a load resistance. A lumped-parameter model is used to model the electromechanical response of the harvester when subjected to harmonic excitations. A linear comprehensive analysis is performed to investigate the effects of an electrical inductance on the coupled frequencies and damping of the harvester. It is shown that including an electrical inductance connected in series or in parallel to an electrical load resistance can result in the appearance of a second coupled frequency of electrical type. The results show that the inclusion of an inductance may give the opportunity to tune one of the coupled frequencies of mechanical and electrical types to the available excitation frequency in the environment. Using the gradient method, an optimization analysis is then performed to determine the optimum values of the electrical inductance and load resistance that maximize the harvested power. It is demonstrated that, for each excitation frequency, there is a combination of optimum values of the electrical inductance and resistance in such a way an optimum constant value of the harvested power is found. Numerical analysis is then performed to show the importance of considering an additional inductance in the harvester's circuitry in order to design broadband energy harvesters. The results show that the presence of the second coupled frequency of electrical type due to the inductance gives the possibility to design optimal broadband inductive-resistive piezoelectric energy harvesters with minimum displacement due to shunt damping effect.

Nickel quantification in serum by a validated sector-field inductively coupled plasma mass spectrometry method: Assessment of tentative reference values for an Italian population.

Science.gov (United States)

Bocca, Beatrice; Forte, Giovanni; Ronchi, Anna; Gaggeri, Raffaella; Alimonti, Alessandro; Minoia, Claudio

2006-01-01

The daily exposure to Ni from food, industrial processes, jewellery and coins makes the determination of Ni in human serum an important way to monitor the health status in non-occupationally exposed subjects. To this end, a method based on sector-field inductively coupled plasma mass spectrometry was developed and validated. The limits of detection (LoD) and quantification (LoQ), sensitivity, linearity range, trueness, repeatability, within-laboratory reproducibility and robustness were the considered issues of the validation process. The uncertainty associated with the measurements was also calculated, according to the Eurachem/Citac Guide. The method LoD and LoQ were 0.03 and 0.09 ng mL(-1), linearity was over two order of magnitude, trueness was -3.57%, and the repeatability and reproducibility showed relative standard deviations equal to 4.56% and 6.52%, respectively. The relative expanded uncertainty was 21.8% at the Ni levels found in the general population. The tentative reference value for serum Ni was 0.466 +/- 0.160 ng mL(-1) with a related interval between 0.226 and 1.026 ng mL(-1). Copyright 2006 John Wiley & Sons, Ltd.

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

Development of Exact Matrix-Matching Inductively Coupled Plasma-Optical Emission Spectroscopy for the Analysis of Cu and K in Infant Formula

Energy Technology Data Exchange (ETDEWEB)

Lee, Ye-Ji; Yim, Yong-Hyeon [University of Science and Technology, Daejeon (Korea, Republic of); Heo, Sung Woo; Han, Myung-Sub; Lim, Youngran [Korea Research Institute of Standards and Science, Daejeon (Korea, Republic of)

2016-08-15

In the present study, we have developed an exact matrix-matching inductively coupled plasma-optical emission spectroscopy (ICP-OES) as a low-cost alternative to the isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) method for accurate and precise measurements of nutrient elements K and Cu in infant formula. In spite of its high precision and accuracy, ICP-OES analysis of complex samples was not reliable due to biases originating from various matrix effects. The elaborated exact matrix-matching approach tested here demonstrated its potential to minimize biases due to matrix mismatch. The exact matrix-matching ICP-OES method was successfully validated by comparing the results with those from an isotope dilution ICP-M S method. Because the model provides reliable results without significant loss of precision, it will be an excellent choice for major element analysis in a complex sample, especially when isotope dilution is not applicable due to the l ck of alternative isotopes or the high cost of enriched isotopes.

Systematic analysis and experiment of inductive coupling and induced voltage for inductively coupled wireless implantable neurostimulator application

International Nuclear Information System (INIS)

Xue, Ning; Cho, Sung-Hoon; Chang, Sung-Pil; Lee, Jeong-Bong

2012-01-01

The main strategy for wireless power transfer to implantable devices is to use inductive coupling technology. The induced voltage of implanted devices highly depends on factors such as mutual inductance between the external transmitter coil and the receiver coil, quality factor of the receiver circuit and operation frequency. In this paper, the mutual inductance under a variety of geometries of external coil and under the condition of different vertical distances, lateral displacements and angular misalignments between two coils were theoretically calculated and simulated. To ascertain the condition of maximum power transmission for certain coils’ position requirements, an LC tank (2.7 mm × 2 mm) consisting of a microfabricated gold inductor coil and a small surface mounted capacitor was designed and fabricated as the telemetric part of a neurostimulator. The induced voltage of the LC tank was measured in both air and artificial tissue media under different sizes of power coil and operation frequencies. As a result, the optimum size of a transmitter coil is selected to be of 4 mm inner radius with six turns of coil, while the whole coupling system operates at 94 MHz resonant frequency within 5–11 mm vertical distance, 0–4 mm lateral and 0°–50° angular misalignment between two coils. With the change of the above coils’ positions, the measured induced voltage drops within 30%, satisfying the surgical requirement for neurostimulator implantation. (paper)

Investigation of plasma-related matrix effects in inductively coupled plasma-atomic emission spectrometry caused by matrices with low second ionization potentials-identification of the secondary factor

International Nuclear Information System (INIS)

Chan, George C.-Y.; Hieftje, Gary M.

2006-01-01

Plasma-related matrix effects induced by a comprehensive list of matrix elements (a total of fifty-one matrices) in inductively coupled plasma-atomic emission spectrometry were investigated and used to confirm that matrix effects caused by elements with a low second ionization potential are more severe than those from matrix elements having a low first ionization potential. Although the matrix effect is correlated unambiguously with the second ionization potential of a matrix, the correlation is not monotonic, which suggests that at least one other factor is operative. Through study of a large pool of matrix elements, it becomes possible to identify another critical parameter that defines the magnitude of the matrix effect; namely the presence of low-lying energy levels in the doubly charged matrix ion. Penning ionization by Ar excited states is proposed as the dominant mechanism for both analyte ionization/excitation and matrix effects; matrices with a low second ionization potential can effectively quench the population of Ar excited states through successive Penning ionization followed by ion-electron recombination and lead to more severe matrix effects

Arsenic, cadmium and lead concentrations in Yerba mate commercialized in Southern Brazil by inductively coupled plasma mass spectrometry

