Ultra-trace determination of plutonium in marine samples using multi-collector inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Lindahl, Patric, E-mail: patriclindahl@yahoo.com [Marine Environment Research Department, Korea Ocean Research and Development Institute, 1270 Sadong, Ansan 426-744 (Korea, Republic of); School of Geography, Earth and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth PL48AA (United Kingdom); Keith-Roach, Miranda; Worsfold, Paul [School of Geography, Earth and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth PL48AA (United Kingdom); Choi, Min-Seok; Shin, Hyung-Seon [Division of Earth and Environmental Science, Korea Basic Science Institute, 113 Gwahangno, Yusung-gu, Daejon 305-333 (Korea, Republic of); Lee, Sang-Hoon [Marine Geology and Geophysics Laboratory, Korea Ocean Research and Development Institute, 1270 Sadong, Ansan 426-744 (Korea, Republic of)

2010-06-25

Sources of plutonium isotopes to the marine environment are well defined, both spatially and temporally, which makes Pu a potential tracer for oceanic processes. This paper presents the selection, optimisation and validation of a sample preparation method for the ultra-trace determination of Pu isotopes ({sup 240}Pu and {sup 239}Pu) in marine samples by multi-collector (MC) ICP-MS. The method was optimised for the removal of the interference from {sup 238}U and the chemical recovery of Pu. Comparison of various separation strategies using AG1-X8, TEVA, TRU, and UTEVA resins to determine Pu in marine calcium carbonate samples is reported. A combination of anion-exchange (AG1-X8) and extraction chromatography (UTEVA/TRU) was the most suitable, with a radiochemical Pu yield of 87 {+-} 5% and a U decontamination factor of 1.2 x 10{sup 4}. Validation of the method was accomplished by determining Pu in various IAEA certified marine reference materials. The estimated MC-ICP-MS instrumental limit of detection for {sup 239}Pu and {sup 240}Pu was 0.02 fg mL{sup -1}, with an absolute limit of quantification of 0.11 fg. The proposed method allows the determination of ultra-trace Pu, at femtogram levels, in small size marine samples (e.g., 0.6-2.0 g coral or 15-20 L seawater). Finally, the analytical method was applied to determining historical records of the Pu signature in coral samples from the tropical Northwest Pacific and {sup 239+240}Pu concentrations and {sup 240}Pu/{sup 239}Pu atom ratios in seawater samples as part of the 2008 GEOTRACES intercalibration exercise.

Ultra-trace determination of plutonium in marine samples using multi-collector inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Lindahl, Patric; Keith-Roach, Miranda; Worsfold, Paul; Choi, Min-Seok; Shin, Hyung-Seon; Lee, Sang-Hoon

2010-01-01

Sources of plutonium isotopes to the marine environment are well defined, both spatially and temporally, which makes Pu a potential tracer for oceanic processes. This paper presents the selection, optimisation and validation of a sample preparation method for the ultra-trace determination of Pu isotopes ( 240 Pu and 239 Pu) in marine samples by multi-collector (MC) ICP-MS. The method was optimised for the removal of the interference from 238 U and the chemical recovery of Pu. Comparison of various separation strategies using AG1-X8, TEVA, TRU, and UTEVA resins to determine Pu in marine calcium carbonate samples is reported. A combination of anion-exchange (AG1-X8) and extraction chromatography (UTEVA/TRU) was the most suitable, with a radiochemical Pu yield of 87 ± 5% and a U decontamination factor of 1.2 x 10 4 . Validation of the method was accomplished by determining Pu in various IAEA certified marine reference materials. The estimated MC-ICP-MS instrumental limit of detection for 239 Pu and 240 Pu was 0.02 fg mL -1 , with an absolute limit of quantification of 0.11 fg. The proposed method allows the determination of ultra-trace Pu, at femtogram levels, in small size marine samples (e.g., 0.6-2.0 g coral or 15-20 L seawater). Finally, the analytical method was applied to determining historical records of the Pu signature in coral samples from the tropical Northwest Pacific and 239+240 Pu concentrations and 240 Pu/ 239 Pu atom ratios in seawater samples as part of the 2008 GEOTRACES intercalibration exercise.

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

Science.gov (United States)

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

2018-03-24

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

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

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Brian Gulson

2018-04-01

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

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

Science.gov (United States)

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

2018-04-11

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

Improved precision and speed of thermal ionisation mass spectrometry with a multicollector

International Nuclear Information System (INIS)

Turner, P.J.; Cantle, J.E.; Haines, R.C.

1984-01-01

The analytical accuracy of uranium analysis is limited by fractionation occuring before and during the data acquisition period. With peak jumping methods, increasing the data measuring period beyond 15 to 20 minutes can result in a deteriorating, internal precision because the ratio being measured is changing significantly. In addition the operator often has the choice of taking poor data when the beam is unstable or decaying rapidly or waiting for beam stability and measuring a more fractionated ratio to higher precision. Either way measurement accuracy is reduced. Simultaneous measurement of the ion beams using a multicollector greatly eases these difficulties. Multicollector analysis offers the following advantages for uranium analysis: (1) greatly reduced analysis time; (2) improved internal errors duing data acquisition allowing: (a) smaller samples to be measured, (b) greater dynamic ratios to be measured before internal errors become comparable to the external errors; (3) short data acquisition time giving better results on rapidly fractionating samples; (4) great tolerance to unstable and rapidly decaying beams resulting in fewer ''unsatisfactory'' analyses. 4 figs

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

Science.gov (United States)

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

2012-01-01

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

Lead isotope measurements on aerosol samples with ICP-MS

International Nuclear Information System (INIS)

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

2000-01-01

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

Separation of Platinum from Palladium and Iridium in Iron Meteorites and Accurate High-Precision Determination of Platinum Isotopes by Multi-Collector ICP-MS.

Science.gov (United States)

Hunt, Alison C; Ek, Mattias; Schönbächler, Maria

2017-12-01

This study presents a new measurement procedure for the isolation of Pt from iron meteorite samples. The method also allows for the separation of Pd from the same sample aliquot. The separation entails a two-stage anion-exchange procedure. In the first stage, Pt and Pd are separated from each other and from major matrix constituents including Fe and Ni. In the second stage, Ir is reduced with ascorbic acid and eluted from the column before Pt collection. Platinum yields for the total procedure were typically 50-70%. After purification, high-precision Pt isotope determinations were performed by multi-collector ICP-MS. The precision of the new method was assessed using the IIAB iron meteorite North Chile. Replicate analyses of multiple digestions of this material yielded an intermediate precision for the measurement results of 0.73 for ε 192 Pt, 0.15 for ε 194 Pt and 0.09 for ε 196 Pt (2 standard deviations). The NIST SRM 3140 Pt solution reference material was passed through the measurement procedure and yielded an isotopic composition that is identical to the unprocessed Pt reference material. This indicates that the new technique is unbiased within the limit of the estimated uncertainties. Data for three iron meteorites support that Pt isotope variations in these samples are due to exposure to galactic cosmic rays in space.

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.

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

Interhemispheric controls on deep ocean circulation and carbon chemistry during the last two glacial cycles

Digital Repository Service at National Institute of Oceanography (India)

Wilson, D.J.; Galy, A.; Piotrowski, A.M.; Banakar, V.K.

composition was analysed on the Nu Plasma multi-collector inductively-coupled plasma mass spectrometer (MC-ICP-MS) in the Department of Earth Sciences at the University of Cambridge, using an exponential mass fractionation correction (to 146Nd/144Nd = 0...

Measurement of inclusion size by laser ablation ICP mass spectrometry

International Nuclear Information System (INIS)

Karasev, Andrey V.; Suito, Hideaki

2004-01-01

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

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

{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.

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

International Nuclear Information System (INIS)

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

1989-01-01

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

An overview of the LAM-MC-ICP MS national facility: prospects and priorities. PD-3-1

International Nuclear Information System (INIS)

Bhaskar Rao, Y.J.; Vijaya Gopal, B.; Babu, E.V.S.S.K.; Sukumaran, N.P.; Sreenivas, B.; Vijaya Kumar, T.; Krishna, K.V.S.S.; Tomson, J.K.

2007-01-01

Unraveling the complex history of earth and other planetary bodies is a fundamental challenge to all earth scientists. Trace element distributions and isotopic variations in terrestrial rocks and minerals, materials from the Moon, and other inaccessible parts of the Universe as represented in meteorites hold the key to understanding many planetary and earth processes. At the same time, high precision isotopic data on samples of the Earth's hydrosphere and biosphere are important to understanding Man's habitat and environment. The fact that these natural processes operate on a range of scales in space and time necessitates isotopic composition measurements of many responsive and geochemically distinct trace elements including several naturally radioactive parent and radiogenic daughter isotope systems with half-lives between 10 3 -10 15 years and isotopes of many non-radiogenic (stable) elements as well. This article forms a brief introduction to the instrumentation, capabilities and some current priority projects of the Laser Ablation Microprobe (LAM)-Multicollector Inductively Coupled Plasma Mass Spectrometer (MC-ICP MS) National Facility

Sulfate and sulfide sulfur isotopes (δ34S and δ33S) measured by solution and laser ablation MC-ICP-MS: An enhanced approach using external correction

Science.gov (United States)

Pribil, Michael; Ridley, William I.; Emsbo, Poul

2015-01-01

Isotope ratio measurements using a multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS) commonly use standard-sample bracketing with a single isotope standard for mass bias correction for elements with narrow-range isotope systems measured by MC-ICP-MS, e.g. Cu, Fe, Zn, and Hg. However, sulfur (S) isotopic composition (δ34S) in nature can range from at least − 40 to + 40‰, potentially exceeding the ability of standard-sample bracketing using a single sulfur isotope standard to accurately correct for mass bias. Isotopic fractionation via solution and laser ablation introduction was determined during sulfate sulfur (Ssulfate) isotope measurements. An external isotope calibration curve was constructed using in-house and National Institute of Standards and Technology (NIST) Ssulfate isotope reference materials (RM) in an attempt to correct for the difference. The ability of external isotope correction for Ssulfate isotope measurements was evaluated by analyzing NIST and United States Geological Survey (USGS) Ssulfate isotope reference materials as unknowns. Differences in δ34Ssulfate between standard-sample bracketing and standard-sample bracketing with external isotope correction for sulfate samples ranged from 0.72‰ to 2.35‰ over a δ34S range of 1.40‰ to 21.17‰. No isotopic differences were observed when analyzing Ssulfide reference materials over a δ34Ssulfide range of − 32.1‰ to 17.3‰ and a δ33S range of − 16.5‰ to 8.9‰ via laser ablation (LA)-MC-ICP-MS. Here, we identify a possible plasma induced fractionation for Ssulfate and describe a new method using external isotope calibration corrections using solution and LA-MC-ICP-MS.

Limitation of secondary electron multiplier non-linearity on accurate U-Th isotopic determination by MC-ICP-MS

Science.gov (United States)

Shen, C.; Wu, C.; Gallet, S.; Cheng, H.; Edwards, R.; Hsieh, Y.; Lin, K.

2008-12-01

Contemporary multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS) with discrete dynode secondary electron multipliers (SEMs) can offer U-Th isotopic determinations with subpermil-permil- level precision in femtogram quantities. However, accurate isotopic measurement requires fully understanding SEM mass and intensity biases. In additional to dead-time effect, Richter et al (2001, Int. J. Mass Spectrom., 206, 105-127) reported a nonlinearity on SEMs produced by ETP and MasCom for count rates > 20 thousand counts per second (cps). We evaluated the possible biases for ion beams of 500- 1,600,000 cps on a latest MasCom SEM, SEV TE-Z/17, with more effective ion optical acceptance area (>50%) and better peak shape than previous models, used in a MC-ICP-MS, Thermo Fisher NEPTUNE. With the retarding potential quadruple lens (RPQ) turned off, ion beam intensity can be biased by only dead- time effect, which can be precisely corrected online or offline. With the RPQ on, two additional biases, an exponential-like increase of ion beam intensity from 100-100,000 s cps and an apparent dead-time effect (-2 to 2 ns) at high count rates, are observed. They are likely caused by the slightly defocused ions with a wide kinetic energy spread of ~5 eV, 10 times worse than that with thermal source, passing through the RPQ lens to the SEM, which is installed behind the focal plane. Fortunately, the two biases, which are stable during the daily measurements with the same settings of inlet system, source lenses, zoom optics, and RPQ, can be corrected effectively offline to earn accurate U-Th isotopic measurement.

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

Science.gov (United States)

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

2017-10-02

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-06-15

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

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.

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

International Nuclear Information System (INIS)

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

1996-01-01

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

87Sr/86Sr isotope ratio analysis by laser ablation MC-ICP-MS in scales, spines, and fin rays as a nonlethal alternative to otoliths for reconstructing fish life history

Science.gov (United States)

Willmes, Malte; Glessner, Justin J. G.; Carleton, Scott A.; Gerrity, Paul C.; Hobbs, James A.

2016-01-01

Strontium isotope ratios (87Sr/86Sr) in otoliths are a well-established tool to determine origins and movement patterns of fish. However, otolith extraction requires sacrificing fish, and when working with protected or endangered species, the use of nonlethal samples such as scales, spines, and fin rays is preferred. Unlike otoliths that are predominantly aragonite, these tissues are composed of biological apatite. Laser ablation multicollector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) analysis of biological apatite can induce significant interference on mass 87, causing inaccurate 87Sr/86Sr measurements. To quantify this interference, we applied LA-MC-ICP-MS to three marine samples (white seabass (Atractoscion nobilis) otolith; green sturgeon (Acipenser medirostris) pectoral fin ray; salmon shark (Lamna ditropis) tooth), and freshwater walleye (Sander vitreus) otoliths, scales, and spines). Instrument conditions that maximize signal intensity resulted in elevated 87Sr/86Sr isotope ratios in the bioapatite samples, related to a polyatomic interference (40Ca31P16O, 40Ar31P16O). Retuning instrument conditions to reduce oxide levels removed this interference, resulting in accurate 87Sr/86Sr ratios across all tissue samples. This method provides a novel, nonlethal alternative to otolith analysis to reconstruct fish life histories.

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

International Nuclear Information System (INIS)

Mohammed, A.E.W.M.

2013-01-01

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

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

International Nuclear Information System (INIS)

Peng Zicheng; Nie Baofu; Chen Tegu

2004-01-01

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

Use of plasma-source multicollector magnetic-sector mass spectrometry for uranium and plutonium analysis in environmental samples

International Nuclear Information System (INIS)

Price Russ, G.; Williams, Ross

2001-01-01

Full text: The ability to detect and isotopically characterize uranium and plutonium in environmental samples is of primary importance in the search for nuclear proliferation. The utility of isotope ratio measurements for environmental monitoring is limited by sample preparation costs, measurement precision, and sensitivity. This is particularly true for wide-area monitoring where the number of samples required varies inversely with obtainable precision and sensitivity. Historically isotopic measurements have been made by thermal ionization mass spectrometry (TIMS). While requiring extensive sample preparation, no other technique matched its precision and sensitivity for such measurements. Inductively-coupled-plasma, magnetic-sector, multicollector, mass spectrometry offers the prospect of extending the state-of-the-art to higher precision while increasing sensitivity and reducing costs through more rapid analysis and reduced sample preparation. At LLNL this technique is being implemented in the form of an IsoProbe (Micromass, UK). This paper will present data for both standards and IAEA supplied samples demonstrating the power and limitations of the technique. The precision and sensitivity of the IsoProbe results will be compared to TIMS performance for comparable samples. For 48 determinations of natural uranium, using the double spike to correct for bias, a relative standard deviation of 0.04% (1σ) for 238 U/ 235 U has been obtained in a preliminary study. This is a substantial improvement over the TIMS result of 0.1% reported at the previous conference. Further improvements can be expected as we gain a better understanding of the background peaks occurring in the IsoProbe spectra. (author)

Measurement of the delta34S value in methionine by double spike multi-collector thermal ionization mass spectrometry using Carius tube digestion.

Science.gov (United States)

Mann, Jacqueline L; Kelly, W Robert

2010-09-15

Methionine is an essential amino acid and is the primary source of sulfur for humans. Using the double spike ((33)S-(36)S) multi-collector thermal ionization mass spectrometry (MC-TIMS) technique, three sample bottles of a methionine material obtained from the Institute for Reference Materials and Measurements have been measured for delta(34)S and sulfur concentration. The mean delta(34)S value, relative to Vienna Canyon Diablo Troilite (VCDT), determined was 10.34 +/- 0.11 per thousand (n = 9) with the uncertainty reported as expanded uncertainties (U). These delta(34)S measurements include a correction for blank which has been previously ignored in studies of sulfur isotopic composition. The sulfur concentrations for the three bottles range from 56 to 88 microg/g. The isotope composition and concentration results demonstrate the high accuracy and precision of the DS-MC-TIMS technique for measuring sulfur in methionine.

My 25 years of experience in CPMS: applications in geochemical, mineral exploration, environment, nuclear, food, petroleum, pharmaceutical and industry sectors

International Nuclear Information System (INIS)

Balaram, V.

2012-01-01

A unique instrument incorporating an inductively coupled plasma (ICP) source and a double focusing magnetic sector high resolution mass analyzer (HR-ICP- MS) has been developed, having a practical resolving power of about 10000 or more whilst also achieving high sensitivity (Bradshaw et al, 1989). During this period, techniques like multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) and sensitive high resolution ion micro probe (SHRIMP), etc., have brought in the analytical revolution by taking the detection limits for several elements to parts per quadrillion (ppq) levels and the isotope ratio precisions to <0.001% RSD. These advances have contributed to the pioneering research in several areas of science and technology during the last six decades

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

Science.gov (United States)

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

2005-01-01

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

Application of enriched stable isotopes as tracers in biological systems

DEFF Research Database (Denmark)

Stürup, Stefan; Hansen, Helle Rüsz; Gammelgaard, Bente

2008-01-01

The application of enriched stable isotopes of minerals and trace elements as tracers in biological systems is a rapidly growing research field that benefits from the many new developments in inorganic mass spectrometric instrumentation, primarily within inductively coupled plasma mass spectrometry...... (ICP-MS) instrumentation, such as reaction/collision cell ICP-MS and multicollector ICP-MS with improved isotope ratio measurement and interference removal capabilities. Adaptation and refinement of radioisotope tracer experiment methodologies for enriched stable isotope experiments......, and the development of new methodologies coupled with more advanced compartmental and mathematical models for the distribution of elements in living organisms has enabled a broader use of enriched stable isotope experiments in the biological sciences. This review discusses the current and future uses of enriched...

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.

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

International Nuclear Information System (INIS)

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

1994-01-01

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

In situ Sr/Sr investigation of igneous apatites and carbonates using laser-ablation MC-ICP-MS

DEFF Research Database (Denmark)

Bizzarro, Martin; Simonetti, A.; Stevenson, R.K.

2003-01-01

In situ Sr isotopic compositions of coexisting apatite and carbonate for carbonatites from the Sarfartoq alkaline complex, Greenland, have been determined by laser-ablation multicollector inductively coupled plasma mass spectrometry. This study is the first to examine the extent of Sr isotopic ho...

Non-linear signal response functions and their effects on the statistical and noise cancellation properties of isotope ratio measurements by multi-collector plasma mass spectrometry

International Nuclear Information System (INIS)

Doherty, W.

2013-01-01

A nebulizer-centric response function model of the analytical inductively coupled argon plasma ion source was used to investigate the statistical frequency distributions and noise reduction factors of simultaneously measured flicker noise limited isotope ion signals and their ratios. The response function model was extended by assuming i) a single gaussian distributed random noise source (nebulizer gas pressure fluctuations) and ii) the isotope ion signal response is a parabolic function of the nebulizer gas pressure. Model calculations of ion signal and signal ratio histograms were obtained by applying the statistical method of translation to the non-linear response function model of the plasma. Histograms of Ni, Cu, Pr, Tl and Pb isotope ion signals measured using a multi-collector plasma mass spectrometer were, without exception, negative skew. Histograms of the corresponding isotope ratios of Ni, Cu, Tl and Pb were either positive or negative skew. There was a complete agreement between the measured and model calculated histogram skew properties. The nebulizer-centric response function model was also used to investigate the effect of non-linear response functions on the effectiveness of noise cancellation by signal division. An alternative noise correction procedure suitable for parabolic signal response functions was derived and applied to measurements of isotope ratios of Cu, Ni, Pb and Tl. The largest noise reduction factors were always obtained when the non-linearity of the response functions was taken into account by the isotope ratio calculation. Possible applications of the nebulizer-centric response function model to other types of analytical instrumentation, large amplitude signal noise sources (e.g., lasers, pumped nebulizers) and analytical error in isotope ratio measurements by multi-collector plasma mass spectrometry are discussed. - Highlights: ► Isotope ion signal noise is modelled as a parabolic transform of a gaussian variable. ► Flicker

Characterization of spent nuclear fuels by an online combination of chromatographic and mass spectrometric techniques

International Nuclear Information System (INIS)

Guenther-Leopold, Ines; Wernli, Beat; Kopajtic, Zlatko

2003-01-01

The determination of the burn-up is one of the essential parts in post-irradiation examinations on nuclear fuel samples. In the frame of national and international research programs the analysis of the isotopic vectors of uranium, plutonium, neodymium and some other fission products and actinides was carried out in the Hot lab of the Paul Scherrer Institute in the last years by using high-performance liquid chromatography coupled online with an inductively coupled plasma quadrupole mass spectrometer. In the meantime a multicollector ICP-MS, suitable for high precision isotope ratio measurements, was installed within the Hot lab and has been used now in combination with a chromatographic separation system for the first time for burn-up determinations of nuclear fuel samples. The results of these investigations, a comparison of both methods with the classical technique for burn-up analyses (thermal ionization mass spectrometry), the advantages and limitations of the methods and the accuracy and precision of this type of analyses are presented in the paper. (author)

Isotope pattern deconvolution as a tool to study iron metabolism in plants.

Science.gov (United States)

Rodríguez-Castrillón, José Angel; Moldovan, Mariella; García Alonso, J Ignacio; Lucena, Juan José; García-Tomé, Maria Luisa; Hernández-Apaolaza, Lourdes

2008-01-01

Isotope pattern deconvolution is a mathematical technique for isolating distinct isotope signatures from mixtures of natural abundance and enriched tracers. In iron metabolism studies measurement of all four isotopes of the element by high-resolution multicollector or collision cell ICP-MS allows the determination of the tracer/tracee ratio with simultaneous internal mass bias correction and lower uncertainties. This technique was applied here for the first time to study iron uptake by cucumber plants using 57Fe-enriched iron chelates of the o,o and o,p isomers of ethylenediaminedi(o-hydroxyphenylacetic) acid (EDDHA) and ethylenediamine tetraacetic acid (EDTA). Samples of root, stem, leaves, and xylem sap, after exposure of the cucumber plants to the mentioned 57Fe chelates, were collected, dried, and digested using nitric acid. The isotopic composition of iron in the samples was measured by ICP-MS using a high-resolution multicollector instrument. Mass bias correction was computed using both a natural abundance iron standard and by internal correction using isotope pattern deconvolution. It was observed that, for plants with low 57Fe enrichment, isotope pattern deconvolution provided lower tracer/tracee ratio uncertainties than the traditional method applying external mass bias correction. The total amount of the element in the plants was determined by isotope dilution analysis, using a collision cell quadrupole ICP-MS instrument, after addition of 57Fe or natural abundance Fe in a known amount which depended on the isotopic composition of the sample.

Isotope pattern deconvolution as a tool to study iron metabolism in plants

Energy Technology Data Exchange (ETDEWEB)

Rodriguez-Castrillon, Jose A.; Moldovan, Mariella; Garcia Alonso, J.I. [University of Oviedo, Department of Physical and Analytical Chemistry, Oviedo (Spain); Lucena, Juan J.; Garcia-Tome, Maria L.; Hernandez-Apaolaza, Lourdes [Autonoma University of Madrid, Department of Agricultural Chemistry, Madrid (Spain)

2008-01-15

Isotope pattern deconvolution is a mathematical technique for isolating distinct isotope signatures from mixtures of natural abundance and enriched tracers. In iron metabolism studies measurement of all four isotopes of the element by high-resolution multicollector or collision cell ICP-MS allows the determination of the tracer/tracee ratio with simultaneous internal mass bias correction and lower uncertainties. This technique was applied here for the first time to study iron uptake by cucumber plants using {sup 57}Fe-enriched iron chelates of the o,o and o,p isomers of ethylenediaminedi(o-hydroxyphenylacetic) acid (EDDHA) and ethylenediamine tetraacetic acid (EDTA). Samples of root, stem, leaves, and xylem sap, after exposure of the cucumber plants to the mentioned {sup 57}Fe chelates, were collected, dried, and digested using nitric acid. The isotopic composition of iron in the samples was measured by ICP-MS using a high-resolution multicollector instrument. Mass bias correction was computed using both a natural abundance iron standard and by internal correction using isotope pattern deconvolution. It was observed that, for plants with low {sup 57}Fe enrichment, isotope pattern deconvolution provided lower tracer/tracee ratio uncertainties than the traditional method applying external mass bias correction. The total amount of the element in the plants was determined by isotope dilution analysis, using a collision cell quadrupole ICP-MS instrument, after addition of {sup 57}Fe or natural abundance Fe in a known amount which depended on the isotopic composition of the sample. (orig.)

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

Science.gov (United States)

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

2017-12-01

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

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

International Nuclear Information System (INIS)

Fortunato, G.; Wunderli, S.

2003-01-01

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

Accurate and precise 40Ar/39Ar dating by high-resolution, multi-collection, mass spectrometry

DEFF Research Database (Denmark)

Storey, Michael; Rivera, Tiffany; Flude, Stephanie

New generation, high resolution, multi-collector noble gas mass spectrometers equipped with ion-counting electron multipliers provide opportunities for improved accuracy and precision in 40Ar/39Ar dating. Here we report analytical protocols and age cross-calibration studies using a NU-Instruments......New generation, high resolution, multi-collector noble gas mass spectrometers equipped with ion-counting electron multipliers provide opportunities for improved accuracy and precision in 40Ar/39Ar dating. Here we report analytical protocols and age cross-calibration studies using a NU......-Instruments multi-collector Noblesse noble gas mass spectrometer configured with a faraday detector and three ion-counting electron multipliers. The instrument has the capability to measure several noble gas isotopes simultaneously and to change measurement configurations instantaneously by the use of QUAD lenses...... (zoom optics). The Noblesse offer several advantages over previous generation noble gas mass spectrometers and is particularly suited for single crystal 40Ar/39Ar dating because of: (i) improved source sensitivity (ii) ion-counting electron multipliers, which have much lower signal to noise ratios than...

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.

High-precision measurement of mercury isotope ratios in sediments using cold-vapor generation multi-collector inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

Foucher, Delphine; Hintelmann, Holger

2006-01-01

An on-line Hg reduction technique using stannous chloride as the reductant was applied for accurate and precise mercury isotope ratio determinations by multi-collector (MC)-ICP/MS. Special attention has been paid to ensure optimal conditions (such as acquisition time and mercury concentration) allowing precision measurements good enough to be able to significantly detect the anticipated small differences in Hg isotope ratios in nature. Typically, internal precision was better than 0.002% (1 RSE) on all Hg ratios investigated as long as approximately 20 ng of Hg was measured with a 10-min acquisition time. Introducing higher amounts of mercury (50 ng Hg) improved the internal precision to 205 Tl/ 203 Tl correction coupled to a standard-sample bracketing approach. The large number of data acquired allowed us to validate the consistency of our measurements over a one-year period. On average, the short-term uncertainty determined by repeated runs of NIST SRM 1641d Hg standard during a single day was 202 Hg/ 198 Hg, 202 Hg/ 199 Hg, 202 Hg/ 200 Hg, and 202 Hg/ 201 Hg). The precision fell to 202 Hg/ 198 Hg expressed as δ values (per mil deviations relative to NIST SRM 1641d Hg standard solution) displayed differences from +0.74 to -4.00 permille. The magnitude of the Hg fractionation per amu was constant within one type of sample and did not exceed 1.00 permille. Considering all results (the reproducibility of Hg standard solutions, reference sediment samples, and the examination of natural samples), the analytical error of our δ values for the overall method was within ±0.28 permille (1 SD), which was an order of magnitude lower than the extent of fractionation (4.74 permille) observed in sediments. This study confirmed that analytical techniques have reached a level of long-term precision and accuracy that is sufficiently sensitive to detect even small differences in Hg isotope ratios that occur within one type of samples (e.g., between different sediments) and so

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.

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

International Nuclear Information System (INIS)

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

2002-01-01

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

Development of ICP-MS and ICP-OES methods for determination of gadolinium in samples related to hospital waste water treatment

Czech Academy of Sciences Publication Activity Database

Bendakovská, L.; Krejčovská, A.; Černohorský, T.; Zelenková, Jana

2016-01-01

Roč. 70, č. 9 (2016), s. 1155-1165 ISSN 0366-6352 Institutional support: RVO:67985874 Keywords : gadolinium * rare-earth elements * bioaccumulation * gadolinium anomaly * inductively coupled plasma mass spectrometry (ICP-MS) * inductively coupled plasma optical emission spectrometry (ICP-OES) Subject RIV: BK - Fluid Dynamics Impact factor: 1.258, year: 2016

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-07-01

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

ICP magnetic sector multiple collector mass spectrometry and the precise measurement of isotopic compositions using nebulization of solutions and laser ablation of solids

International Nuclear Information System (INIS)

Halliday, A.N.; Lee, D-C.; Christensen, J.N.; Yi, W.; Hall, C.M.; Jones, C.E.; Teagle, D.A.H.; Freedman, P.A.

1996-01-01

Inductively-coupled plasma (ICP) sources offer considerable advantages over thermal sources because the high ionization efficiency facilitates measurements of relatively high sensitivity for elements such as Hf or Sn, which can be difficult to measure precisely with thermal ionization mass spectrometry (TIMS). The mass discrimination (bias) is larger than for TIMS, favours the heavier ions, and decreases in magnitude with increasing mass. However, in contrast to TIMS, this discrimination is largely independent of the chemical or physical properties of the element or the duration of the analysis. This has been demonstrated to high precision with a double focussing multiple collector magnetic sector mass spectrometer with an ICP source. The principle of this instrument is briefly described. The potential of the instrument for high precision isotopic measurements of a very broad range of elements, using solution aspiration or laser ablation, is indicated. 15 refs

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

Energy Technology Data Exchange (ETDEWEB)

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

2002-09-01

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

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

Quality control of Al alloy by ICP-MS

International Nuclear Information System (INIS)

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

2000-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-07-04

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

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

International Nuclear Information System (INIS)

Ohno, Takeshi; Muramatsu, Yasuyuki

2015-01-01

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

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

Science.gov (United States)

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

2016-05-30

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-09-28

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

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

Multielement determination and speciation of major-to-ultratrace elements in green tea leaves by ICP-AES and ICP-MS

International Nuclear Information System (INIS)

Matsuura, Hirotaka; Hokura, Akiko; Haraguchi, Hiroki

2000-01-01

In order to investigate the multi-elemental composition of green tea leaves as well as chemical species in tea infusions, inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS) were used for elemental analysis and elemental speciation with the aid of size exclusion chromatography (SEC). As a result, the multielement determination of major-to-ultratrace elements in green tea leaves and green tea infusions was carried out by ICP-AES and ICP-MS. About 40 elements in these tea samples could be determined in a wide concentration range of over 8 orders of magnitude. The extraction efficiency of each element was estimated as the ratio of its concentration in tea infusion to that in tea leaves. It was found from the experimental results that the elements in tea leaves could be classified into three characteristic groups, depending on their extraction efficiencies. Furthermore, tea infusions were analyzed by a combined system of SEC, UV absorption detector, and ICP-AES (or ICP-MS) for the speciation of major-to-ultratrace elements. Most of the elements in tea infusions were found to be present as associated complexes with large organic molecules. (author)

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

ICP-MS analysis for long-lived radionuclides

International Nuclear Information System (INIS)

Roos, P.

2010-01-01

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

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

Science.gov (United States)

Linscheid, Michael W

2018-03-30

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

Classifying wine according to geographical origin via quadrupole-based ICP-mass spectrometry measurements of boron isotope ratios

Energy Technology Data Exchange (ETDEWEB)

Coetzee, Paul P. [University of Johannesburg, Department of Chemistry, Johannesburg (South Africa); Vanhaecke, Frank [Institute for Nuclear Sciences, Laboratory of Analytical Chemistry Ghent University, Ghent (Belgium)

2005-11-01

The potential of quadrupole-based ICP-MS as a tool for B-isotopic analysis of wines and its usefulness in provenance determinations were assessed. A precision of 0.1-0.25% RSD (corresponding to a relative standard deviation of the mean of three replicate measurements of 0.06-0.12%) was sufficient to establish small differences in the B isotope ratios in wines from different geographical origins. Each sample measurement was bracketed by measurements of a standard and mass bias drift correction made by interpolation. Sample preparation was kept to a minimum to avoid possible fractionation. Dilution of the wine samples by a factor of 100 with 0.65% HNO{sub 3} was found to reduce matrix-induced mass discrimination substantially. Wines from three wine-producing regions, Stellenbosch, Robertson, and Swartland, in the Western Cape Province of South Africa, and wines from specific regions in France (Bergerac) and Italy (Valpolicella) were analyzed by ICP-QMS for their B-isotopic compositions. It was concluded that the {sup 11}B/{sup 10}B ratios can be used to characterize wines from different geographical origins. Average {sup 11}B/{sup 10}B ratios in red wines from South Africa (Stellenbosch), France (Bergerac), and Italy (Valpolicella) were found to differ by between 0.5 and 1.5%. (orig.)