Directory of Open Access Journals (Sweden)

Lisia Maria Gobbo dos Santos

2017-12-01

Full Text Available ABSTRACT: “Mate” or “Yerba Mate” (Ilex paraguariensis is a native South American plant, commonly consumed in Argentina, Paraguay, Uruguay and southern Brazil. Recent research has detected the presence of many vitamins and metals in this plant. Theses metals are also part of yerba mate’s mineral composition, due to soil and water contamination by pesticides and fertilizers, coal and oil combustion, vehicle emissions, mining, smelting, refining and the incineration of urban and industrial waste. Regardless of their origin, some inorganic elements, such as arsenic, cadmium and lead, are considered toxic, since they accumulate in all plant tissues and are, thus, introduced into the food chain. In this context, the aim of the present study was to determine and compare arsenic, cadmium, lead concentrations in 104 samples of yerba mate (Ilex paraguariensis marketed, and consumed in three southern Brazilian States, namely Paraná (PR, Santa Catarina (SC and Rio Grande do Sul (RS. Each element was determined by inductively coupled plasma mass spectrometry (ICP-MS, on a Nexion 300D equipment (Perkin Elmer. As, Cd and Pb concentrations in yerba mate leaves ranged from 0.015 to 0.15mg kg-1, 0.18 to 1.25mg kg-1 and 0.1 to 1.20mg kg-1, respectively. Regarding Cd, 84% of the samples from RS, 63% from PR and 75% from SC showed higher concentrations than the maximum permissible limit of 0.4mg kg-1 established by the Brazilian National Sanitary Surveillance Agency (ANVISA, while 7% of the samples from RS and 5% from PR were unsatisfactory for Pb. Concentrations were below the established ANVISA limit of 0.6mg kg-1 for all samples.

The influence of laser-particle interaction in laser induced breakdown spectroscopy and laser ablation inductively coupled plasma spectrometry

International Nuclear Information System (INIS)

Lindner, Helmut; Loper, Kristofer H.; Hahn, David W.; Niemax, Kay

2011-01-01

Particles produced by previous laser shots may have significant influence on the analytical signal in laser-induced breakdown spectroscopy (LIBS) and laser ablation inductively coupled plasma (LA-ICP) spectrometry if they remain close to the position of laser sampling. The effects of these particles on the laser-induced breakdown event are demonstrated in several ways. LIBS-experiments were conducted in an ablation cell at atmospheric conditions in argon or air applying a dual-pulse arrangement with orthogonal pre-pulse, i.e., plasma breakdown in a gas generated by a focussed laser beam parallel and close to the sample surface followed by a delayed crossing laser pulse in orthogonal direction which actually ablates material from the sample and produces the LIBS plasma. The optical emission of the LIBS plasma as well as the absorption of the pre-pulse laser was measured. In the presence of particles in the focus of the pre-pulse laser, the plasma breakdown is affected and more energy of the pre-pulse laser is absorbed than without particles. As a result, the analyte line emission from the LIBS plasma of the second laser is enhanced. It is assumed that the enhancement is not only due to an increase of mass ablated by the second laser but also to better atomization and excitation conditions favored by a reduced gas density in the pre-pulse plasma. Higher laser pulse frequencies increase the probability of particle-laser interaction and, therefore, reduce the shot-to-shot line intensity variation as compared to lower particle loadings in the cell. Additional experiments using an aerosol chamber were performed to further quantify the laser absorption by the plasma in dependence on time both with and without the presence of particles. The overall implication of laser-particle interactions for LIBS and LA-ICP-MS/OES are discussed.

The influence of laser-particle interaction in laser induced breakdown spectroscopy and laser ablation inductively coupled plasma spectrometry

Science.gov (United States)

Lindner, Helmut; Loper, Kristofer H.; Hahn, David W.; Niemax, Kay

2011-02-01

Particles produced by previous laser shots may have significant influence on the analytical signal in laser-induced breakdown spectroscopy (LIBS) and laser ablation inductively coupled plasma (LA-ICP) spectrometry if they remain close to the position of laser sampling. The effects of these particles on the laser-induced breakdown event are demonstrated in several ways. LIBS-experiments were conducted in an ablation cell at atmospheric conditions in argon or air applying a dual-pulse arrangement with orthogonal pre-pulse, i.e., plasma breakdown in a gas generated by a focussed laser beam parallel and close to the sample surface followed by a delayed crossing laser pulse in orthogonal direction which actually ablates material from the sample and produces the LIBS plasma. The optical emission of the LIBS plasma as well as the absorption of the pre-pulse laser was measured. In the presence of particles in the focus of the pre-pulse laser, the plasma breakdown is affected and more energy of the pre-pulse laser is absorbed than without particles. As a result, the analyte line emission from the LIBS plasma of the second laser is enhanced. It is assumed that the enhancement is not only due to an increase of mass ablated by the second laser but also to better atomization and excitation conditions favored by a reduced gas density in the pre-pulse plasma. Higher laser pulse frequencies increase the probability of particle-laser interaction and, therefore, reduce the shot-to-shot line intensity variation as compared to lower particle loadings in the cell. Additional experiments using an aerosol chamber were performed to further quantify the laser absorption by the plasma in dependence on time both with and without the presence of particles. The overall implication of laser-particle interactions for LIBS and LA-ICP-MS/OES are discussed.

[Inductively coupled plasma mass spectrometry for the simultaneous determination of thirty metals and metalloids elements in blood samples].