Classifying wine according to geographical origin via quadrupole-based ICP-mass spectrometry measurements of boron isotope ratios

International Nuclear Information System (INIS)

Coetzee, Paul P.; Vanhaecke, Frank

2005-01-01

The potential of quadrupole-based ICP-MS as a tool for B-isotopic analysis of wines and its usefulness in provenance determinations were assessed. A precision of 0.1-0.25% RSD (corresponding to a relative standard deviation of the mean of three replicate measurements of 0.06-0.12%) was sufficient to establish small differences in the B isotope ratios in wines from different geographical origins. Each sample measurement was bracketed by measurements of a standard and mass bias drift correction made by interpolation. Sample preparation was kept to a minimum to avoid possible fractionation. Dilution of the wine samples by a factor of 100 with 0.65% HNO 3 was found to reduce matrix-induced mass discrimination substantially. Wines from three wine-producing regions, Stellenbosch, Robertson, and Swartland, in the Western Cape Province of South Africa, and wines from specific regions in France (Bergerac) and Italy (Valpolicella) were analyzed by ICP-QMS for their B-isotopic compositions. It was concluded that the 11 B/ 10 B ratios can be used to characterize wines from different geographical origins. Average 11 B/ 10 B ratios in red wines from South Africa (Stellenbosch), France (Bergerac), and Italy (Valpolicella) were found to differ by between 0.5 and 1.5%. (orig.)

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

International Nuclear Information System (INIS)

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

2002-01-01

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

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Nuclear Forensics: Measurements of Uranium Oxides Using Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS)

Science.gov (United States)

2010-03-01

Isotope Ratio Analysis of Actinides , Fission Products, and Geolocators by High- efficiency Multi-collector Thermal Ionization Mass Spectrometry...Information, 1999. Hou, Xiaolin, and Per Roos. “ Critical Comparison of radiometric and Mass Spectrometric Methods for the Determination of...NUCLEAR FORENSICS: MEASUREMENTS OF URANIUM OXIDES USING TIME-OF-FLIGHT SECONDARY ION MASS

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

Science.gov (United States)

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

2008-04-01

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

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...

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.

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

International Nuclear Information System (INIS)

Schlagenhaufen, C.

1996-08-01

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

高分解能ICP-MSの特徴とその測定例<総説 レビュー>

OpenAIRE

石井, 清孝

2000-01-01

At present, there are two kind of the instruments of ICP-MS. One is HR-ICP-MS that used double focusing mass spectrometer the other one is Q-ICP-MS that used a quadrupole mass spectrometer. HR-ICP-MS has many characteristics in comparison with Q-ICP-MS. It is reported of the HR-ICP-MS structure and characteristics and also reported one of the examples of the measurement that made the most of the characteristic of it’s high resolving power in this time.概要：現在，一般的に使用されているICP-MS にはその分光器に四重極形質量分析計...

40Ar/39Ar dating of Quaternary volcanic ashes by multi-collection noble gas mass spectrometry: protocols, precision and intercalibration

DEFF Research Database (Denmark)

Storey, Michael; Rivera, Tiffany; Flude, Stephanie

) higher mass resolution allows hydrocarbon interferences to be pseudo resolved for the different argon isotopes; and (iv) multi-collection, allowing more data to be gathered in a fixed time in comparison with single-collector peak-switching measurements. We evaluate (i) protocols for detector inter......The recent availability of commercial high-resolution, multi-collector, noble gas mass spectrometers equipped with ion-counting electron multipliers provides new opportunities for improved precision in 40Ar/39Ar dating. This is particularly true for single crystal dating of Quaternary aged samples...... where potassium-bearing phenocrysts may contain relatively small amounts of radiogenic 40Ar. In 2005, the Quaternary Dating Laboratory, Roskilde University, installed a Nu-Instruments multi-collector Noblesse noble gas mass spectrometer, which is configured with a Faraday detector and three ion...

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

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

Science.gov (United States)

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

2003-02-01

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

Fit for purpose validated method for the determination of the strontium isotopic signature in mineral water samples by multi-collector inductively coupled plasma mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Brach-Papa, Christophe; Van Bocxstaele, Marleen; Ponzevera, Emmanuel [European Commission - Joint Research Centre - Institute for Reference Materials and Measurements, Retieseweg 111 - 2440 Geel (Belgium); Quetel, Christophe R. [European Commission - Joint Research Centre - Institute for Reference Materials and Measurements, Retieseweg 111 - 2440 Geel (Belgium)], E-mail: christophe.quetel@ec.europa.eu

2009-03-15

A robust method allowing the routine determination of n({sup 87}Sr)/n({sup 86}Sr) with at least five significant decimal digits for large sets of mineral water samples is described. It is based on 2 consecutive chromatographic separations of Sr associated to multi-collector inductively coupled plasma mass spectrometry (MC-ICPMS) measurements. Separations are performed using commercial pre-packed columns filled with 'Sr resin' to overcome isobaric interferences affecting the determination of strontium isotope ratios. The careful method validation scheme applied is described. It included investigations on all parameters influencing both chromatographic separations and MC-ICPMS measurements, and also the test on a synthetic sample made of an aliquot of the NIST SRM 987 certified reference material dispersed in a saline matrix to mimic complex samples. Correction for mass discrimination was done internally using the n({sup 88}Sr)/n({sup 86}Sr) ratio. For comparing mineral waters originating from different geological backgrounds or identifying counterfeits, calculations involved the well known consensus value (1/0.1194) {+-} 0 as reference. The typical uncertainty budget estimated for these results was 40 'ppm' relative (k = 2). It increased to 150 'ppm' (k = 2) for the establishment of stand alone results, taking into account a relative difference of about 126 'ppm' systematically observed between measured and certified values of the NIST SRM 987. In case there was suspicion of a deviation of the n({sup 88}Sr)/n({sup 86}Sr) ratio (worst case scenario) our proposal was to use the NIST SRM 987 value 8.37861 {+-} 0.00325 (k = 2) as reference, and assign a typical relative uncertainty budget of 300 'ppm' (k = 2). This method is thus fit for purpose and was applied to eleven French samples.

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

International Nuclear Information System (INIS)

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

2015-01-01

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

ICP27-dependent resistance of herpes simplex virus type 1 to leptomycin B is associated with enhanced nuclear localization of ICP4 and ICP0

International Nuclear Information System (INIS)

Lengyel, Joy; Strain, Anna K.; Perkins, Keith D.; Rice, Stephen A.

2006-01-01

It was previously shown that herpes simplex virus type 1 (HSV-1) is sensitive to leptomycin B (LMB), an inhibitor of nuclear export factor CRM1, and that a single methionine to threonine change at residue 50 (M50T) of viral immediate-early (IE) protein ICP27 can confer LMB resistance. In this work, we show that deletion of residues 21-63 from ICP27 can also confer LMB resistance. We further show that neither the M50T mutation nor the presence of LMB affects the nuclear shuttling activity of ICP27, suggesting that another function of ICP27 determines LMB resistance. A possible clue to this function emerged when it was discovered that LMB treatment of HSV-1-infected cells dramatically enhances the cytoplasmic accumulation of two other IE proteins, ICP0 and ICP4. This effect is completely dependent on ICP27 and is reversed in cells infected with LMB-resistant mutants. Moreover, LMB-resistant mutations in ICP27 enhance the nuclear localization of ICP0 and ICP4 even in the absence of LMB, and this effect can be discerned in transfected cells. Thus, the same amino (N)-terminal region of ICP27 that determines sensitivity to LMB also enhances ICP27's previously documented ability to promote the cytoplasmic accumulation of ICP4 and ICP0. We speculate that ICP27's effects on ICP4 and ICP0 may contribute to HSV-1 LMB sensitivity

Multielement analytical procedure coupling INAA, ICP-MS and ICP-AES: Application to the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco)

International Nuclear Information System (INIS)

Bounouira, H.; CEA - CNRS/UMR, Centre de Saclay, 91 - Gif sur Yvette; Choukri, A.; Hakam, O.K.; Cherkaoui, R.; Gaudry, A.; Delmas, R.; Mariet, C.; Chakiri, S.

2008-01-01

Instrumental neutron activation analysis (INAA), inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) were used for the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco). The reliability of the results was checked, by using IAEA Soil-7 certified reference material. Results obtained by the three techniques were compared to control digestions efficiencies. A general good agreement was found between INAA and both ICP-MS and ICP-AES after alkaline fusion (ICPf). The ICP-MS technique used after acid attack (ICPa) was satisfactory for a few elements. A principal component analysis (PCA) has been used for analyzing the variability of concentrations, and defining the most influential sites with respect to the general variation trends. Three groups of elements could be distinguished. For these groups a normalization of concentrations to the central element concentration (that means Mn, Si or Al) is proposed. (author)

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Precise Monitoring of Depleted Uranium in human and environment of South Iraq using Multi-collector ICP-MS

International Nuclear Information System (INIS)

Gerdes, A.; Weyer, S.; Brey, G.; Zimmermann, I.; Durakovic, A.

2004-01-01

Multi-collector Inductive Coupled Plasma Mass Spectrometry (MC-ICPMS) becomes increasingly important in monitoring environmental contamination, because it allows detection of long-lived radionuclides at ultra trace levels. High sample throughout combined with high precision and accuracy, low detection limits for most elements and simultaneous detection of up to 9 isotopes makes it prior to most other techniques. For homogeneous samples concentration and isotope composition can be determined with a precision and uncertainty of usually better than 0.5 % using the isotope dilution method, e.g. isotope measurements relative to a well characterized 233 U tracer. Exposure to low-level radioactive dust released into the environment accidentally or by the use of Depleted Uranium (DU) munitions in the military theatre demands precise screening of humans and local environment. Sensitive methods are also needed for monitoring and understanding the pathway of radionuclides in the biosphere and the human body. Using a method recently developed at our department it is for instance possible to detect urinary excretion of DU in the low fg/ml range or at fractions below 0.2% of the total urinary uranium concentration. This allows monitoring the inhalation of up to a few micrograms of insoluble non-natural uranium particles in the lung several months or even years later. As example we will show and discuss results from our study of the uranium isotope composition and concentration of surface water, topsoil and dust from different sites of Baghdad, Basra, and the Suweirah farming area. We also analyzed urine from people living in these areas or stayed their for a relative short time. The samples, also including highly contaminated ones, such as wipes of tank top debris and penetrator channels, were collected from the Uranium Medical Research Centre field team after coalition operation Iraqi Freedom in early October 2003. Total soil samples, separated soil fine-fractions ( 233 U

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

Science.gov (United States)

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

2018-01-01

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

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

International Nuclear Information System (INIS)

Fabien Pointurier; Amelie Hubert; Anne-Claire Pottin

2013-01-01

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

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.

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

Science.gov (United States)

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

2008-11-01

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

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

International Nuclear Information System (INIS)

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

2008-01-01

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

Multielement determination of major-to-ultratrace elements in vegetable samples by ICP-MS and ICP-AES after acid digestion

Energy Technology Data Exchange (ETDEWEB)

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

2000-06-01

A multielement determination of major-to-ultratrace elements in vegetable samples was carried out by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Spinach samples (0.5 g) were digested with nitric acid and hydrofluoric acid in a Teflon beaker on a hot plate. The decomposed samples were dissolved in a 1 M ( = mol dm{sup -3}) HNO{sub 3} solution containing internal standard elements (Ge, In, and Re, 10 ppb each), and were subjected to multielement analyses by ICP-AES and ICP-MS. As a result, about 40 elements were successfully determined over a wide concentration range from % to ppb level. Spinach samples grown in different production areas were also analyzed in order to understand the influences of the environmental conditions on growth. Among the major and minor elements, the values of the coefficient of variance (CV) for B, Mg, P, and K were < 20%, and those for Ca, Na, Al, and Mn were higher than 50%. On the other hand, the values of CV for trace and ultratrace elements were significantly high. Furthermore, the present analytical method was also applied to the determination of major-to-ultratrace elements in various vegetable samples (23 species in 11 families); the similarities and differences of the elemental distributions in vegetables were found in the experimental results. (author)

Multielement determination of major-to-ultratrace elements in vegetable samples by ICP-MS and ICP-AES after acid digestion

International Nuclear Information System (INIS)

Hokura, Akiko; Oguri, Sachiko; Matsuura, Hirotaka; Haraguchi, Hiroki

2000-01-01

A multielement determination of major-to-ultratrace elements in vegetable samples was carried out by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Spinach samples (0.5 g) were digested with nitric acid and hydrofluoric acid in a Teflon beaker on a hot plate. The decomposed samples were dissolved in a 1 M ( = mol dm -3 ) HNO 3 solution containing internal standard elements (Ge, In, and Re, 10 ppb each), and were subjected to multielement analyses by ICP-AES and ICP-MS. As a result, about 40 elements were successfully determined over a wide concentration range from % to ppb level. Spinach samples grown in different production areas were also analyzed in order to understand the influences of the environmental conditions on growth. Among the major and minor elements, the values of the coefficient of variance (CV) for B, Mg, P, and K were < 20%, and those for Ca, Na, Al, and Mn were higher than 50%. On the other hand, the values of CV for trace and ultratrace elements were significantly high. Furthermore, the present analytical method was also applied to the determination of major-to-ultratrace elements in various vegetable samples (23 species in 11 families); the similarities and differences of the elemental distributions in vegetables were found in the experimental results. (author)

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

International Nuclear Information System (INIS)

Graser, Carl-Heinrich

2015-01-01

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

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Development of an on-line low gas pressure cell for laser ablation-ICP-mass spectrometry

International Nuclear Information System (INIS)

Hirata, Takafumi

2007-01-01

An on-line low gas pressure cell device has been developed for elemental analysis using laser ablation-ICP-mass spectrometry (LA-ICPMS). Ambient gas in the sample cell was evacuated by a constant-flow diaphragm pump, and the pressure of the sample cell was controlled by changing the flow rate of He-inlet gas. The degree of sample re-deposition around the ablation pit could be reduced when the pressure of the ambient gas was lower than 50 kPa. Produced sample aerosol was drawn and taken from the outlet of the diaphragm pump, and directly introduced into the ICP ion source. The flow rate of He gas controls not only the gas pressure in the sample cell, but also the transport efficiency of the sample particles from the cell to the ICP, and the gas flow rate must be optimized to maximize the signal intensity of the analytes. The flow rates of the He carrier and Ar makeup gas were tuned to maximize the signal intensity of the analytes, and in the case of 238 U from the NIST SRM610 glass material, the signal intensity could be maximized with gas flow rates of 0.4 L/min for He and 1.2 L/min for Ar. The resulting gas pressure in the cell was 30-35 kPa. Using the low gas pressure cell device, the stability in the signal intensities and the resulting precision in isotopic ratio measurements were evaluated. The signal intensity profile of 63 Cu obtained by laser ablation from a metallic sample (NIST SRM976) demonstrated that typical spikes in the transient signal, which can become a large source of analytical error, were no longer found. The resulting precision in the 65 Cu/ 63 Cu ratio measurements was 2-3% (n=10, 2SD), which was half on the level obtained by laser ablation under atmospheric pressure (6-10%). The newly developed low-pressure cell device provides easier optimization of the operational conditions, together with smaller degrees of sample re-deposition and better stability in the signal intensity, even from a metallic sample. (author)

Precise Monitoring of Depleted Uranium in human and environment of South Iraq using Multi-collector ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Gerdes, A.; Weyer, S.; Brey, G. [Frankfurt Univ., Dept. of Mineralogy (Germany); Zimmermann, I.; Durakovic, A. [Uranium Medical Research Centre, Toronto (Italy)

2004-07-01

Multi-collector Inductive Coupled Plasma Mass Spectrometry (MC-ICPMS) becomes increasingly important in monitoring environmental contamination, because it allows detection of long-lived radionuclides at ultra trace levels. High sample throughout combined with high precision and accuracy, low detection limits for most elements and simultaneous detection of up to 9 isotopes makes it prior to most other techniques. For homogeneous samples concentration and isotope composition can be determined with a precision and uncertainty of usually better than 0.5 % using the isotope dilution method, e.g. isotope measurements relative to a well characterized {sup 233}U tracer. Exposure to low-level radioactive dust released into the environment accidentally or by the use of Depleted Uranium (DU) munitions in the military theatre demands precise screening of humans and local environment. Sensitive methods are also needed for monitoring and understanding the pathway of radionuclides in the biosphere and the human body. Using a method recently developed at our department it is for instance possible to detect urinary excretion of DU in the low fg/ml range or at fractions below 0.2% of the total urinary uranium concentration. This allows monitoring the inhalation of up to a few micrograms of insoluble non-natural uranium particles in the lung several months or even years later. As example we will show and discuss results from our study of the uranium isotope composition and concentration of surface water, topsoil and dust from different sites of Baghdad, Basra, and the Suweirah farming area. We also analyzed urine from people living in these areas or stayed their for a relative short time. The samples, also including highly contaminated ones, such as wipes of tank top debris and penetrator channels, were collected from the Uranium Medical Research Centre field team after coalition operation Iraqi Freedom in early October 2003. Total soil samples, separated soil fine-fractions (< 100