Science.gov (United States)

Ding, Chun-guang; Zhu, Chun; Liu, De-ye; Dong, Ming; Zhang, Ai-hua; Pan, Ya-juan; Yan, Hui-fang

2012-08-01

To establish an inductively coupled plasma mass spectrometry(ICP-MS) method for determination of 30 trace elements including As, Ba, Be, Bi, Ni, Cd, Co, Cr, Cs, Cu, Ga, Mn, Pb, Sr, Tl, V, Ge, Mo, Nb, Ti, W, Te, Se, Zr, In, Sb, Hg, Ce, La, and Sm in human blood. The blood samples were analyzed by ICP-MS after diluted 1/10 with 0.01% Triton-X-100 and 0.5% nitric acid solution. Y, Rh and Lu were selected as internal standard in order to correct the matrix interference of Cr, As, Se, and Hg by a hex pole-based collision-reaction cell. Other elements were determined with standard method. The limits of detection, precision and accuracy of the method were evaluated. The accuracy was validated by the determination of the whole blood reference material. All the 30 trace elements have good linearity in their determination range, with the correlation coefficient > 0.9999. The limits of detection of the 30 trace elements were in the range of 1.19 - 2.15 µg/L and the intra-precision and inter-precision (relative standard deviation, RSD) were less than 14.3% (except Hg RSD < 21.2%, and Ni RSD < 15.4%). The spiked recovery for all elements fell within 59.3% - 119.2%. Among the 13 whole blood reference materials, V, Cr, Mn, Co, Ni, Cu, As, Se, Cd, Te, and Pb (1.45, 1.19, 18.40, 0.18, 1.57, 591.00, 2.97, 61.00, 0.35, 1.86, and 9.70 µg/L respectively) fell within the acceptable range and the detection results of Hg (0.59 µg/L) and Mo (1.59 µg/L) were slightly beyond the range. This method was simple, fast and effective. It can be used to monitor the multi-elementary concentration in human blood.

Electrical-thermal coupling of induction machine for improved ...

African Journals Online (AJOL)

Electrical-thermal coupling of induction machine for improved thermal performance. ... Nigerian Journal of Technology ... The interaction of its electrical and mechanical parts leads to an increase in temperature which if not properly monitored ...

Experimental analysis and simulation calculation of the inductances of loosely coupled transformer

Science.gov (United States)

Kerui, Chen; Yang, Han; Yan, Zhang; Nannan, Gao; Ying, Pei; Hongbo, Li; Pei, Li; Liangfeng, Guo

2017-11-01

The experimental design of iron-core wireless power transmission system is designed, and an experimental model of loosely coupled transformer is built. Measuring the air gap on both sides of the transformer 15mm inductor under the parameters. The feasibility and feasibility of using the finite element method to calculate the coil inductance parameters of the loosely coupled transformer are analyzed. The system was modeled by ANSYS, and the magnetic field was calculated by finite element method, and the inductance parameters were calculated. The finite element method is used to calculate the inductive parameters of the loosely coupled transformer, and the basis for the accurate compensation of the capacitance of the wireless power transmission system is established.

A rapid and practical strategy for the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in large amounts of ultrabasic rock by inductively coupled plasma optical emission spectrometry combined with ultrasound extraction

Science.gov (United States)

Zhang, Gai; Tian, Min

2015-04-01

This proposed method regulated the determination of platinum, palladium, ruthenium, rhodium, iridium and gold in platinum-group ores by nickel sulfide fire assay—inductively coupled plasma optical emission spectrometry (ICP-OES) combined with ultrasound extraction for the first time. The quantitative limits were 0.013-0.023μg/g. The samples were fused to separate the platinum-group elements from matrix. The nickel sulfide button was then dissolved with hydrochloric acid and the insoluble platinum-group sulfide residue was dissolved with aqua regia by ultrasound bath and finally determined by ICP-OES. The proposed method has been applied into the determination of platinum-group element and gold in large amounts of ultrabasic rocks from the Great Dyke of Zimbabwe.

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.

Trace metal analysis by laser ablation-inductively coupled plasmamass spectrometry and x-ray K-edge densitometry of forensic samples

Energy Technology Data Exchange (ETDEWEB)

Berry, Jonna Elizabeth [Iowa State Univ., Ames, IA (United States)

2016-10-25

This dissertation describes a variety of studies on the determination of trace elements in samples with forensic importance. Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) was used to determine the trace element composition of numerous lipstick samples. Lipstick samples were determined to be homogeneous. Most lipstick samples of similar colors were readily distinguishable at a 95% confidence interval based on trace element composition. Numerous strands of a multi-strand speaker cable were analyzed by LA-ICP-MS. The strands in this study are spatially heterogeneous in trace element composition. In actual forensic applications, the possibility of spatial heterogeneity must be considered, especially in cases where only small samples (e.g., copper wire fragments after an explosion) are available. The effects of many unpredictable variables, such as weather, temperature, and human activity, on the retention of gunshot residue (GSR) around projectile wounds were assessed with LAICP- MS. Skin samples around gunshot and stab wounds and larvae feeding in and around the wounds on decomposing pig carcasses were analyzed for elements consistent with GSR (Sb, Pb, Ba, and Cu). These elements were detected at higher levels in skin and larvae samples around the gunshot wounds compared to the stab wounds for an extended period of time throughout decomposition in both a winter and summer study. After decomposition, radiographic images of the pig bones containing possible damage from bullets revealed metallic particles embedded within a number of bones. Metallic particles within the bones were analyzed with x-ray, K-edge densitometry and determined to contain lead, indicating that bullet residue can be retained throughout decomposition and detected within bones containing projectile trauma.

SPECIATION OF SELENIUM AND ARSENIC COMPOUNDS BY CAPILLARY ELECTROPHORESIS WITH HYDRODYNAMICALLY MODIFIED ELECTROOSMOTIC FLOW AND ON-LINE REDUCTION OF SELENIUM(VI) TO SELENIUM(IV) WITH HYDRIDE GENERATION INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRIC DETECTION

Science.gov (United States)

Capillary electrophoresis (CE) with hydride generation inductively coupled plasma mass spectrometry was used to determine four arsenicals and two selenium species. Selenate (SeVI) was reduced on-line to selenite (SeIV') by mixing the CE effluent with concentrated HCl. A microporo...

An ultrasound-assisted digestion method for the determination of toxic element concentrations in ash samples by inductively coupled plasma optical emission spectrometry

International Nuclear Information System (INIS)

Ilander, Aki; Vaeisaenen, Ari

2007-01-01

A method of ultrasound-assisted digestion followed by inductively coupled plasma optical emission spectrometry (ICP-OES) used for the determination of toxic element concentrations (arsenic, barium, cobalt, copper, lead, nickel, strontium, vanadium and zinc) in ash samples was developed. All the measurements were performed in robust plasma conditions which were tested by measuring the Mg(II) 280.270 nm/Mg(I) 285.213 nm line intensity ratios. The highest line intensity ratios were observed when a nebulizer gas flow of 0.6 L min -1 , auxiliary gas flow of 0.2 L min -1 and plasma power of 1400 W were used for radially viewed plasma. The analysis of SRM 1633b showed that the ultrasound-assisted method developed is highly comparable with the microwave digestion method standardized by the United States Environmental Protection Agency (EPA-3052). The ultrasound-assisted digestion with a digestion solution of aqua regia and hydrofluoric acid (HF) resulted in recovery rates of over 81%. One exception is arsenic which resulted in recoveries of about 60% only; however, it could be digested with good recovery (>90%) using a digestion solution of 5 mL of water and 5 mL of aqua regia. The major advantage of the ultrasound-assisted digestion over microwave digestion is the high treatment rate (30 samples simultaneously with a sonication time of 18 min)

Simultaneous separation and determination of six arsenic species in rice by anion-exchange chromatography with inductively coupled plasma mass spectrometry.