Mass-spectrometric mining of Hadean zircons by automated SHRIMP multi-collector and single-collector U/Pb zircon age dating: The first 100,000 grains

Science.gov (United States)

Holden, Peter; Lanc, Peter; Ireland, Trevor R.; Harrison, T. Mark; Foster, John J.; Bruce, Zane

2009-09-01

The identification and retrieval of a large population of ancient zircons (>4 Ga; Hadean) is of utmost priority if models of the early evolution of Earth are to be rigorously tested. We have developed a rapid and accurate U-Pb zircon age determination protocol utilizing a fully automated multi-collector ion microprobe, the ANU SHRIMP II, to screen and date these zircons. Unattended data acquisition relies on the calibration of a digitized sample map to the Sensitive High Resolution Ion MicroProbe (SHRIMP) sample-stage co-ordinate system. High precision positioning of individual grains can be produced through optical image processing of a specified mount location. The focal position of the mount can be optimized through a correlation between secondary-ion steering and the spot position on the target. For the Hadean zircon project, sample mounts are photographed and sample locations (normally grain centers) are determined off-line. The sample is loaded, reference points calibrated, and the target positions are then visited sequentially. In SHRIMP II multiple-collector mode, zircons are initially screened (ca. 5 s data acquisition) through their 204Pb corrected 207Pb/206Pb ratio; suitable candidates are then analyzed in a longer routine to obtain better measurement statistics, U/Pb, and concentration data. In SHRIMP I and SHRIMP RG, we have incorporated the automated analysis protocol to single-collector measurements. These routines have been used to analyze over 100,000 zircons from the Jack Hills quartzite. Of these, ca. 7%, have an age greater than 3.8 Ga, the oldest grain being 4372 +/- 6 Ma (2[sigma]), and this age is part of a group of analyses around 4350 Ma which we interpret as the age when continental crust first began to coalesce in this region. In multi-collector mode, the analytical time taken for a single mount with 400 zircons is approximately 6 h; whereas in single-collector mode, the analytical time is ca. 17 h. With this productivity, we can produce

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

International Nuclear Information System (INIS)

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

2005-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-07-16

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

DEFF Research Database (Denmark)

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

2015-01-01

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

Application of 1013 ohm Faraday cup current amplifiers for boron isotopic analyses by solution mode and laser ablation multicollector inductively coupled plasma mass spectrometry.

Science.gov (United States)

Lloyd, Nicholas S; Sadekov, Aleksey Yu; Misra, Sambuddha

2018-01-15

Boron isotope ratios (δ 11 B values) are used as a proxy for seawater paleo-pH, amongst several other applications. The analytical precision can be limited by the detection of low intensity ion beams from limited sample amounts. High-gain amplifiers offer improvements in signal/noise ratio and can be used to increase measurement precision and reduce sample amounts. 10 13 ohm amplifier technology has previously been applied to several radiogenic systems, but has thus far not been applied to non-traditional stable isotopes. Here we apply 10 13 ohm amplifier technology for the measurement of boron isotope ratios using solution mode MC-ICP-MS and laser ablation mode (LA-)MC-ICP-MS techniques. Precision is shown for reference materials as well as for low-volume foraminifera samples. The baseline uncertainty for a 0.1 pA 10 B + ion beam is reduced to ohm amplifier technology is demonstrated to offer advantages for the determination of δ 11 B values by both MC-ICP-MS and LA-MC-ICP-MS for small samples of biogenic carbonates, such as foraminifera shells. 10 13 ohm amplifier technology will also be of benefit to other non-traditional stable isotope measurements. Copyright © 2017 John Wiley & Sons, Ltd.

Accurate determination of Curium and Californium isotopic ratios by inductively coupled plasma quadrupole mass spectrometry (ICP-QMS) in 248Cm samples for transmutation studies

Energy Technology Data Exchange (ETDEWEB)

Gourgiotis, A.; Isnard, H.; Aubert, M.; Dupont, E.; AlMahamid, I.; Cassette, P.; Panebianco, S.; Letourneau, A.; Chartier, F.; Tian, G.; Rao, L.; Lukens, W.

2011-02-01

The French Atomic Energy Commission has carried out several experiments including the mini-INCA (INcineration of Actinides) project for the study of minor-actinide transmutation processes in high intensity thermal neutron fluxes, in view of proposing solutions to reduce the radiotoxicity of long-lived nuclear wastes. In this context, a Cm sample enriched in {sup 248}Cm ({approx}97 %) was irradiated in thermal neutron flux at the High Flux Reactor (HFR) of the Laue-Langevin Institute (ILL). This work describes a quadrupole ICP-MS (ICP-QMS) analytical procedure for precise and accurate isotopic composition determination of Cm before sample irradiation and of Cm and Cf after sample irradiation. The factors that affect the accuracy and reproducibility of isotopic ratio measurements by ICP-QMS, such as peak centre correction, detector dead time, mass bias, abundance sensitivity and hydrides formation, instrumental background, and memory blank were carefully evaluated and corrected. Uncertainties of the isotopic ratios, taking into account internal precision of isotope ratio measurements, peak tailing, and hydrides formations ranged from 0.3% to 1.3%. This uncertainties range is quite acceptable for the nuclear data to be used in transmutation studies.

Separation techniques for the clean-up of radioactive mixed waste for ICP-AES/ICP-MS analysis

International Nuclear Information System (INIS)

Swafford, A.M.; Keller, J.M.

1993-01-01

Two separation techniques were investigated for the clean-up of typical radioactive mixed waste samples requiring elemental analysis by Inductively Coupled Plasma-Atomic Emission Spectroscopy (ICP-AES) or Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). These measurements frequently involve regulatory or compliance criteria which include the determination of elements on the EPA Target Analyte List (TAL). These samples usually consist of both an aqueous phase and a solid phase which is mostly an inorganic sludge. Frequently, samples taken from the waste tanks contain high levels of uranium and thorium which can cause spectral interferences in ICP-AES or ICP-MS analysis. The removal of these interferences is necessary to determine the presence of the EPA TAL elements in the sample. Two clean-up methods were studied on simulated aqueous waste samples containing the EPA TAL elements. The first method studied was a classical procedure based upon liquid-liquid extraction using tri-n- octylphosphine oxide (TOPO) dissolved in cyclohexane. The second method investigated was based on more recently developed techniques using extraction chromatography; specifically the use of a commercially available Eichrom TRU·Spec trademark column. Literature on these two methods indicates the efficient removal of uranium and thorium from properly prepared samples and provides considerable qualitative information on the extraction behavior of many other elements. However, there is a lack of quantitative data on the extraction behavior of elements on the EPA Target Analyte List. Experimental studies on these two methods consisted of determining whether any of the analytes were extracted by these methods and the recoveries obtained. Both methods produced similar results; the EPA target analytes were only slightly or not extracted. Advantages and disadvantages of each method were evaluated and found to be comparable

Mass spectrometry of long-lived radionuclides

International Nuclear Information System (INIS)

Becker, Johanna Sabine.

2003-01-01

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

Total evaporation in thermal ionization mass spectrometry

International Nuclear Information System (INIS)

Callis, E.L.; Cappis, J.H.

1996-01-01

Experiments were conducted to assess the effects of impurities on the total evaporation method for mass spectrometric measurement of the isotope ratio of uranium. Standard samples were spiked with Na, Ca, Fe, Zr and Ba. The results indicated that only Fe, and possible Na, displayed any interference, and then only at high concentrations. One problem limiting the accuracy of the method is the determination of the relative efficiency of the collectors in the multicollector system. 3 refs., 1 tab

Determination of actinides using ICP-SFMS

International Nuclear Information System (INIS)

Nygren, Ulrika

2006-01-01

Interest in the determination of the actinides using ICP-MS has steadily increased with the development of systems capable of more sensitive and precise measurements. However, the analysis of less abundant actinides such as Pu and Am is not straightforward due to the need for chemical separation of these elements prior to determination. In many applications of mass-spectrometric actinide analysis, isotope ratio measurements are important, either for the analysis of the isotopic composition of, e.g., U or Pu in the sample, or for quantitative determinations using isotope dilution mass spectrometry. In order to achieve high precision and accuracy in an isotope ratio measurement, corrections for instrumentally induced systematic errors, e.g., due to dead-time and mass bias, need to be considered. In this thesis, different aspects of actinide analysis using ICP-SFMS have been addressed. In Papers I and III, separation procedures based on solid phase extraction for Pu, Am and U were developed and evaluated with respect to chemical yield and separation from elements causing spectral interferences. Applications of the analytical procedures developed comprised measurement of the 240 Pu/ 2 3 9Pu ratio in environmental reference materials, and age determination of Pu based on the 241 Pu/ 241 Am and 240 Pu/ 236 U ratios. In the application of different separation procedures for Pu, previously unidentified spectral interferences were discovered. In Paper II, these interferences were identified as lanthanide phosphate ions and the composition and formation of these species with respect to different instrumental parameters were further examined. Due to the importance of precise and accurate isotope ratio determination, a thorough investigation of the instrumental dead time of an ICP-SFMS system was performed. The dead time was evaluated via both isotope ratio and electronic measurements of the output from the detector amplifier. It was found that the overall uncertainty in ratio

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

Science.gov (United States)

Marcinkowska, Monika; Barałkiewicz, Danuta

2016-12-01

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

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

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.

ICP-MS and elemental tags for the life sciences

Energy Technology Data Exchange (ETDEWEB)

Giesen, Charlotte

2012-08-07

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

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

International Nuclear Information System (INIS)

Boulyga, Sergei F.; Prohaska, Thomas

2008-01-01

This paper presents the application of a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS) - a Nu Plasma HR - equipped with three ion-counting multipliers and coupled to a laser ablation system (LA) for the rapid and sensitive determination of the 235 U/ 238 U, 236 U/ 238 U, 145 Nd/ 143 Nd, 146 Nd/ 143 Nd, 101 Ru/( 99 Ru+ 99 Tc) and 102 Ru/( 99 Ru+ 99 Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred μm to about 1 mm and with surface alpha activities of 3-38 mBq were first identified using nuclear track radiography. U, Nd and Ru isotope systems were then measured sequentially for the same microsample by LA-MC-ICP-MS. The application of a zoom ion optic for aligning the ion beams into the ion counters allows fast switching between different isotope systems, which enables all of the abovementioned isotope ratios to be measured for the same microsample within a total analysis time of 15-20 min (excluding MC-ICP-MS optimization and calibration). The 101 Ru/( 99 Ru+ 99 Tc) and 102 Ru/( 99 Ru+ 99 Tc) isotope ratios were measured for four microsamples and were found to be significantly lower than the natural ratios, indicating that the microsamples were contaminated with the corresponding fission products (Ru and Tc). A slight depletion in 146 Nd of about 3-5% was observed in the contaminated samples, but the Nd isotopic ratios measured in the contaminated samples coincided with natural isotopic composition within the measurement uncertainty, as most of the Nd in the analyzed samples originates from the natural soil load of this element. The 235 U/ 238 U and 236 U/ 238 U isotope ratios were the most sensitive indicators of irradiated uranium. The present work yielded a significant variation in uranium isotope ratios in microsamples, in contrast with previously published results from the bulk analysis of contaminated samples originating from the vicinity of Chernobyl. Thus

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

Science.gov (United States)

Boulyga, Sergei F; Prohaska, Thomas

2008-01-01

This paper presents the application of a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS)--a Nu Plasma HR--equipped with three ion-counting multipliers and coupled to a laser ablation system (LA) for the rapid and sensitive determination of the 235U/238U, 236U/238U, 145Nd/143Nd, 146Nd/143Nd, 101Ru/(99Ru+99Tc) and 102Ru/(99Ru+99Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred mum to about 1 mm and with surface alpha activities of 3-38 mBq were first identified using nuclear track radiography. U, Nd and Ru isotope systems were then measured sequentially for the same microsample by LA-MC-ICP-MS. The application of a zoom ion optic for aligning the ion beams into the ion counters allows fast switching between different isotope systems, which enables all of the abovementioned isotope ratios to be measured for the same microsample within a total analysis time of 15-20 min (excluding MC-ICP-MS optimization and calibration). The 101Ru/(99Ru+99Tc) and 102Ru/(99Ru+99Tc) isotope ratios were measured for four microsamples and were found to be significantly lower than the natural ratios, indicating that the microsamples were contaminated with the corresponding fission products (Ru and Tc). A slight depletion in 146Nd of about 3-5% was observed in the contaminated samples, but the Nd isotopic ratios measured in the contaminated samples coincided with natural isotopic composition within the measurement uncertainty, as most of the Nd in the analyzed samples originates from the natural soil load of this element. The 235U/238U and 236U/238U isotope ratios were the most sensitive indicators of irradiated uranium. The present work yielded a significant variation in uranium isotope ratios in microsamples, in contrast with previously published results from the bulk analysis of contaminated samples originating from the vicinity of Chernobyl. Thus, the 235U/238U ratios measured in ten

An improved data acquisition system for isotopic ratio mass spectrometers

International Nuclear Information System (INIS)

Saha, T.K.; Reddy, B.; Nazare, C.K.; Handu, V.K.

1999-01-01

Isotopic ratio mass spectrometers designed and fabricated to measure the isotopic ratios with a precision of better than 0.05%. In order to achieve this precision, the measurement system consisting of ion signal to voltage converters, analog to digital converters, and data acquisition electronics should be at least one order better than the overall precision of measurement. Using state of the art components and techniques, a data acquisition system, which is an improved version of the earlier system, has been designed and developed for use with multi-collector isotopic ratio mass spectrometers

Characterisation of Supra- and Infratentorial ICP Profiles.

Science.gov (United States)

Moyse, Emmanuel; Ros, Maxime; Marhar, Fouad; Swider, Pascal; Schmidt, Eric Albert

2016-01-01

In pathophysiology and clinical practice, the intracranial pressure (ICP) profiles in the supratentorial and infratentorial compartments are unclear. We know that the pressure within the skull is unevenly distributed, with demonstrated ICP gradients. We recorded and characterised the supra- and infratentorial ICP patterns to understand what drives the transtentorial ICP gradient.A 70-year-old man was operated on for acute cerebellar infarction. One supratentorial probe and one cerebellar probe were implanted. Both signals were recorded concurrently and analysed off-line. We calculated mean ICP, ICP pulse amplitude, respiratory waves, slow waves and the RAP index of supra- and infratentorial ICP signals. Then, we measured transtentorial difference and performed correlation analysis for every index.Supratentorial ICP mean was 8.5 mmHg lower than infratentorial ICP, but the difference lessens for higher values. Both signals across the tentorium showed close correlation. Supra- and infratentorial pulse amplitude, respiratory waves and slow waves also showed a high degree of correlation. The compensatory reserve (RAP) showed good correlation. In this case report, we demonstrate that the mean value of ICP is higher in the posterior fossa, with a strong correlation across the tentorium. All other ICP-derived parameters display a symmetrical profile.

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-11-15

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

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

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov

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

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

DEFF Research Database (Denmark)

Qiao, Jixin; Lagerkvist, Petra; Rodushkin, Ilia

2018-01-01

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

ICP-oa TOFMS utilisation to determine the Gd isotopic abundance in gadolinium nitrate

International Nuclear Information System (INIS)

Dragomir, M.; Ohai, D.; Dumitrescu, I.; Furtuna, I.

2010-01-01

This paper is describes the development of a method that should permit the determination of isotope abundance of gadolinium in gadolinium nitrate, used as burnable poison at Cernavoda NPP. To determine the isotopic abundance of gadolinium the inductively coupled plasma orthogonal acceleration time-of-flight mass spectrometer (ICP-oa TOFMS) was used. The ICP-oa TOFMS allows the elimination of noise associated with instrumental drift and instability (flicker noise). The absence of flicker noise in the ICP-oa TOFMS means that the isotope ratios can be measured up to the statistical limit of ion counting. With TOFMS, each spectrum acquired represents signals from ions extracted from the plasma during the same time interval, formed from identical plasma and sample introduction events. Therefore, the ICP-oa TOFMS, Optimass 8000, has been successfully used for isotope ratio measurements of Gd in gadolinium nitrate [Gd (NO 3 ) 3 x 6H 2 O] sample solutions. (authors)

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

Energy Technology Data Exchange (ETDEWEB)

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

2006-03-15

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

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

International Nuclear Information System (INIS)

Todoli, Jose L.; Mermet, Jean M.

2006-01-01

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

Development, optimisation, and application of ICP-SFMS methods for the measurement of isotope ratios

International Nuclear Information System (INIS)

Stuerup, S.

2000-07-01

The measurement of isotopic composition and isotope ratios in biological and environmental samples requires sensitive, precise, and accurate analytical techniques. The analytical techniques used are traditionally based on mass spectrometry, among these techniques is the ICP-SFMS technique, which became commercially available in the mid 1990s. This technique is characterised by high sensitivity, low background, and the ability to separate analyte signals from spectral interferences. These features are beneficial for the measurement of isotope ratios and enable the measurement of isotope ratios of elements, which it has not previously been possible to measure due to either spectral interferences or poor sensitivity. The overall purpose of the project was to investigate the potential of the single detector ICP-SFMS technique for the measurement of isotope ratios in biological and environmental samples. One part of the work has focused on the fundamental aspects of the ICP-SFMS technique with special emphasize on the features important to the measurement of isotope ratios, while another part has focused on the development, optimisation and application of specific methods for the measurement of isotope ratios of elements of nutritional interest and radionuclides. The fundamental aspects of the ICP-SFMS technique were investigated theoretically and experimentally by the measurement of isotope ratios applying different experimental conditions. It was demonstrated that isotope ratios could be measured reliably using ICP-SFMS by educated choice of acquisition parameters, scanning mode, mass discrimination correction, and by eliminating the influence of detector dead time. Applying the knowledge gained through the fundamental study, ICP-SFMS methods for the measurement of isotope ratios of calcium, zinc, molybdenum and iron in human samples and a method for the measurement of plutonium isotope ratios and ultratrace levels of plutonium and neptunium in environmental samples

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

Science.gov (United States)

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

2015-09-01

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

Toepassing ICP-AES op het RIKILT

NARCIS (Netherlands)

Ruig, de W.G.

1980-01-01

Rapportage over de toepassing van ICP-AES op het RIKILT. Bij ICP-AES worden twee manieren van lichtemissie detectie toegepast nl. simultaan en sequentieel. De voor- en nadelen van ICP-AES t.o.v. AAS worden op een rij gezet.

Using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to characterize copper, zinc and mercury along grizzly bear hair providing estimate of diet

International Nuclear Information System (INIS)

Noël, Marie; Christensen, Jennie R.; Spence, Jody; Robbins, Charles T.

2015-01-01

We enhanced an existing technique, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), to function as a non-lethal tool in the temporal characterization of trace element exposure in wild mammals. Mercury (Hg), copper (Cu), cadmium (Cd), lead (Pb), iron (Fe) and zinc (Zn) were analyzed along the hair of captive and wild grizzly bears (Ursus arctos horribilis). Laser parameters were optimized (consecutive 2000 μm line scans along the middle line of the hair at a speed of 50 μm/s; spot size = 30 μm) for consistent ablation of the hair. A pressed pellet of reference material DOLT-2 and sulfur were used as external and internal standards, respectively. Our newly adapted method passed the quality control tests with strong correlations between trace element concentrations obtained using LA-ICP-MS and those obtained with regular solution-ICP-MS (r 2 = 0.92, 0.98, 0.63, 0.57, 0.99 and 0.90 for Hg, Fe, Cu, Zn, Cd and Pb, respectively). Cross-correlation analyses revealed good reproducibility between trace element patterns obtained from hair collected from the same bear. One exception was Cd for which external contamination was observed resulting in poor reproducibility. In order to validate the method, we used LA-ICP-MS on the hair of five captive grizzly bears fed known and varying amounts of cutthroat trout over a period of 33 days. Trace element patterns along the hair revealed strong Hg, Cu and Zn signals coinciding with fish consumption. Accordingly, significant correlations between Hg, Cu, and Zn in the hair and Hg, Cu, and Zn intake were evident and we were able to develop accumulation models for each of these elements. While the use of LA-ICP-MS for the monitoring of trace elements in wildlife is in its infancy, this study highlights the robustness and applicability of this newly adapted method. - Highlights: • LA-ICP-MS provides temporal trace metal exposure information for wild grizzly bears. • Cu and Zn temporal exposures provide

Using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to characterize copper, zinc and mercury along grizzly bear hair providing estimate of diet

Energy Technology Data Exchange (ETDEWEB)

Noël, Marie, E-mail: marie.noel@stantec.com [Stantec Consulting Ltd. 2042 Mills Road, Unit 11, Sidney BC V8L 4X2 (Canada); Christensen, Jennie R., E-mail: jennie.christensen@stantec.com [Stantec Consulting Ltd. 2042 Mills Road, Unit 11, Sidney BC V8L 4X2 (Canada); Spence, Jody, E-mail: jodys@uvic.ca [School of Earth and Ocean Sciences, Bob Wright Centre A405, University of Victoria, PO BOX 3065 STN CSC, Victoria, BC V8W 3V6 (Canada); Robbins, Charles T., E-mail: ctrobbins@wsu.edu [School of the Environment and School of Biological Sciences, Washington State University, Pullman, WA 99164-4236 (United States)

2015-10-01

We enhanced an existing technique, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), to function as a non-lethal tool in the temporal characterization of trace element exposure in wild mammals. Mercury (Hg), copper (Cu), cadmium (Cd), lead (Pb), iron (Fe) and zinc (Zn) were analyzed along the hair of captive and wild grizzly bears (Ursus arctos horribilis). Laser parameters were optimized (consecutive 2000 μm line scans along the middle line of the hair at a speed of 50 μm/s; spot size = 30 μm) for consistent ablation of the hair. A pressed pellet of reference material DOLT-2 and sulfur were used as external and internal standards, respectively. Our newly adapted method passed the quality control tests with strong correlations between trace element concentrations obtained using LA-ICP-MS and those obtained with regular solution-ICP-MS (r{sup 2} = 0.92, 0.98, 0.63, 0.57, 0.99 and 0.90 for Hg, Fe, Cu, Zn, Cd and Pb, respectively). Cross-correlation analyses revealed good reproducibility between trace element patterns obtained from hair collected from the same bear. One exception was Cd for which external contamination was observed resulting in poor reproducibility. In order to validate the method, we used LA-ICP-MS on the hair of five captive grizzly bears fed known and varying amounts of cutthroat trout over a period of 33 days. Trace element patterns along the hair revealed strong Hg, Cu and Zn signals coinciding with fish consumption. Accordingly, significant correlations between Hg, Cu, and Zn in the hair and Hg, Cu, and Zn intake were evident and we were able to develop accumulation models for each of these elements. While the use of LA-ICP-MS for the monitoring of trace elements in wildlife is in its infancy, this study highlights the robustness and applicability of this newly adapted method. - Highlights: • LA-ICP-MS provides temporal trace metal exposure information for wild grizzly bears. • Cu and Zn temporal exposures provide

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

Science.gov (United States)

Boulyga, Sergei F; Tibi, Markus; Heumann, Klaus G

2004-01-01

The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3x10(-13) g g(-1) for Pu isotopes in soil samples containing uranium at a concentration of a few microg g(-1). The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH+ and PbO2+ ions and by the peak tail of 238U+ ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of alpha-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of (239+240)Pu (9.8 +/- 3.0 mBq g(-1)) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4 +/- 0.2 mBq g(-1). However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if "hot" particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples.

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

International Nuclear Information System (INIS)

Boulyga, Sergei F.; Tibi, Markus; Heumann, Klaus G.

2004-01-01

The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3 x 10 -13 g g -1 for Pu isotopes in soil samples containing uranium at a concentration of a few μg g -1 . The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH + and PbO 2 + ions and by the peak tail of 238 U + ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of α-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of 239+240 Pu (9.8±3.0 mBq g -1 ) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4±0.2 mBq g -1 . However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if ''hot'' particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples. (orig.)

High spatial resolution analysis of ferromanganese concretions by LA-ICP-MS†

Directory of Open Access Journals (Sweden)

Ingri Johan

2002-06-01

Full Text Available A procedure was developed for the determination of element distributions in cross-sections of ferromanganese concretions using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS. The effects of carrier flow rates, rf forward power, ablation energy, ablation spot size, repetition rate and number of shots per point on analyte intensity were studied. It is shown that different carrier gas flow rates are required in order to obtain maximum sensitivities for different groups of elements, thus complicating the optimisation of ICP parameters. On the contrary, LA parameters have very similar effects on almost all elements studied, thus providing a common optimum parameter set for the entire mass range. However, for selected LA parameters, the use of compromise conditions was necessary in order to compensate for relatively slow data acquisition by ICP-MS and maintain high spatial resolution without sacrificing the multielemental capabilities of the technique. Possible variations in ablation efficiency were corrected for mathematically using the sum of Fe and Mn intensities. Quantification by external calibration against matrix-matched standards was successfully used for more than 50 elements. These standards, in the form of pressed pellets (no binder, were prepared in-house using ferromanganese concentrates from a deep-sea nodule reference material as well as from shallow-marine concretions varying in size and having different proportions of three major phases: aluminosilicates, Fe- and Mn-oxyhydroxides. Element concentrations in each standard were determined by means of conventional solution nebulisation ICP-MS following acid digestion. Examples of selected inter-element correlations in distribution patterns along the cross-section of a concretion are given.

Fundamental studies of interferences in ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Rowley, L.K

2000-11-01

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

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

International Nuclear Information System (INIS)

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

2001-01-01

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

Measurement of in situ sulfur isotopes by laser ablation multi-collector ICPMS: opening Pandora’s Box

Science.gov (United States)

Ridley, William I.; Pribil, Michael; Koenig, Alan E.; Slack, John F.

2015-01-01

Laser ablation multi-collector ICPMS is a modern tool for in situ measurement of S isotopes. Advantages of the technique are speed of analysis and relatively minor matrix effects combined with spatial resolution sufficient for many applications. The main disadvantage is a more destructive sampling mechanism relative to the ion microprobe technique. Recent advances in instrumentation allow precise measurement with spatial resolutions down to 25 microns. We describe specific examples from economic geology where increased spatial resolution has greatly expanded insights into the sources and evolution of fluids that cause mineralization and illuminated genetic relations between individual deposits in single mineral districts.

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

Data.gov (United States)

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

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

Science.gov (United States)

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

2018-01-24

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

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

Science.gov (United States)

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

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

Science.gov (United States)

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

2003-02-01

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

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

International Nuclear Information System (INIS)

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

2003-01-01

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

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

OpenAIRE

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

1992-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-01-15

This paper presents the application of a multicollector inductively coupled plasma mass spectrometer (MC-ICP-MS) - a Nu Plasma HR - equipped with three ion-counting multipliers and coupled to a laser ablation system (LA) for the rapid and sensitive determination of the {sup 235}U/{sup 238}U, {sup 236}U/{sup 238}U, {sup 145}Nd/{sup 143}Nd, {sup 146}Nd/{sup 143}Nd, {sup 101}Ru/({sup 99}Ru+{sup 99}Tc) and {sup 102}Ru/({sup 99}Ru+{sup 99}Tc) isotope ratios in microsamples collected in the vicinity of Chernobyl. Microsamples with dimensions ranging from a hundred {mu}m to about 1 mm and with surface alpha activities of 3-38 mBq were first identified using nuclear track radiography. U, Nd and Ru isotope systems were then measured sequentially for the same microsample by LA-MC-ICP-MS. The application of a zoom ion optic for aligning the ion beams into the ion counters allows fast switching between different isotope systems, which enables all of the abovementioned isotope ratios to be measured for the same microsample within a total analysis time of 15-20 min (excluding MC-ICP-MS optimization and calibration). The {sup 101}Ru/({sup 99}Ru+{sup 99}Tc) and {sup 102}Ru/({sup 99}Ru+{sup 99}Tc) isotope ratios were measured for four microsamples and were found to be significantly lower than the natural ratios, indicating that the microsamples were contaminated with the corresponding fission products (Ru and Tc). A slight depletion in {sup 146}Nd of about 3-5% was observed in the contaminated samples, but the Nd isotopic ratios measured in the contaminated samples coincided with natural isotopic composition within the measurement uncertainty, as most of the Nd in the analyzed samples originates from the natural soil load of this element. The {sup 235}U/{sup 238}U and {sup 236}U/{sup 238}U isotope ratios were the most sensitive indicators of irradiated uranium. The present work yielded a significant variation in uranium isotope ratios in microsamples, in contrast with previously

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

Science.gov (United States)

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

2017-11-01

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

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

International Nuclear Information System (INIS)

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

1996-01-01

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

ICP (ITER Collaborative Platform)

Energy Technology Data Exchange (ETDEWEB)

Capuano, C.; Carayon, F.; Patel, V. [ITER, 13 - St. Paul-Lez Durance (France)

2009-07-01

The ITER organization has the necessity to manage a massive amount of data and processes. Each team requires different process and databases often interconnected with those of others teams. ICP is the current central ITER repository of structured and unstructured data. All data in ICP is served and managed via a web interface that provides global accessibility with a common user friendly interface. This paper will explain the model used by ICP and how it serves the ITER project by providing a robust and agile platform. ICP is developed in ASP.NET using MSSQL Server for data storage. It currently houses 15 data driven applications, 150 different types of record, 500 k objects and 2.5 M references. During European working hours the system averages 150 concurrent users and 20 requests per second. ICP connects to external database applications to provide a single entry point to ITER data and a safe shared storage place to maintain this data long-term. The Core model provides an easy to extend framework to meet the future needs of the Organization. ICP follows a multi-tier architecture, providing logical separation of process. The standard three-tier architecture is expanded, with the data layer separated into data storage, data structure, and data access components. The business or applications logic layer is broken up into a common business functionality layer, a type specific logic layer, and a detached work-flow layer. Finally the presentation tier comprises a presentation adapter layer and an interface layer. Each layer is built up from small blocks which can be combined to create a wide range of more complex functionality. Each new object type developed gains access to a wealth of existing code functionality, while also free to adapt and extend this. The hardware structure is designed to provide complete redundancy, high availability and to handle high load. This document is composed of an abstract followed by the presentation transparencies. (authors)

Application of isotope-dilution laser ablation ICP-MS for direct determination of Pu concentrations in soils at pg g{sup -1} levels

Energy Technology Data Exchange (ETDEWEB)

Boulyga, Sergei F.; Tibi, Markus; Heumann, Klaus G. [Institute of Inorganic Chemistry and Analytical Chemistry, Johannes Gutenberg-University Mainz, Duesbergweg 10-14, 55099, Mainz (Germany)

2004-01-01

The methods available for determination of environmental contamination by plutonium at ultra-trace levels require labor-consuming sample preparation including matrix removal and plutonium extraction in both nuclear spectroscopy and mass spectrometry. In this work, laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was applied for direct analysis of Pu in soil and sediment samples. Application of a LINA-Spark-Atomizer system (a modified laser ablation system providing high ablation rates) coupled with a sector-field ICP-MS resulted in detection limits as low as 3 x 10{sup -13} g g{sup -1} for Pu isotopes in soil samples containing uranium at a concentration of a few {mu}g g{sup -1}. The isotope dilution (ID) technique was used for quantification, which compensated for matrix effects in LA-ICP-MS. Interferences by UH{sup +} and PbO{sub 2}{sup +} ions and by the peak tail of {sup 238}U{sup +} ions were reduced or separated by use of dry plasma conditions and a mass resolution of 4000, respectively. No other effects affecting measurement accuracy, except sample inhomogeneity, were revealed. Comparison of results obtained for three contaminated soil samples by use of {alpha}-spectrometry, ICP-MS with sample decomposition, and LA-ICP-IDMS showed, in general, satisfactory agreement of the different methods. The specific activity of {sup 239+240}Pu (9.8{+-}3.0 mBq g{sup -1}) calculated from LA-ICP-IDMS analysis of SRM NIST 4357 coincided well with the certified value of 10.4{+-}0.2 mBq g{sup -1}. However, the precision of LA-ICP-MS for determination of plutonium in inhomogeneous samples, i.e. if ''hot'' particles are present, is limited. As far as we are aware this paper reports the lowest detection limits and element concentrations yet measured in direct LA-ICP-MS analysis of environmental samples. (orig.)

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

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

Science.gov (United States)

Boulyga, S F; Becker, J S

2001-07-01

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

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

International Nuclear Information System (INIS)

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

2005-01-01

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

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

Science.gov (United States)

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

2004-09-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2004-09-01

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

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

International Nuclear Information System (INIS)

Forsyth, Roy

1997-07-01

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

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

International Nuclear Information System (INIS)

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

2011-01-01

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

Normal variations in the isotopic composition of metabolically relevant transition metals in human blood

Science.gov (United States)

Van Heghe, L.; Cloquet, C.; Vanhaecke, F.