Science.gov (United States)

Ma, Li; Yang, Zhaoguang; Tang, Jie; Wang, Lin

2016-06-01

The simultaneous separation and determination of arsenite As(III), arsenate As(V), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AsB), and arsenocholine (AsC) in rice samples have been carried out in one single anion-exchange column run by high-performance liquid chromatography with inductively coupled plasma mass spectrometry. To estimate the effect of variables on arsenic (As) speciation, the chromatographic conditions including type of competing anion, ionic strength, pH of elution buffer, and flow rate of mobile phase have been investigated by a univariate approach. Under the optimum chromatographic conditions, baseline separation of six As species has been achieved within 10 min by gradient elution program using 4 mM NH4 HCO3 at pH 8.6 as mobile phase A and 4 mM NH4 HCO3 , 40 mM NH4 NO3 at pH 8.6 as mobile phase B. The method detection limits for As(III), As(V), MMA, DMA, AsB, and AsC were 0.4, 0.9, 0.2, 0.4, 0.5, and 0.3 μg/kg, respectively. The proposed method has been applied to separation and quantification of As species in real rice samples collected from Hunan Province, China. The main As species detected in all samples were As(III), As(V) and DMA, with inorganic As accounting for over 80% of total As in these samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Elevated metallothionein-bound cadmium concentrations in urine from bladder carcinoma patients, investigated by size exclusion chromatography-inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Wolf, Christian [Department of Molecular Trace Element Research in the Life Sciences, Helmholtz Centre Berlin for Materials and Energy, Glienicker Str. 100, 14109 Berlin (Germany)], E-mail: wolf@helmholtz-berlin.de; Strenziok, Romy [Department of Urology, Charite University Medicine Berlin, Campus Benjamin Franklin, Hindenburgdamm 30, 12203 Berlin (Germany); Kyriakopoulos, Antonios [Department of Molecular Trace Element Research in the Life Sciences, Helmholtz Centre Berlin for Materials and Energy, Glienicker Str. 100, 14109 Berlin (Germany)

2009-01-12

Cadmium is discussed as being involved in the development of transitional cell carcinoma (TCC) of the bladder and can be observed in urine of these patients. Investigations of urinary samples from bladder cancer patients and normal controls were carried out with special emphasis on metallothionein (MT)-bound cadmium. Compounds that are constituents of urine were separated in urine samples by means of size exclusion chromatography and cadmium was monitored continuously with a hyphenated inductively coupled plasma mass spectrometry (ICP-MS) system. MT-bound cadmium was quantified by peak area integration, taking into account the intensity of the rhodium signal which was added continuously before ICP-MS detection. The obtained results show that urinary cadmium is predominantly bound to the observed MT-fraction. The median of the MT-bound cadmium concentration in the control group was found to be 0.8 {mu}g L{sup -1} whereas the cancer group has a median of 1.8 {mu}g L{sup -1}. The variance of the data in the cancer group is much higher than in the controls. However, the urinary MT-bound cadmium is significantly elevated in the cancer group; odds-ratio test: 7.11 (95% C.I.: 1.89-26.80), taking into account the total protein content. Due to the fact that only one main cadmium-containing fraction was observed, there is no necessity to separate the MT-fraction before cadmium determination in urine samples in future studies.

Flagging and correcting non-spectral matrix interferences with spatial emission profiles and gradient dilution in inductively coupled plasma-atomic emission spectrometry

International Nuclear Information System (INIS)

Cheung, Yan; Schwartz, Andrew J.; Chan, George C.-Y.; Hieftje, Gary M.

2015-01-01

Matrix interference remains one of the most daunting challenges commonly encountered in inductively coupled plasma-atomic emission spectrometry (ICP-AES). In the present study, a method is described that enables identification and correction of matrix interferences in axial-viewed ICP-AES through a combination of spatial mapping and on-line gradient dilution. Cross-sectional emission maps of the plasma are used to indicate the presence of non-spectral (plasma-related and sample-introduction-related) matrix interferences. In particular, apparent concentrations of an analyte species determined at various radial locations in the plasma differ in the presence of a matrix interference, which allows the interference to be flagged. To correct for the interference, progressive, on-line dilution of the sample, performed by a gradient high-performance liquid-chromatograph pump, is utilized. The spatially dependent intensities of analyte emission are monitored at different levels of sample dilution. As the dilution proceeds, the matrix-induced signal variation is reduced. At a dilution where the determined concentrations become independent of location in the plasma, the matrix interference is minimized. - Highlights: • Non-spectral matrix interference in ICP-AES is flagged and minimized. • Emission from different locations of the plasma are collected simultaneously. • Spatially dependent determined concentrations indicate the presence of interference. • Gradient dilution is performed on both calibration standards and sample. • Optimal dilution factor to minimize interference is found as dilution increases

Flagging and correcting non-spectral matrix interferences with spatial emission profiles and gradient dilution in inductively coupled plasma-atomic emission spectrometry

Energy Technology Data Exchange (ETDEWEB)

Cheung, Yan; Schwartz, Andrew J.; Chan, George C.-Y.; Hieftje, Gary M., E-mail: hieftje@indiana.edu

2015-08-01

Matrix interference remains one of the most daunting challenges commonly encountered in inductively coupled plasma-atomic emission spectrometry (ICP-AES). In the present study, a method is described that enables identification and correction of matrix interferences in axial-viewed ICP-AES through a combination of spatial mapping and on-line gradient dilution. Cross-sectional emission maps of the plasma are used to indicate the presence of non-spectral (plasma-related and sample-introduction-related) matrix interferences. In particular, apparent concentrations of an analyte species determined at various radial locations in the plasma differ in the presence of a matrix interference, which allows the interference to be flagged. To correct for the interference, progressive, on-line dilution of the sample, performed by a gradient high-performance liquid-chromatograph pump, is utilized. The spatially dependent intensities of analyte emission are monitored at different levels of sample dilution. As the dilution proceeds, the matrix-induced signal variation is reduced. At a dilution where the determined concentrations become independent of location in the plasma, the matrix interference is minimized. - Highlights: • Non-spectral matrix interference in ICP-AES is flagged and minimized. • Emission from different locations of the plasma are collected simultaneously. • Spatially dependent determined concentrations indicate the presence of interference. • Gradient dilution is performed on both calibration standards and sample. • Optimal dilution factor to minimize interference is found as dilution increases.