2012-04-01

Cu, Fe and Zn are transition metals with great catalytic, structural and regulating importance in the human body. Hence, an aberrant metabolism of these elements can have serious implications on the health of a person. It is assumed that, due to differences in isotope fractionation, the isotopic composition of these elements in whole blood of patients can be different from that in blood of healthy subjects. Therefore, isotopic analysis of the element affected by the disease can be a promising approach for early diagnosis. A method for isotopic analysis of Cu, Fe and Zn in human whole blood was developed. The simultaneous chromatographic isolation of these elements and the conditions for isotope ratio measurement via multi-collector ICP - mass spectrometry (MC-ICP-MS) were optimized. So far, only whole blood of supposedly healthy volunteers (reference population) was analyzed. Results for Fe confirmed the known differences in isotopic composition between male and female blood. It is also shown that other parameters can have influence as well, e.g., the isotopic composition of Zn seems to be governed by the diet.

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

Multielement determination of major-to-ultratrace elements in deep-seawater salts by ICP-AES and ICP-MS

International Nuclear Information System (INIS)

Sakai, Takeshi; Nakagawa, Koji; Nakajima, Hiroshi; Itoh, Akihide; Ji, Shan; Haraguchi, Hiroki

2002-01-01

Major-to-ultratrace elements in deep-seawater salts were determined by ICP-AES and ICP-MS, after they were separated into the water-soluble, acid-soluble, and insoluble particle components. Deep-seawater salts were prepared from seawater collected at 344 m deep near the off-shore of Cape Muroto in Kochi Prefecture. The major and minor elements in salts were determined by ICP-AES after appropriate dilution with pure water. Trace and ultratrace elements in the water-soluble and acid-soluble components were preconcentrated by a chelating resin preconcentration method. In addition, the major to-ultratrace elements in the insoluble particle component were determined by ICP-AES and ICP-MS, after acid-digestion using HNO 3 /HF/HClO 4 . As a result, 21-35 elements in deep-seawater salts could be determined over the wide concentration range. It was found that the elements, such as Al, V, Fe, Mn, Co, Cu, Zn, and rare earth elements, were more abundant in the acid-soluble component of deep-seawater salts, which may play some essential roles in physiological effectiveness for intake of salt. (author)

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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

Science.gov (United States)

Tagami; Uchida; Hamilton; Robison

2000-07-01

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

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

International Nuclear Information System (INIS)

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

2000-01-01

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

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

International Nuclear Information System (INIS)

Syarbaini

2000-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-07-01

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

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

Science.gov (United States)

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

2018-04-02

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

ICP measurement accuracy: the effect of temperature drift. Design of a laboratory test for assessment of ICP transducers.

Science.gov (United States)

Morgalla, M H; Mettenleiter, H; Katzenberger, T

1999-01-01

Intracranial pressure (ICP) monitoring has become the mainstay of multimodal neuromonitoring of comatous patients after head injury. In the presence of rising ICP and faced with pressures, difficult to control, aggressive measures, such as hypothermia may be used. The ICP readings should not be influenced by temperature changes. A laboratory test was designed to simulate temperature variations between 20 degrees C and 45 degrees C at different pressure levels under physiological conditions. Five types of transducers were examined: Epidyn Braun Melsungen, ICT/B-Titan Gaeltec, Camino-OLM-110-4B, Codman MicroSensor ICP-Transducer, Neurovent ICP transducer Rehau Ag+Co. Tests were performed at 6 different pressure levels between 0 mmHg and 50 mmHg. The results show very low drifts of less than 0.15 mmHg degree C-1 for Codman, Epidyn and Neurovent. Gaeltec and Camino exhibited higher drifts of 0.18 mmHg and 0.2 mmHg degree C-1 respectively. Within the temperature range from 35 degrees C to 42 degrees C all probes tested show insignificant temperature drift. Whether these results also apply to other types of transducers needs further evaluation. Problems and requirements related to the design of a laboratory test for the in vitro assessment of ICP transducers are discussed in detail.

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

International Nuclear Information System (INIS)

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

2003-01-01

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

Exploiting dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) for sequential determination of trace elements in blood using a dilute-and-shoot procedure

International Nuclear Information System (INIS)

Lemos Batista, Bruno; Lisboa Rodrigues, Jairo; Andrade Nunes, Juliana; Oliveira Souza, Vanessa Cristina de; Barbosa, Fernando

2009-01-01

Inductively coupled plasma mass spectrometry with quadrupole (q-ICP-MS) and dynamic reaction cell (DRC-ICP-MS) were evaluated for sequential determination of As, Cd, Co, Cr, Cu, Mn, Pb, Se, Tl, V and Zn in blood. The method requires as little as 100 μL of blood. Prior to analysis, samples (100 μL) were diluted 1:50 in a solution containing 0.01% (v/v) Triton X-100 and 0.5% (v/v) nitric acid. The use of the DRC was only mandatory for Cr, Cu, V and Zn. For the other elements the equipment may be operated in a standard mode (q-ICP-MS). Ammonia was used as reaction gas. Selection of best flow rate of ammonium gas and optimization of the quadrupole dynamic band-pass tuning parameter (RPq) were carried out, using a ovine base blood for Cr and V and a synthetic matrix solution (SMS) for Zn and Cu diluted 1:50 and spiked to contain 1 μg L -1 of each element. Method detection limits (3 s) for 75 As, 114 Cd, 59 Co, 51 Cr, 63 Cu 55 Mn, 208 Pb, 82 Se, 205 Tl, 51 V, and 64 Zn were 14.0, 3.0, 11.0, 7.0, 280, 9.0, 3.0, 264, 0.7, 6.0 and 800 ng L -1 , respectively. Method validation was accomplished by the analysis of blood Reference Materials produced by the L'Institut National de Sante Publique du Quebec (Canada).

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

OpenAIRE

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

2001-01-01

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

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

International Nuclear Information System (INIS)

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

1998-01-01

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

Development and validation of an analytical method for the determination of lead isotopic composition using ICP-QMS

OpenAIRE

Rodríguez-Salazar, M. T.; Morton Bermea, O.; Hernández-Álvarez, E.; García-Arreola, M. E.; Ortuño-Arzate, M. T.

2010-01-01

This work reports a method for the precise and accurate determination of Pb isotope composition in soils and geological matrices by ICP-QMS. Three reference materials (AGV-2, SRM 2709 and JSO-1) were repeatedly measured, using ICP-QMS instruments in order to assess the quality of this analytical procedure. Mass discrimination was evaluated for Pb/Pb with Pb isotope reference material NIST SRM 981, and the correction applied to the above mentioned reference materials to achieve good accuracy o...

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

Science.gov (United States)

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

2003-10-01

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

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

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

International Nuclear Information System (INIS)

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

2008-01-01

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

High-precision determination of the isotopic composition of dissolved iron in iron depleted seawater by double spike multicollector-ICPMS.

Science.gov (United States)

Lacan, Francois; Radic, Amandine; Labatut, Marie; Jeandel, Catherine; Poitrasson, Franck; Sarthou, Geraldine; Pradoux, Catherine; Chmeleff, Jerome; Freydier, Remi

2010-09-01

This work demonstrates the feasibility of the measurement of the isotopic composition of dissolved iron in seawater for an iron concentration range, 0.05-1 nmol L(-1), allowing measurements in most oceanic waters, including Fe depleted waters of high nutrient low chlorophyll areas. It presents a detailed description of our previously published protocol, with significant improvements on detection limit and blank contribution. Iron is preconcentrated using a nitriloacetic acid superflow resin and purified using an AG 1-x4 anion exchange resin. The isotopic ratios are measured with a multicollector-inductively coupled plasma mass spectrometer (MC-ICPMS) Neptune, coupled with a desolvator (Aridus II or Apex-Q), using a (57)Fe-(58)Fe double spike mass bias correction. A Monte Carlo test shows that optimum precision is obtained for a double spike composed of approximately 50% (57)Fe and 50% (58)Fe and a sample to double spike quantity ratio of approximately 1. Total procedural yield is 91 +/- 25% (2SD, n = 55) for sample sizes from 20 to 2 L. The procedural blank ranges from 1.4 to 1.1 ng, for sample sizes ranging from 20 to 2 L, respectively, which, converted into Fe concentrations, corresponds to blank contributions of 0.001 and 0.010 nmol L(-1), respectively. Measurement precision determined from replicate measurements of seawater samples and standard solutions is 0.08 per thousand (delta(56)Fe, 2SD). The precision is sufficient to clearly detect and quantify isotopic variations in the oceans, which so far have been observed to span 2.5 per thousand and thus opens new perspectives to elucidate the oceanic iron cycle.

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

NARCIS (Netherlands)

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

2001-01-01

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

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

Science.gov (United States)

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

2018-03-01

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

ICP curve morphology and intracranial flow-volume changes

DEFF Research Database (Denmark)

Unnerbäck, Mårten; Ottesen, Johnny T.; Reinstrup, Peter

2018-01-01

proposed to shape the ICP curve. This study tested the hypothesis that the ICP curve correlates to intracranial volume changes. METHODS: Cine phase contrast magnetic resonance imaging (MRI) examinations were performed in neuro-intensive care patients with simultaneous ICP monitoring. The MRI was set......BACKGROUND: The intracranial pressure (ICP) curve with its different peaks has been extensively studied, but the exact physiological mechanisms behind its morphology are still not fully understood. Both intracranial volume change (ΔICV) and transmission of the arterial blood pressure have been...

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

DEFF Research Database (Denmark)

Gammelgaard, B.; Larsen, Erik Huusfeldt

1998-01-01

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

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2001-07-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1993-05-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2002-04-01

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

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

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

Science.gov (United States)

Boulyga, Sergei F.; Heumann, Klaus G.

2005-04-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2000-07-15

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

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

International Nuclear Information System (INIS)

Leiterer, M.; Muench, U.

1994-01-01

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

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

Czech Academy of Sciences Publication Activity Database

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

2015-01-01

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

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

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

2015-07-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2000-11-01

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

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.

High-precision measurements of uranium and thorium isotopic ratios by multi-collector inductively coupled plasma mass spectrometry (MC-ICPMS)

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Wang, Lisheng; Ma, Zhibang; Duan, Wuhui

2015-04-01

Isotopic compositions of U-Th and 230Th dating have been widely used in earth sciences, such as chronology, geochemistry, oceanography and hydrology. In this study, five ages of different carbonate samples were measured using 230Th dating technique with U-Th high-precision isotopic measurements by multi-collector inductively coupled plasma mass spectrometry, in Uranium-series Chronology Laboratory, Institute of Geology and Geophysics, Chinese Academy of Sciences.In this study, the precision and accuracy of uranium isotopic composition were estimated by measuring the uranium ratios of NBS-CRM 112A, NBS-CRM U500 and HU-1. The mean measured ratios, 234U/238U = 52.86 (±0.04) × 10-6 and δ234U = -38.36 (±0.77) × 10-3 for NBS-CRM 112A, 234U/238U = 10.4184 (±0.0001) × 10-3, 236U/238U = 15.43 (±0.01) × 10-4 and 238U/235U = 1.00021 (±0.00002) for NBS-CRM U500, 234U/238U = 54.911 (±0.007) and δ234U = -1.04 (±0.13) × 10-3 for HU-1 (95% confidence levels). The U isotope data for standard reference materials are in excellent agreement with previous studies, further highlighting the reliability and analytical capabilities of our technique. We measured the thorium isotopic ratios of three different thorium standards by MC-ICPMS. The three standards (Th-1, Th-2 and Th-3) were mixed by HU-1 and NBS 232Th standard, with the 230Th/232Th ratios from 10-4 to 10-6. The mean measured atomic ratios, 230Th/232Th = 2.1227 (±0.0024) × 10-6, 2.7246 (±0.0026) × 10-5, and 2.8358 (±0.0007) × 10-4 for Th-1, Th-2 and Th-3 (95% confidence levels), respectively. Using this technique, the following standard samples were dated by MC-ICPMS. Sample RKM-4, collected from Babardos Kendal Hill terrace, was used during the first stage of the Uranium-Series Intercomparison Project (USIP-I). Samples 76001, RKM-5 and RKM-6 were studied during the second stage of the USIP program (USIP-II). Sample 76001 is a laminated flowstone, collected from Sumidero Terejapa, Chiapas, Mexico, and samples

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

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

2011-11-01

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

Nano-SIMS analysis of Mg, Sr, Ba and U in natural calcium carbonate

International Nuclear Information System (INIS)

Sano, Yuji; Shirai, Kotaro; Takahata, Naoto; Hirata, Takafumi; Sturchio, Neil C.

2005-01-01

Concentrations of minor (Mg and Sr) and trace (Ba and U) elements in four natural calcium carbonate samples were first analyzed by inductively coupled plasma mass spectrometry (ICP-MS) after chemical dissolution and calibrated against a standard dolomite. Their homogeneities were checked by in situ laser ablation (LA) ICP-MS with 10-20 spots. The carbonate samples were measured by using a high lateral resolution secondary ion mass spectrometer (Nano-SIMS NS50). A ∼4 nA O - primary beam was used to sputter a 5 - 6-μm diameter crater on the sample surface, and secondary positive ions were extracted for mass analysis using an accelerating voltage of 8 kV and a Mattauch-Herzog geometry. A multi-collector system was adjusted to detect 26 Mg + , 43 Ca + , 88 Sr + , 138 Ba + , 238 U 16 O 2 + ions at the same time. A resolving power of 2500 - 5000 at 10% peak height was attained by an entrance slit set at 40 μm, and each exit slit at 50 μm with adequate flat-topped peaks. The observed 26 Mg/ 43 Ca, 88 Sr/ 43 Ca, 138 Ba/ 43 Ca and 238 U 16 O 2 / 43 Ca ratios agreed well with those measured by LA-ICP-MS. Foraminifera shells were analyzed at 5 - 6 μm scale by Nano-SIMS. There was a large variation of the Mg/Ca ratios, up to ±38%, even in a single fragment of the shell, suggesting that although the ratios provide a useful paleoceanographic proxy at bulk scale, they may reflect a more complex pattern at <10 μm scale. (author)

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

International Nuclear Information System (INIS)

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

2005-01-01

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

Elemental Analysis in Biological Matrices Using ICP-MS.

Science.gov (United States)

Hansen, Matthew N; Clogston, Jeffrey D

2018-01-01

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

Inductively coupled plasma source mass spectrometry

International Nuclear Information System (INIS)

Price Russ, G. III

1993-01-01

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

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

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

2017-12-19

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

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

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Cong-ying Li

2018-03-01

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

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

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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.

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

International Nuclear Information System (INIS)

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

2001-01-01

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

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

Science.gov (United States)

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

2002-08-01

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

A new major adze quarry from Nanakuli, O'ahu: implications for interaction studies in Hawai'i

International Nuclear Information System (INIS)

Weisler, M.I.; Collins, S.L.; Feng, Y.; Zhao, J.; Shipton, C.; Wei, S.

2013-01-01

A major new basalt adze quarry at Nanakuli Valley, Hawaiian Islands is described which now ranks as one of the two largest on O'ahu and aside from the Mauna Kea adze quarry complex on Hawai'i island and the Haleakala source on Maui, is one of the major quarries in the archipelago. We defined the approximate limits of the quarry complex, located the in situ geological source of the fine-grained basalt used for adze manufacture, report the petrographic and geochemical variability of the source rock, and describe the adze reduction strategies from analysis of adze blanks and preforms, as well as hammerstones and debitage. The geochemical variation of the nine source rocks and artefacts were defined by a comprehensive array of 10 fully quantitative major element concentrations, 43 trace element abundances, and high-precision Sr-Nd-Pb isotopic ratios obtained using the state-of-the-art Thermal Ionization Mass Spectrometry (TIMS, for Sr isotopes), Multi-Collector Inductively Coupled Plasma Mass Spectrometry (MC-ICP-MS, for Nd-Pb isotopes), quadrupole ICP-MS (for trace elements) and Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES, for major elements), respectively. A piece of branch coral was recovered from the surface of a rockshelter that provided a U-series date of possible quarry use in the mid-13th century. It is advocated that a comprehensive range of major and trace element concentrations and Sr-Nd-Pb isotopic ratios are required for geochemically characterising adze quarries to facilitate the long-term viability of sourcing studies. (author)

Characterization of arsenic-contaminated aquifer sediments from eastern Croatia by ion microbeam, PIXE and ICP-OES techniques

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Ujević Bošnjak, M., E-mail: magdalena.ujevic@hzjz.hr [Croatian National Institute of Public Health, Rockefelerova 7, 10000 Zagreb (Croatia); Fazinić, S. [Institute Ruđer Bošković, Bijenička cesta, 10000 Zagreb (Croatia); Duić, Ž. [University of Zagreb, Faculty of Mining, Geology and Petroleum Engineering, Pierottijeva 6, Zagreb (Croatia)

2013-10-01

Highlights: •ICP-OES and PIXE used in the characterization of As-contaminated sediments. •Observed high correlations between the results obtained by those techniques. •Discrepancies observed for Mn, and for the highest As concentrations. •Microbeam analyses showed As association with sulphides and iron. -- Abstract: Groundwater arsenic contamination has been evidenced in eastern Croatia and hydrochemical results suggest that the occurrence of arsenic in the groundwater depends on the local geology, hydrogeology, and geochemical characteristics of the aquifer. In order to perform the sediment characterization and to investigate arsenic association with the other elements in the sediments, 10 samples from two boreholes (PVc-3 and Gundinci 1) in eastern Croatia were analyzed using two techniques: PIXE (without sample pre-treatment) and ICP-OES (after digestion), as well by ion microbeam analyses. The results of the PIXE and ICP-OES techniques showed quite good agreement; however, greater discrepancies were observed at the higher arsenic and manganese mass ratios. According to both techniques, higher As mass ratios were observed in the sediments from the PVc-3 core (up to 651 mg/kg and 491 mg/kg using PIXE and ICP-OES analyses respectively) than from the Gundinci 1 core (up to 60 mg/kg using both techniques). Although arsenic association with Fe is expected, no correlation was observed. The microbeam analyses demonstrated that arsenic is associated with sulphides and iron in the most As-contaminated sample from the PVc-3 core, while this relationship was not evident in the most As-contaminated sample from the Gundinci 1 borehole.

Characterization of arsenic-contaminated aquifer sediments from eastern Croatia by ion microbeam, PIXE and ICP-OES techniques

International Nuclear Information System (INIS)

Ujević Bošnjak, M.; Fazinić, S.; Duić, Ž.

2013-01-01

Highlights: •ICP-OES and PIXE used in the characterization of As-contaminated sediments. •Observed high correlations between the results obtained by those techniques. •Discrepancies observed for Mn, and for the highest As concentrations. •Microbeam analyses showed As association with sulphides and iron. -- Abstract: Groundwater arsenic contamination has been evidenced in eastern Croatia and hydrochemical results suggest that the occurrence of arsenic in the groundwater depends on the local geology, hydrogeology, and geochemical characteristics of the aquifer. In order to perform the sediment characterization and to investigate arsenic association with the other elements in the sediments, 10 samples from two boreholes (PVc-3 and Gundinci 1) in eastern Croatia were analyzed using two techniques: PIXE (without sample pre-treatment) and ICP-OES (after digestion), as well by ion microbeam analyses. The results of the PIXE and ICP-OES techniques showed quite good agreement; however, greater discrepancies were observed at the higher arsenic and manganese mass ratios. According to both techniques, higher As mass ratios were observed in the sediments from the PVc-3 core (up to 651 mg/kg and 491 mg/kg using PIXE and ICP-OES analyses respectively) than from the Gundinci 1 core (up to 60 mg/kg using both techniques). Although arsenic association with Fe is expected, no correlation was observed. The microbeam analyses demonstrated that arsenic is associated with sulphides and iron in the most As-contaminated sample from the PVc-3 core, while this relationship was not evident in the most As-contaminated sample from the Gundinci 1 borehole

Ion sampling and transport in Inductively Coupled Plasma Mass Spectrometry

Science.gov (United States)

Farnsworth, Paul B.; Spencer, Ross L.

2017-08-01

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

Evaluation of new geological reference materials for uranium-series measurements: Chinese Geological Standard Glasses (CGSG) and macusanite obsidian.

Science.gov (United States)

Denton, J S; Murrell, M T; Goldstein, S J; Nunn, A J; Amato, R S; Hinrichs, K A

2013-10-15

Recent advances in high-resolution, rapid, in situ microanalytical techniques present numerous opportunities for the analytical community, provided accurately characterized reference materials are available. Here, we present multicollector thermal ionization mass spectrometry (MC-TIMS) and multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) uranium and thorium concentration and isotopic data obtained by isotope dilution for a suite of newly available Chinese Geological Standard Glasses (CGSG) designed for microanalysis. These glasses exhibit a range of compositions including basalt, syenite, andesite, and a soil. Uranium concentrations for these glasses range from ∼2 to 14 μg g(-1), Th/U weight ratios range from ∼4 to 6, (234)U/(238)U activity ratios range from 0.93 to 1.02, and (230)Th/(238)U activity ratios range from 0.98 to 1.12. Uranium and thorium concentration and isotopic data are also presented for a rhyolitic obsidian from Macusani, SE Peru (macusanite). This glass can also be used as a rhyolitic reference material, has a very low Th/U weight ratio (around 0.077), and is approximately in (238)U-(234)U-(230)Th secular equilibrium. The U-Th concentration data agree with but are significantly more precise than those previously measured. U-Th concentration and isotopic data agree within estimated errors for the two measurement techniques, providing validation of the two methods. The large (238)U-(234)U-(230)Th disequilibria for some of the glasses, along with the wide range in their chemical compositions and Th/U ratios should provide useful reference points for the U-series analytical community.

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

Science.gov (United States)

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

2018-04-15

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

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

International Nuclear Information System (INIS)

Rukihati; Sumadjo

2001-01-01

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

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

Czech Academy of Sciences Publication Activity Database

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

2015-01-01

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

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).

[Determination of total mass and morphology analysis of heavy metal in soil with potassium biphthalate-sodium hydroxide by ICP-AES].

Science.gov (United States)

Qu, Jiao; Yuan, Xing; Cong, Qiao; Wang, Shuang

2008-11-01

Blank soil was used as quality controlling samples, soil sample dealt by potassium biphthalate-sodium hydroxide buffer solution was used as check sample, mixed acid HNO3-HF-HClO4 was chosen to nitrify soil samples, and plasma emission spectrometer (ICP-AES) was used as detecting method. The authors determined the total metal mass of Mo, Pb, As, Hg, Cr, Cd, Zn, Cu and Ni in the extracted and dealt soil samples, and determined the mass of Mo, Pb, As, Hg, Cr, Cd, Zn, Cu and Ni in the three chemical morphologies, including acid extractable morphology, oxide associated morphology, and organics associated modality. The experimental results indicated that the different pH of potassium biphthalate-sodium hydroxide buffer solution had obvious influence on the total mass of heavy metal and morphology transformation. Except for metal element Pb and Zn, the addition of different pH potassium dihydrogen phosphate-sodium hydroxide buffer solution could accelerate the soil samples nitrification and the total mass determination of heavy metal in the soil samples. The potassium biphthalate-sodium hydroxide buffer solution could facilitate the acid extractable morphology of Cr, Cu, Hg and Pb, oxidation associated morphology of As, Hg, Pb and Zn and the organic associated morphology transforming of As and Hg. At pH 5.8, the maximum acid extractable morphology contents of Cu and Hg were 2.180 and 0.632 mg x kg(-1), respectively; at pH 6.2, the maximal oxidation associated morphology content of Pb could achieve 27.792 mg x kg(-1); at pH 6.0, the maximum organic associated morphology content of heavy metal Hg was 4.715 mg x kg(-1).

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

Science.gov (United States)

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

2017-11-07

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

Ophthalmodynamometry for ICP prediction and pilot test on Mt. Everest.

Science.gov (United States)

Querfurth, Henry W; Lieberman, Philip; Arms, Steve; Mundell, Steve; Bennett, Michael; van Horne, Craig

2010-11-01

A recent development in non-invasive techniques to predict intracranial pressure (ICP) termed venous ophthalmodynamometry (vODM) has made measurements in absolute units possible. However, there has been little progress to show utility in the clinic or field. One important application would be to predict changes in actual ICP during adaptive responses to physiologic stress such as hypoxia. A causal relationship between raised intracranial pressure and acute mountain sickness (AMS) is suspected. Several MRI studies report that modest physiologic increases in cerebral volume, from swelling, normally accompany subacute ascent to simulated high altitudes. 1) Validate and calibrate an advanced, portable vODM instrument on intensive patients with raised intracranial pressure and 2) make pilot, non-invasive ICP estimations of normal subjects at increasing altitudes. The vODM was calibrated against actual ICP in 12 neurosurgical patients, most affected with acute hydrocephalus and monitored using ventriculostomy/pressure transducers. The operator was blinded to the transducer read-out. A clinical field test was then conducted on a variable data set of 42 volunteer trekkers and climbers scaling Mt. Everest, Nepal. Mean ICPs were estimated at several altitudes on the ascent both across and within subjects. Portable vODM measurements increased directly and linearly with ICP resulting in good predictability (r = 0.85). We also found that estimated ICP increases normally with altitude (10 ± 3 mm Hg; sea level to 20 ± 2 mm Hg; 6553 m) and that AMS symptoms did not correlate with raised ICP. vODM technology has potential to reliably estimate absolute ICP and is portable. Physiologic increases in ICP and mild-mod AMS are separate responses to high altitude, possibly reflecting swelling and vasoactive instability, respectively.

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

Directory of Open Access Journals (Sweden)

Jie Lin

2016-06-01

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

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

Science.gov (United States)

Nadoll, P.; Koenig, A.E.

2011-01-01

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

Optoelectronic properties of Black-Silicon generated through inductively coupled plasma (ICP) processing for crystalline silicon solar cells

Energy Technology Data Exchange (ETDEWEB)

Hirsch, Jens, E-mail: J.Hirsch@emw.hs-anhalt.de [Anhalt University of Applied Sciences, Faculty EMW, Bernburger Str. 55, DE-06366 Köthen (Germany); Fraunhofer Center for Silicon Photovoltaics CSP, Otto-Eißfeldt-Str. 12, DE-06120 Halle (Saale) (Germany); Gaudig, Maria; Bernhard, Norbert [Anhalt University of Applied Sciences, Faculty EMW, Bernburger Str. 55, DE-06366 Köthen (Germany); Lausch, Dominik [Fraunhofer Center for Silicon Photovoltaics CSP, Otto-Eißfeldt-Str. 12, DE-06120 Halle (Saale) (Germany)

2016-06-30

Highlights: • Fabrication of black silicon through inductively coupled plasma (ICP) processing. • Suppressed formation a self-bias and therefore a reduced ion bombardment of the silicon sample. • Reduction of the average hemispherical reflection between 300 and 1120 nm up to 8% within 5 min ICP process time. • Reflection is almost independent of the angle of incidence up to 60°. • 2.5 ms effective lifetime at 10{sup 15} cm{sup −3} MCD after ALD Al{sub 2}O{sub 3} surface passivation. - Abstract: The optoelectronic properties of maskless inductively coupled plasma (ICP) generated black silicon through SF{sub 6} and O{sub 2} are analyzed by using reflection measurements, scanning electron microscopy (SEM) and quasi steady state photoconductivity (QSSPC). The results are discussed and compared to capacitively coupled plasma (CCP) and industrial standard wet chemical textures. The ICP process forms parabolic like surface structures in a scale of 500 nm. This surface structure reduces the average hemispherical reflection between 300 and 1120 nm up to 8%. Additionally, the ICP texture shows a weak increase of the hemispherical reflection under tilted angles of incidence up to 60°. Furthermore, we report that the ICP process is independent of the crystal orientation and the surface roughness. This allows the texturing of monocrystalline, multicrystalline and kerf-less wafers using the same parameter set. The ICP generation of black silicon does not apply a self-bias on the silicon sample. Therefore, the silicon sample is exposed to a reduced ion bombardment, which reduces the plasma induced surface damage. This leads to an enhancement of the effective charge carrier lifetime up to 2.5 ms at 10{sup 15} cm{sup −3} minority carrier density (MCD) after an atomic layer deposition (ALD) with Al{sub 2}O{sub 3}. Since excellent etch results were obtained already after 4 min process time, we conclude that the ICP generation of black silicon is a promising technique

Ophthalmodynamometry for ICP prediction and pilot test on Mt. Everest

Directory of Open Access Journals (Sweden)

Bennett Michael

2010-11-01

Full Text Available Abstract Background A recent development in non-invasive techniques to predict intracranial pressure (ICP termed venous ophthalmodynamometry (vODM has made measurements in absolute units possible. However, there has been little progress to show utility in the clinic or field. One important application would be to predict changes in actual ICP during adaptive responses to physiologic stress such as hypoxia. A causal relationship between raised intracranial pressure and acute mountain sickness (AMS is suspected. Several MRI studies report that modest physiologic increases in cerebral volume, from swelling, normally accompany subacute ascent to simulated high altitudes. Objectives 1 Validate and calibrate an advanced, portable vODM instrument on intensive patients with raised intracranial pressure and 2 make pilot, non-invasive ICP estimations of normal subjects at increasing altitudes. Methods The vODM was calibrated against actual ICP in 12 neurosurgical patients, most affected with acute hydrocephalus and monitored using ventriculostomy/pressure transducers. The operator was blinded to the transducer read-out. A clinical field test was then conducted on a variable data set of 42 volunteer trekkers and climbers scaling Mt. Everest, Nepal. Mean ICPs were estimated at several altitudes on the ascent both across and within subjects. Results Portable vODM measurements increased directly and linearly with ICP resulting in good predictability (r = 0.85. We also found that estimated ICP increases normally with altitude (10 ± 3 mm Hg; sea level to 20 ± 2 mm Hg; 6553 m and that AMS symptoms did not correlate with raised ICP. Conclusion vODM technology has potential to reliably estimate absolute ICP and is portable. Physiologic increases in ICP and mild-mod AMS are separate responses to high altitude, possibly reflecting swelling and vasoactive instability, respectively.

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

Science.gov (United States)

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

2018-01-01

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

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

Science.gov (United States)

2015-04-01

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

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

Science.gov (United States)

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

2018-05-15

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

Laser ablation ICP-MS for quantitative biomedical applications

International Nuclear Information System (INIS)

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

2012-01-01

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

Analysis of humic colloid borne trace elements by flow field-flow fractionation, gel permeation chromatography and icp-mass spectrometry

International Nuclear Information System (INIS)

Ngo, Manh Thang; Beck, H.P; Geckeis, H.; Kim, J.I.

1999-01-01

Groundwater samples containing aquatic humic substances are analyzed by flow field- flow fractionation (FFFF) and gel permeation chromatography (GPC). Natural concentrations of U, Th and rare earth elements (REE) in a size-fractionated groundwater sample are analyzed by on-line coupling of inductively coupled plasma-mass spectrometry (ICP-MS) to either FFFF or GPC. The uranium, thorium, and REE are found to be quantitatively attached to colloidal species in the investigated groundwater sample. Their distribution in different colloid size fractions, however, is quite heterogeneous. Both, FFFF and GPC reveal that Th and REE are preferentially located in the size fraction > 50 kDalton. U is also attached to low molecular weight humic acid, similar to Fe and Al. This finding could be qualitatively reproduced by sequential ultrafiltration. The results are interpreted in terms of different binding mechanisms for the individual elements in the heterogeneous humic macromolecules. The inclusion of actinides into larger aggregates of aquatic humic acid might explain the considerable kinetic hindrance of actinide-humic acid dissociation reactions described in the literature. (authors)

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

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

International Nuclear Information System (INIS)

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

1993-01-01

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

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

International Nuclear Information System (INIS)

Wahlen, Raimund; Wolff-Briche, Celine

2003-01-01

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Science.gov (United States)

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

2017-01-01

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

Determination of 129I/127I isotope ratios in liquid solutions and environmental soil samples by ICP-MS with hexapole collision cell

OpenAIRE

Izmer, A. V.; Boulyga, S. F.; Becker, J. S.

2003-01-01

The determination of I-129 in environmental samples at ultratrace levels is very difficult by ICP-MS due to a high noise caused by Xe impurities in argon plasma gas (interference of Xe-129(+)), possible (IH2+)-I-127 interference and an insufficient abundance ratio sensitivity of the ICP mass spectrometer for I-129/I-127 isotope ratio measurement. A sensitive, powerful and fast analytical technique for iodine isotope ratio measurements in aqueous solutions and contaminated soil samples directl...

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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

International Nuclear Information System (INIS)

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

2000-01-01

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

Analysis of inorganic and organic constituents of myrrh resin by GC–MS and ICP-MS: An emphasis on medicinal assets

Directory of Open Access Journals (Sweden)

Syed Rizwan Ahamad

2017-07-01

Full Text Available The aim of the present investigation was to explore the constituents of the Arabian myrrh resin obtained from Commiphora myrrha. The organic and inorganic composition of the myrrh gum resin has been investigated using gas chromatography-mass spectrometry (GC–MS and inductively coupled plasma-mass spectrometry (ICP-MS. Analysis executed by ICP-MS reveals the presence of various inorganic elements in significant amount in the myrrh resin. The elements that were found to be present in large amounts include calcium, magnesium, aluminum, phosphorus, chlorine, chromium, bromine and scandium. The important organic constituents identified in the myrrh ethanolic extract include limonene, curzerene, germacrene B, isocericenine, myrcenol, beta selinene, and spathulenol,. The present work complements other myrrh associated investigations done in the past and provides additional data for the future researches.