Determination and pharmacokinetic properties of arsenic speciation in Xiao-Er-Zhi-Bao-Wan by high-performance liquid chromatography with inductively coupled plasma mass spectrometry.

Science.gov (United States)

Han, Xu; Luo, Jiaoyang; Zhou, Wenju; Yang, Shihai; Yang, Meihua

2016-10-01

A method of high performance liquid chromatography with a Hamilton PRP-X100 ion-exchange column (250 × 4.1 mm id, 10 μm) coupled to inductively coupled plasma mass spectrometry was employed to generate a full concentration-time profile of arsenic speciation after oral administration. The results exhibited good linearity and revealed that, in the pills, the average arsenic concentration was 10105.4 ± 380.7 mg/kg, and in the water extraction solution, the inorganic As(III) and As(V) concentrations were 220.1 ± 12.6 and 45.5 ± 2.3 mg/kg, respectively. No trace of monomethyl arsenic acid was detected in any of the plasma samples. We then successfully applied the established methodology to examine the pharmacokinetics of arsenic speciation. The resulting data revealed that, after oral administration in rats, the plasma concentration of each arsenic species reached C max shortly after initial dosing, and that the distribution and elimination of As(V) was faster than that of As(III) and dimethyl arsenic acid. Additionally, the t 1/2 values of As(V), As(III), and dimethyl arsenic acid were 3.4 ± 1.6, 14.3 ± 4.0, and 19.9 ± 1.6 h, respectively. This study provides references for the determination of arsenic speciation in mineral-containing medicines and could serve as a useful tool in measuring the true toxicity in traditional medicines that contain them. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of rare-earth elements, yttrium and scandium in manganese nodules by inductively-coupled argon-plastma emission spectrometry

Science.gov (United States)

Fries, T.; Lamothe, P.J.; Pesek, J.J.

1984-01-01

A sequential-scanning, inductively-coupled argon plasma emission spectrometer is used for the determination of the rare-earth elements, plus yttrium and scandium, in manganese nodules. Wavelength selection is optimized to minimize spectral interferences from manganese nodule components. Samples are decomposed with mixed acids in a sealed polycarbonate vessel, and elements are quantified without further treatment. Results for U.S. Geological Survey manganese nodule standards A-1 and P-1 had average relative standard deviations of 6.8% and 8.1%, respectively, and results were in good agreement with those obtained by other methods. ?? 1984.

Application of laser ablation inductively coupled plasma multicollector mass spectometry in determination of lead isotope ratios in common glass for forensic purposes

International Nuclear Information System (INIS)

Sjåstad, Knut-Endre; Andersen, Tom; Simonsen, Siri Lene

2013-01-01

Samples of glass used as trace evidence in criminal cases are commonly small, with particle sizes below a millimeter. To perform chemical analysis suitable for forensic purposes, methods capable of analyzing such small samples are required. In this paper, analyses of lead isotope ratios by means of laser ablation inductively coupled multicollector mass spectrometry (LA-MC-ICP-MS) are presented. Sampling by use of laser ablation allows fragments down to 0.1 mg to be analyzed with sufficient precision to discriminate between glasses of different origin. In fact, the use of lead isotopes determined by LA-MC-ICP-MS approaches the discrimination attainable by multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) analysis of dissolved samples of 5 mg or more. Further, we have obtained a probability distribution by two dimensional kernel density estimates for the collected data set as an alternative presentation method to the well-established bivariate plot. The underlying information available from kernel density estimates is of importance for forensic scientists involved in probabilistic interpretation of physical evidence. - Highlights: • Lead isotope ratios prove suitable to discriminate glass for forensic purposes. • 96% of glass samples from different sources were separated by lead isotopic ratios. • Laser ablation allows fragments of glass with extension of 0.5 mm to be analyzed. • Isotopic ratios of lead are well suited for statistical analysis of evidence

Simultaneous Pre-Concentration of Cadmium and Lead in Environmental Water Samples with Dispersive Liquid-Liquid Microextraction and Determination by Inductively Coupled Plasma-Atomic Emission Spectrometry

Directory of Open Access Journals (Sweden)

M. Salahinejad

2013-06-01

Full Text Available The dispersive liquid–liquid microextraction (DLLME method for determination of Pb+2 and Cd+2 ions in the environmental water samples was combined with inductively coupled plasma-atomic emission spectrometry (ICP-AES. Ammonium pyrrolidine dithiocarbamate (APDC, chloroform and ethanol were used as chelating agent, extraction solvent and disperser solvent, respectively. Some effective parameters on the microextraction and the complex formation were selected and optimized. These parameters included extraction and disperser solvent type as well as their volume, extraction time, salt effect, pH, sample volume and amount of the chelating agent.   Under the optimum conditions, the enrichment factor of 75 and 105 for Cd+2 and Pb+2 ions respectively was obtained from only 5.00mL of water sample. The detection limit (S/N=3 was 12 and 0.8ngmL−1 for Pb and Cd respectively. The relative standard deviation (RSDs for five replicate measurements of 0.50 mgL−1 of lead and cadmium was 6.5 and 4.4 % respectively. Mineral, tap, river, sea, dam and spiked water samples were analyzed for Cd and Pb amount.

Problems, possibilities and limitations of inductively coupled plasma atomic emission spectrometry in the determination of platinum, palladium and rhodium in samples with different matrix composition

Energy Technology Data Exchange (ETDEWEB)

Petrova, P.; Velichkov, S. [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria); Velitchkova, N. [Geological Institute, Bulgarian Academy of Sciences, Acad. G. Bontchev Str., bl.24, 1113 Sofia (Bulgaria); Havezov, I. [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria); Daskalova, N., E-mail: das15482@svr.igic.bas.b [Institute of General and Inorganic Chemistry, Bulgarian Academy of Sciences, Acad. G. Bontchev Str. bl. 11, 1113 Sofia (Bulgaria)

2010-02-15

The economic and geological importance of platinum group of elements has led to the development of analytical methods to quantify them in different types of samples. In the present paper the quantitative information for spectral interference in radial viewing 40.68 MHz inductively coupled plasma atomic emission spectrometry in the determination of Pt, Pd and Rh in the presence of complex matrix, containing Al, Ca, Fe, Mg, Mn, P and Ti as matrix constituents was obtained. The database was used for optimum line selections. By using the selected analysis lines the following detection limits in ng g{sup -1} were obtained: Pt 1700, Pd-1440, Rh-900. The reached detection limits determine the possibilities and limitation of the direct ICP-AES method in the determination of Pt, Pd and Rh in geological and environmental materials. The database for spectral interferences in the presence of aluminum can be used for the determination of platinum group of elements in car catalysts. The accuracy of the analytical results was experimentally demonstrated by two certified reference materials that were analyzed: SARM 7, Pt ore and recycled auto-catalyst certified reference material SRM 2556.

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

Method development for speciation analysis of nanoparticle and ionic forms of gold in biological samples by high performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry

Science.gov (United States)

Malejko, Julita; Świerżewska, Natalia; Bajguz, Andrzej; Godlewska-Żyłkiewicz, Beata

2018-04-01

A new method based on coupling high performance liquid chromatography (HPLC) to inductively coupled plasma mass spectrometry (ICP MS) has been developed for the speciation analysis of gold nanoparticles (AuNPs) and dissolved gold species (Au(III)) in biological samples. The column type, the composition and the flow rate of the mobile phase were carefully investigated in order to optimize the separation conditions. The usefulness of two polymeric reversed phase columns (PLRP-S with 100 nm and 400 nm pore size) to separate gold species were investigated for the first time. Under the optimal conditions (PLRP-S400 column, 10 mmol L-1 SDS and 5% methanol as the mobile phase, 0.5 mL min-1 flow rate), detection limits of 2.2 ng L-1 for Au(III), 2.8 ng L-1 for 10 nm AuNPs and 3.7 ng L-1 for 40 nm AuNPs were achieved. The accuracy of the method was proved by analysis of reference material RM 8011 (NIST) of gold nanoparticles of nominal diameter of 10 nm. The HPLC-ICP MS method has been successfully applied to the detection and size characterization of gold species in lysates of green algae Acutodesmus obliquus, typical representative of phytoplankton flora, incubated with 10 nm AuNPs or Au(III).

Separation of uranium and plutonium isotopes for measurement by multi collector inductively coupled plasma mass spectroscopy

International Nuclear Information System (INIS)

Martinelli, R.E.; Hamilton, T.F.; Kehl, S.R.; Williams, R.W.

2009-01-01

Uranium (U) and plutonium (Pu) isotopes in coral soils, contaminated by nuclear weapons testing in the northern Marshall Islands, were isolated by ion-exchange chromatography and analyzed by mass spectrometry. The soil samples were spiked with 233 U and 242 Pu tracers, dissolved in minerals acids, and U and Pu isotopes isolated and purified on commercially available ion-exchange columns. The ion-exchange technique employed a TEVA R column coupled to a UTEVA R column. U and Pu isotope fractions were then further isolated using separate elution schemes, and the purified fractions containing U and Pu isotopes analyzed sequentially using multi-collector inductively coupled plasma mass spectrometer (MCICP-MS). High precision measurements of 234 U/ 235 U, 238 U/ 235 U, 236 U/ 235 U, and 240 Pu/ 239 Pu in soil samples were attained using the described methodology and instrumentation, and provide a basis for conducting more detailed assessments of the behavior and transfer of uranium and plutonium in the environment. (author)

An Investigation on the Extraction and Quantitation of a Hexavalent Chromium in Acrylonitrile Butadiene Styrene Copolymer (ABS) and Printed Circuit Board (PCB) by Ion Chromatography Coupled with Inductively Coupled Plasma Atomic Emission Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Nam, Sang Ho; Kim, Yu Na [Mokpo National University, Muan (Korea, Republic of)

2012-06-15

A hexavalent chromium (Cr (VI)) is one of the hazardous substances regulated by the RoHS. The determination of Cr (VI) in various polymers and printed circuit board (PCB) has been very important. In this study, the three different analytical methods were investigated for the determination of a hexavalent chromium in Acrylonitrile Butadiene Styrene copolymer (ABS) and PCB. The results by three analytical methods were obtained and compared. An analytical method by UV-Visible spectrometer has been generally used for the determination of Cr (VI) in a sample, but a hexavalent chromium should complex with diphenylcarbazide for the detection in the method. The complexation did make an adverse effect on the quantitative analysis of Cr (VI) in ABS. The analytical method using diphenylcarbazide was also not applicable to printed circuit board (PCB) because PCB contained lots of irons. The irons interfered with the analysis of hexavalent chromium because those also could complex with diphenylcarbazide. In this study, hexavalent chromiums in PCB have been separated by ion chromatography (IC), then directly and selectively detected by inductively coupled plasma atomic emission spectrometry (ICP-AES). The quantity of Cr (VI) in PCB was 0.1 mg/kg

MRI surface-coil pair with strong inductive coupling.

Science.gov (United States)

Mett, Richard R; Sidabras, Jason W; Hyde, James S

2016-12-01

A novel inductively coupled coil pair was used to obtain magnetic resonance phantom images. Rationale for using such a structure is described in R. R. Mett et al. [Rev. Sci. Instrum. 87, 084703 (2016)]. The original rationale was to increase the Q-value of a small diameter surface coil in order to achieve dominant loading by the sample. A significant improvement in the vector reception field (VRF) is also seen. The coil assembly consists of a 3-turn 10 mm tall meta-metallic self-resonant spiral (SRS) of inner diameter 10.4 mm and outer diameter 15.1 mm and a single-loop equalization coil of 25 mm diameter and 2 mm tall. The low-frequency parallel mode was used in which the rf currents on each coil produce magnetic fields that add constructively. The SRS coil assembly was fabricated and data were collected using a tissue-equivalent 30% polyacrylamide phantom. The large inductive coupling of the coils produces phase-coherency of the rf currents and magnetic fields. Finite-element simulations indicate that the VRF of the coil pair is about 4.4 times larger than for a single-loop coil of 15 mm diameter. The mutual coupling between coils influences the current ratio between the coils, which in turn influences the VRF and the signal-to-noise ratio (SNR). Data on a tissue-equivalent phantom at 9.4 T show a total SNR increase of 8.8 over the 15 mm loop averaged over a 25 mm depth and diameter. The experimental results are shown to be consistent with the magnetic resonance theory of the emf induced by spins in a coil, the theory of inductively coupled resonant circuits, and the superposition principle. The methods are general for magnetic resonance and other types of signal detection and can be used over a wide range of operating frequencies.

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)

Speciation Analysis of Trace Mercury in Sea Cucumber Species of Apostichopus japonicus Using High-Performance Liquid Chromatography Conjunction With Inductively Coupled Plasma Mass Spectrometry.

Science.gov (United States)

Liu, Hao; Luo, Jiaoyang; Ding, Tong; Gu, Shanyong; Yang, Shihai; Yang, Meihua

2018-03-25

In this paper, a simple and cost-effective method using high-performance liquid chromatography in conjunction with inductively coupled plasma mass spectrometry with a rapid ultrasound-assisted extraction was used for analysis speciation of trace mercury in sea cucumber species of Apostichopus japonicus. The effective separation of inorganic mercury, methylmercury, and ethylmercury was achieved within 10 min using Agilent ZORBAX SB-C 18 analytical and guard columns with an isocratic mobile phase consisting of 8% methanol and 92% H 2 O containing 0.12% L-cysteine (m/v) and 0.01 mol/L ammonium acetate. Mercury species were extracted from A. japonicus samples using a solution containing 2-mercaptoethanol, L-cysteine, and hydrochloric acid and sonicating for 0.5 h. The limits of detection of inorganic mercury, methylmercury, and ethylmercury were 0.12, 0.08, and 0.20 μg/L, and the minimum detectable concentrations (measured at 0.500 g sample volume in 10.00 mL) were 2.4, 1.6, and 4.0 μg/kg, respectively. Analysis of a scallop certified reference material (GBW 10024) revealed accordance between the experimental and certified values. This study provides a reference for the evaluation of mercury speciation in sea cucumber and other seafood.

Determination of Cd, Pb, Zn and Cu in Sediment Compartments by Sequential Extraction and Isotope Dilution Inductively Coupled Plasma Mass Spectrometry (ID-ICP-MS

Directory of Open Access Journals (Sweden)

Gardolinski Paulo C. F. C.

2002-01-01

Full Text Available Trace concentrations of Cd, Cu, Pb and Zn in four different sediment fractions extracted in sequence were determined by isotope dilution inductively coupled mass spectrometry (IDICPMS. The metals from each fraction were extracted following the sequential extraction procedure recommended by the Bureau Commun de Référence (BCR of the Commission of the European Communities. As an alternative to external calibration, the elements were quantified by spiking the extracted solutions with 112Cd, 63Cu, 208Pb and 66Zn and application of isotope dilution. The proposed approach was applied to a sample collected from a lake and two standard reference materials, NIST2704 river sediment from the National Institute of Standards & Technology and the BCR-277 estuarine sediment. Detection limits, for each extracted solution, varied from 0.31 to 0.53 mug L¹ for Cd, 0.92 to 2.9 mug L¹ for Cu, 0.22 to 1.1 mug L¹ for Pb and 1.3 to 7.6 mug L¹ for Zn. The sum of the metals concentration in the different fractions was compatible with 95% confidence level found amounts obtained with complete digestion of the samples and with the certified values of the standard reference materials.

A high-throughput solid-phase extraction microchip combined with inductively coupled plasma-mass spectrometry for rapid determination of trace heavy metals in natural water.

Science.gov (United States)

Shih, Tsung-Ting; Hsieh, Cheng-Chuan; Luo, Yu-Ting; Su, Yi-An; Chen, Ping-Hung; Chuang, Yu-Chen; Sun, Yuh-Chang

2016-04-15

Herein, a hyphenated system combining a high-throughput solid-phase extraction (htSPE) microchip with inductively coupled plasma-mass spectrometry (ICP-MS) for rapid determination of trace heavy metals was developed. Rather than performing multiple analyses in parallel for the enhancement of analytical throughput, we improved the processing speed for individual samples by increasing the operation flow rate during SPE procedures. To this end, an innovative device combining a micromixer and a multi-channeled extraction unit was designed. Furthermore, a programmable valve manifold was used to interface the developed microchip and ICP-MS instrumentation in order to fully automate the system, leading to a dramatic reduction in operation time and human error. Under the optimized operation conditions for the established system, detection limits of 1.64-42.54 ng L(-1) for the analyte ions were achieved. Validation procedures demonstrated that the developed method could be satisfactorily applied to the determination of trace heavy metals in natural water. Each analysis could be readily accomplished within just 186 s using the established system. This represents, to the best of our knowledge, an unprecedented speed for the analysis of trace heavy metal ions. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of metallo-organic and particulate wear metals in lubricating oils associated with hybrid ceramic bearings by inductively coupled plasma mass spectrometry

Science.gov (United States)

Russell, Robin Ann

It is possible to increase both the performance and operating environment of jet engines by using hybrid ceramic bearings. Our laboratory is concerned with investigating lubricating fluids for wear metals associated with silicon nitride ball bearings and steel raceways. Silicon nitride is characterized by low weight, low thermal expansion, high strength, and corrosion resistance. These attributes result in longer engine lifetimes than when metallic ball bearings are used. Before the routine use of ceramic ball bearings can be realized, the wear mechanisms of the materials should be thoroughly understood. One important variable in determining wear degradation is the concentration of metal present in the lubricating oils used with the bearings. A complete method for analyzing used lubricating oils for wear metal content must accurately determine all metal forms present. Oil samples pose problems for routine analysis due to complex organic matrices. Nebulizing these types of samples into an Inductively Coupled Plasma - Mass Spectrometer introduces many problems including clogging of the sample cone with carbon and increasing interferences. In addition, other techniques such as Atomic Absorption Spectrometry and Atomic Emission Spectrometry are particle size dependent. They are unable to analyze particles greater than 10 mum in size. This dissertation describes a method of analyzing lubricating oils for both metallo-organic and particulate species by ICP-MS. Microwave digestion of the oil samples eliminates the need for elaborate sample introduction schemes as well as the use of a modified carrier gas. Al, Cr, Fe, Mg, Mo, Ni, Ti, and Y have been determined in both aqueous and organic media. Metallo-organic solutions of these metals were successfully digested, nebulized into the ICP, and the singly charged ions measured by mass spectrometry. Metal particulates in oil matrices have also been quantitatively determined by the above method. Linear analytical curves were

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.)

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.

SYSTEM OPTIMIZATION FOR THE AUTOMATIC SIMULTANEOUS DETERMINATION OF ARSENIC, SELENIUM, AND ANTIMONY, USING HYDRIDE GENERATION INTRODUCTION TO AN INDUCTIVELY COUPLED PLASMA.

Science.gov (United States)

Pyen, Grace S.; Browner, Richard F.; Long, Stephen

1986-01-01

A fixed-size simplex has been used to determine the optimum conditions for the simultaneous determination of arsenic, selenium, and antimony by hydride generation and inductively coupled plasma emission spectrometry. The variables selected for the simplex were carrier gas flow rate, rf power, viewing height, and reagent conditions. The detection limit for selenium was comparable to the preoptimized case, but there were twofold and fourfold improvements in the detection limits for arsenic and antimony, respectively. Precision of the technique was assessed with the use of artificially prepared water samples.

Plasma-related matrix effects in inductively coupled plasma--atomic emission spectrometry by group I and group II matrix-elements

International Nuclear Information System (INIS)

Chan, George C.-Y.; Chan, W.-T.

2003-01-01

The effects of Na, K, Ca and Ba matrices on the plasma excitation conditions in inductively coupled plasma-atomic emission spectrometry (ICP-AES) were studied. Normalized relative intensity was used to indicate the extent of the plasma-related matrix effects. The group I matrices have no effects on the plasma excitation conditions. In contrast, the group II matrices depress the normalized relative intensities of some spectral lines. Specifically, the Group II matrices have no effects on the normalized relative intensity of atomic lines of low upper energy level (soft lines), but reduce the normalized relative intensity of some ionic lines and atomic lines of high energy level (hard lines). The Group II matrices seem to shift the Saha balance of the analytes only; no shift in the Boltzmann balance was observed experimentally. Moreover, for some ionic lines with sum of ionization and excitation potentials close to the ionization potential of argon (15.75 eV), the matrix effect is smaller than other ionic lines of the same element. The reduced matrix effects may be attributed qualitatively to charge transfer excitation mechanism of these ionic lines. Charge transfer reaction renders ionic emission lines from the quasi-resonant levels similar in characteristics of atomic lines. The contribution of charge transfer relative to excitation by other non-specific excitation mechanisms (via Saha balance and Boltzmann balance) determines the degree of atomic behavior of a quasi-resonant level. A significant conclusion of this study is that plasma-related matrix effect depends strongly on the excitation mechanism of a spectral line. Since, in general, more than one excitation mechanism may contribute to the overall excitation of an emission line, the observed matrix effects reflect the sum of the effects due to individual excitation mechanisms. Excitation mechanisms, in addition to the often-used total excitation energy, should be considered in matrix effect studies

Accurate determination of bromine and iodine in medicinal plants by inductively coupled plasma-mass spectrometry after microwave-induced combustion

Science.gov (United States)

Nascimento, Mariele S.; Mendes, Ana Luiza G.; Henn, Alessandra S.; Picoloto, Rochele S.; Mello, Paola A.; Flores, Erico M. M.

2017-12-01

In this work, a method for the determination of bromine and iodine in medicinal plants by inductively coupled plasma mass spectrometry (ICP-MS) after digestion by microwave-induced combustion (MIC) was developed. Medicinal plants were pressed as pellets and combusted at 20 bar of oxygen. The suitability of absorbing solution (water, 50 mmol L- 1 (NH4)2CO3, 10 mmol L- 1, 25 mmol L- 1, 50 mmol L- 1 or 100 mmol L- 1 NH4OH) was evaluated and a reflux step of 5 min was applied after combustion. The accuracy of the proposed method was evaluated by using certified reference materials (CRMs) of apple leaves and peach leaves and also by spiked samples. Using 50 mmol L- 1 NH4OH as absorbing solution, recoveries close to 100% for bromine and iodine were obtained as well as a low relative standard deviation (5%). No statistical difference (t-test, 95% of confidence level) was observed between the values obtained by ICP-MS after MIC digestion and the certified values. One of the important advantages of the proposed method is that it allowed the use of a relatively high sample mass (1000 mg) of medicinal plant resulting in low limits of quantification (0.033 μg g- 1 and 0.003 μg g- 1 for Br and I, respectively). Blanks were always negligible and only diluted solutions were used, in agreement with current recommendations for analytical methods. A high digestion efficiency was achieved (> 99%) assuring quantitative results. The concentration of analytes in medicinal plants was in the range of 0.17 μg g- 1 to 53.1 μg g- 1 for Br and medicinal plants (125 μg g- 1).

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.

Flotation separation of Cd, Co, Cr, Cu, Ni and Tl from calcium minerals and their determination by inductively coupled plasma-atomic emission spectrometry

International Nuclear Information System (INIS)

Zajkova-Paneva, Vesna; Stafilov, Trajche; Boev, Blazho

2003-01-01

The method of inductively coupled plasma-atomic spectrometry (ICP-AES), is developed for determination of Cd, Co, Cr, Cu, Ni and Tl in traces in calcite and gypsum. The interferences of Ca as matrix element on Co, Cr, Cu, Ni and Tl intensities during their ICP-AES determination are investigated. The results reveal that Ca does not interfere on intensities of Cr, but tends to decrease the intensity of the other elements. To eliminate those matrix interferences of Ca on trace elements intensities a flotation separation method is proposed. Lead(II) hexamethylenedithiocarbamate, Pb(HMDTC) 2 , is applied as a collector for flotation of trace elements from acidic solutions of mineral samples. The most suitable concentrations of calcite and gypsum solutions for flotation are ascertained. The detection limits of ICP-AES method following flotation of elements present in calcite and gypsum as impurities are determined: 0.022 and 0.061 μg·g -1 for Cd, 0.071 and 0.042 μg·g -1 for Co, 0.026 and 0.132 μg·g -1 for Cr, 0.164 and 0.149 μg·g -1 for Cu, 0.289 and 0.095 μg·g -1 for Ni and 0.645 and 0.7666 μg·g -1 for Tl, respectively. (Original)

Study of uranium matrix interference on ten analytes using inductively coupled plasma atomic emission spectrometry