Analysis of inorganic and organic constituents of myrrh resin by GC-MS and ICP-MS: An emphasis on medicinal assets.

Science.gov (United States)

Ahamad, Syed Rizwan; Al-Ghadeer, Abdul Rahman; Ali, Raisuddin; Qamar, Wajhul; Aljarboa, Suliman

2017-07-01

The aim of the present investigation was to explore the constituents of the Arabian myrrh resin obtained from Commiphora myrrha. The organic and inorganic composition of the myrrh gum resin has been investigated using gas chromatography-mass spectrometry (GC-MS) and inductively coupled plasma-mass spectrometry (ICP-MS). Analysis executed by ICP-MS reveals the presence of various inorganic elements in significant amount in the myrrh resin. The elements that were found to be present in large amounts include calcium, magnesium, aluminum, phosphorus, chlorine, chromium, bromine and scandium. The important organic constituents identified in the myrrh ethanolic extract include limonene, curzerene, germacrene B, isocericenine, myrcenol, beta selinene, and spathulenol,. The present work complements other myrrh associated investigations done in the past and provides additional data for the future researches.

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

Science.gov (United States)

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

2007-11-28

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

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

Science.gov (United States)

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

2017-12-18

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

Integrated care pathways for airway diseases (AIRWAYS-ICPs)

NARCIS (Netherlands)

Bousquet, J.; Addis, A.; Adcock, I.; Agache, I.; Agusti, A.; Alonso, A.; Annesi-Maesano, I.; Anto, J. M.; Bachert, C.; Baena-Cagnani, C. E.; Bai, C.; Baigenzhin, A.; Barbara, C.; Barnes, P. J.; Bateman, E. D.; Beck, L.; Bedbrook, A.; Bel, E. H.; Benezet, O.; Bennoor, K. S.; Benson, M.; Bernabeu-Wittel, M.; Bewick, M.; Bindslev-Jensen, C.; Blain, H.; Blasi, F.; Bonini, M.; Bonini, S.; Boulet, L. P.; Bourdin, A.; Bourret, R.; Bousquet, P. J.; Brightling, C. E.; Briggs, A.; Brozek, J.; Buhl, R.; Bush, A.; Caimmi, D.; Calderon, M.; Calverley, P.; Camargos, P. A.; Camuzat, T.; Canonica, G. W.; Carlsen, K. H.; Casale, T. B.; Cazzola, M.; Cepeda Sarabia, A. M.; Cesario, A.; Chen, Y. Z.; Chkhartishvili, E.; Chavannes, N. H.; Chiron, R.; Chuchalin, A.; Chung, K. F.; Cox, L.; Crooks, G.; Crooks, M. G.; Cruz, A. A.; Custovic, A.; Dahl, R.; Dahlen, S. E.; de Blay, F.; Dedeu, T.; Deleanu, D.; Demoly, P.; Devillier, P.; Didier, A.; Dinh-Xuan, A. T.; Djukanovic, R.; Dokic, D.; Douagui, H.; Dubakiene, R.; Eglin, S.; Elliot, F.; Emuzyte, R.; Fabbri, L.; Fink Wagner, A.; Fletcher, M.; Fokkens, W. J.; Fonseca, J.; Franco, A.; Frith, P.; Furber, A.; Gaga, M.; Garcés, J.; Garcia-Aymerich, J.; Gamkrelidze, A.; Gonzales-Diaz, S.; Gouzi, F.; Guzmán, M. A.; Haahtela, T.; Harrison, D.; Hayot, M.; Heaney, L. G.; Heinrich, J.; Hellings, P. W.; Hooper, J.; Humbert, M.; Hyland, M.; Iaccarino, G.; Jakovenko, D.; Jardim, J. R.; Jeandel, C.; Jenkins, C.; Johnston, S. L.; Jonquet, O.; Joos, G.; Jung, K. S.; Kalayci, O.; Karunanithi, S.; Keil, T.; Khaltaev, N.; Kolek, V.; Kowalski, M. L.; Kull, I.; Kuna, P.; Kvedariene, V.; Le, L. T.; Lodrup Carlsen, K. C.; Louis, R.; MacNee, W.; Mair, A.; Majer, I.; Manning, P.; de Manuel Keenoy, E.; Masjedi, M. R.; Melen, E.; Melo-Gomes, E.; Menzies-Gow, A.; Mercier, G.; Mercier, J.; Michel, J. P.; Miculinic, N.; Mihaltan, F.; Milenkovic, B.; Molimard, M.; Momas, I.; Montilla-Santana, A.; Morais-Almeida, M.; Morgan, M.; N'Diaye, M.; Nafti, S.; Nekam, K.; Neou, A.; Nicod, L.; O'Hehir, R.; Ohta, K.; Paggiaro, P.; Palkonen, S.; Palmer, S.; Papadopoulos, N. G.; Papi, A.; Passalacqua, G.; Pavord, I.; Pigearias, B.; Plavec, D.; Postma, D. S.; Price, D.; Rabe, K. F.; Radier Pontal, F.; Redon, J.; Rennard, S.; Roberts, J.; Robine, J. M.; Roca, J.; Roche, N.; Rodenas, F.; Roggeri, A.; Rolland, C.; Rosado-Pinto, J.; Ryan, D.; Samolinski, B.; Sanchez-Borges, M.; Schünemann, H. J.; Sheikh, A.; Shields, M.; Siafakas, N.; Sibille, Y.; Similowski, T.; Small, I.; Sola-Morales, O.; Sooronbaev, T.; Stelmach, R.; Sterk, P. J.; Stiris, T.; Sud, P.; Tellier, V.; To, T.; Todo-Bom, A.; Triggiani, M.; Valenta, R.; Valero, A. L.; Valiulis, A.; Valovirta, E.; van Ganse, E.; Vandenplas, O.; Vasankari, T.; Vestbo, J.; Vezzani, G.; Viegi, G.; Visier, L.; Vogelmeier, C.; Vontetsianos, T.; Wagstaff, R.; Wahn, U.; Wallaert, B.; Whalley, B.; Wickman, M.; Williams, D. M.; Wilson, N.; Yawn, B. P.; Yiallouros, P. K.; Yorgancioglu, A.; Yusuf, O. M.; Zar, H. J.; Zhong, N.; Zidarn, M.; Zuberbier, T.

2014-01-01

The objective of Integrated Care Pathways for Airway Diseases (AIRWAYS-ICPs) is to launch a collaboration to develop multi-sectoral care pathways for chronic respiratory diseases in European countries and regions. AIRWAYS-ICPs has strategic relevance to the European Union Health Strategy and will

Integrated care pathways for airway diseases (AIRWAYS-ICPs)

NARCIS (Netherlands)

Bousquet, J.; Addis, A.; Adcock, I.; Agache, I.; Agusti, A.; Alonso, A.; Annesi-Maesano, I.; Anto, J. M.; Bachert, C.; Baena-Cagnani, C. E.; Bai, C.; Baigenzhin, A.; Barbara, C.; Barnes, P. J.; Bateman, E. D.; Beck, L.; Bedbrook, A.; Bel, E. H.; Benezet, O.; Bennoor, K. S.; Benson, M.; Bernabeu-Wittel, M.; Bewick, M.; Bindslev-Jensen, C.; Blain, H.; Blasi, F.; Bonini, M.; Bonini, S.; Boulet, L. P.; Bourdin, A.; Bourret, R.; Bousquet, P. J.; Brightling, C. E.; Briggs, A.; Brozek, J.; Buh, R.; Bush, A.; Caimmi, D.; Calderon, M.; Calverley, P.; Camargos, P. A.; Camuzat, T.; Canonica, G. W.; Carlsen, K. H.; Casale, T. B.; Cazzola, M.; Sarabia, A. M. Cepeda; Cesario, A.; Chen, Y. Z.; Chkhartishvili, E.; Chavannes, N. H.; Chiron, R.; Chuchalin, A.; Chung, K. F.; Cox, L.; Crooks, G.; Crooks, M. G.; Cruz, A. A.; Custovic, A.; Dahl, R.; Dahlen, S. E.; De Blay, F.; Dedeu, T.; Deleanu, D.; Demoly, P.; Devillier, P.; Didier, A.; Dinh-Xuan, A. T.; Djukanovic, R.; Dokic, D.; Douagui, H.; Dubakiene, R.; Eglin, S.; Elliot, F.; Emuzyte, R.; Fabbri, L.; Wagner, A. Fink; Fletcher, M.; Fokkens, W. J.; Fonseca, J.; Franco, A.; Frith, P.; Furber, A.; Gaga, M.; Garces, J.; Garcia-Aymerich, J.; Gamkrelidze, A.; Gonzales-Diaz, S.; Gouzi, F.; Guzman, M. A.; Haahtela, T.; Harrison, D.; Hayot, M.; Heaney, L. G.; Heinrich, J.; Hellings, P. W.; Hooper, J.; Humbert, M.; Hyland, M.; Iaccarino, G.; Jakovenko, D.; Jardim, J. R.; Jeandel, C.; Jenkins, C.; Johnston, S. L.; Jonquet, O.; Joos, G.; Jung, K. S.; Kalayci, O.; Karunanithi, S.; Keil, T.; Khaltaev, N.; Kolek, V.; Kowalski, M. L.; Kull, I.; Kuna, P.; Kvedariene, V.; Le, L. T.; Carlsen, K. C. Lodrup; Louis, R.; MacNee, W.; Mair, A.; Majer, I.; Manning, P.; Keenoy, E. de Manuel; Masjedi, M. R.; Meten, E.; Melo-Gomes, E.; Menzies-Gow, A.; Mercier, G.; Mercier, J.; Michel, J. P.; Miculinic, N.; Mihaltan, F.; Milenkovic, B.; Molimard, M.; Mamas, I.; Montilla-Santana, A.; Morais-Almeida, M.; Morgan, M.; N'Diaye, M.; Nafti, S.; Nekam, K.; Neou, A.; Nicod, L.; O'Hehir, R.; Ohta, K.; Paggiaro, P.; Palkonen, S.; Palmer, S.; Papadopoulos, N. G.; Papi, A.; Passalacqua, G.; Pavord, I.; Pigearias, B.; Plavec, D.; Postma, D. S.; Price, D.; Rabe, K. F.; Pontal, F. Radier; Redon, J.; Rennard, S.; Roberts, J.; Robine, J. M.; Roca, J.; Roche, N.; Rodenas, F.; Roggeri, A.; Rolland, C.; Rosado-Pinto, J.; Ryan, D.; Samolinski, B.; Sanchez-Borges, M.; Schunemann, H. J.; Sheikh, A.; Shields, M.; Siafakas, N.; Sibille, Y.; Similowski, T.; Small, I.; Sola-Morales, O.; Sooronbaev, T.; Stelmach, R.; Sterk, P. J.; Stiris, T.; Sud, P.; Tellier, V.; To, T.; Todo-Bom, A.; Triggiani, M.; Valenta, R.; Valero, A. L.; Valiulis, A.; Valovirta, E.; Van Ganse, E.; Vandenplas, O.; Vasankari, T.; Vestbo, J.; Vezzani, G.; Viegi, G.; Visier, L.; Vogelmeier, C.; Vontetsianos, T.; Wagstaff, R.; Wahn, U.; Wallaert, B.; Whalley, B.; Wickman, M.; Williams, D. M.; Wilson, N.; Yawn, B. P.; Yiallouros, P. K.; Yorgancioglu, A.; Yusuf, O. M.; Zar, H. J.; Zhong, N.; Zidarn, M.; Zuberbier, T.

The objective of Integrated Care Pathways for Airway Diseases (AIRWAYS-ICPs) is to launch a collaboration to develop multi-sectoral care pathways for chronic respiratory diseases in European countries and regions. AIRWAYS-ICPs has strategic relevance to the European Union Health Strategy and will

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

Science.gov (United States)

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

2017-08-01

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

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

International Nuclear Information System (INIS)

Hiroma, Yuki; Nakai, Izumi; Hokura, Akiko

2010-01-01

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

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

Analysis of impurities in uranium oxide by ICP-MS

International Nuclear Information System (INIS)

Paul, M.; Hager, J.

1989-01-01

The method offers detection limits of less than 0.1 μg/g in solid samples and a wide linear dynamic working range and allows a fast sample throughput. The poster summarizes recent authors' experience with the analysis of high purity uranium oxide. The samples are analyzed using both conventional solution analysis and solid sampling method, using a new powerful laser sampling system attached to the ICP mass spectrometer. The total analysis time required for one uranium oxide sample is about 4 minutes including sample handling, data acquisition and processing. The results achieved from semiquantitative and quantitative analysis applying both techniques are in good agreement with the reference values. (author)

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-07-01

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

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

Science.gov (United States)

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

2018-02-01

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

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

International Nuclear Information System (INIS)

Voica, Cezara; Dehelean, Adriana; Pamula, A

2009-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-08-01

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

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

OpenAIRE

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

2016-01-01

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

Soil analyses by ICP-MS (Review)

International Nuclear Information System (INIS)

Yamasaki, Shin-ichi

2000-01-01

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

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

Science.gov (United States)

Qu, W; Du, A; Zhao, D

2001-10-31

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

ICP experiments more durable pavements

International Nuclear Information System (INIS)

Carta Petrolera

1994-01-01

A new asphalts technology that will make more durable the pavement in the highways and roads of the cities of Colombia investigates the Colombian Institute of the Petroleum ICP. The project that will have important incidence in the solution of one of the main problems in the roads of cities like Bogota, is only one of the 35 investigation programs and application of new technologies that with relationship to the sector of the hydrocarbons and its influence branches the ICP advances. The investigation looks for to elevate the current average of useful life of the pavements, with that it would be reached a standard that has the developed countries in this field

Analytical applications of ICP-FTS

International Nuclear Information System (INIS)

Faires, L.M.; Palmer, B.A.; Cunningham, P.T.

1986-01-01

The Analytical Chemistry Group of the Chemistry Division at Los Alamos National Laboratory has been investigating the analytical utility of the inductively coupled plasma (ICP) - Fourier transform spectrometer (FTS) combination. While a new state-of-the-art FTS facility is under construction at Los Alamos, preliminary data has been obtained on the one-meter FTS at the National Solar Observatory at Kitt Peak, Arizona. This paper presents an update of the Los Alamos FTS facility, which is expected to be completed in 1986, and presents data showing the analytical potential of an ICP-FTS system. Some of the potential problems of the multiplex disadvantage are discussed, and the advantages of the high resolution obtainable with the FTS are illustrated

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

Science.gov (United States)

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

2017-05-22

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

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

Science.gov (United States)

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

2017-10-02

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

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

Energy Technology Data Exchange (ETDEWEB)

Pitois, A

2006-04-15

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

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

Science.gov (United States)

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

2017-10-15

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

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

Science.gov (United States)

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

2017-01-01

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

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

DEFF Research Database (Denmark)

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

2018-01-01

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

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

International Nuclear Information System (INIS)

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

2011-01-01

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

High-resolution U-series dates from the Sima de los Huesos hominids yields 600 +∞-66: implications for the evolution of the early Neanderthal lineage

Science.gov (United States)

Bischoff, James L.; Williams, Ross W.; Rosenbauer, Robert J.; Aramburu, Arantza; Arsuaga, Juan Luis; Garcia, Nuria; Cuenca-Bescos, Gloria

2007-01-01

The Sima de los Huesos site of the Atapuerca complex near Burgos, Spain contains the skeletal remains of at least 28 individuals in a mud-breccia underlying an accumulation of the Middle Pleistocene cave bear (Ursus deningeri). We report here on new high-precision dates on the recently discovered speleothem SRA-3 overlaying human bones within the Sima de los Huesos. Earlier analyses of this speleothem by TIMS (thermal-ionization mass-spectrometry) showed the lower part to be indistinguishable from internal isotopic equilibrium at the precision of the TIMS instrumentation used, yielding minimum age of 350 kyr (kyr = 103 yr before present). Reanalysis of six samples of SRA-3 by inductively-coupled plasma-multicollector mass-spectrometry (ICP-MS) produced high-precision analytical results allowing calculation of finite dates. The new dates cluster around 600 kyr. A conservative conclusion takes the lower error limit ages as the minimum age of the speleothem, or 530 kyr. This places the SH hominids at the very beginnings of the Neandertal evolutionary lineage.

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

Energy Technology Data Exchange (ETDEWEB)

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

2001-07-01

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

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

Science.gov (United States)

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

2015-01-01

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

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

Science.gov (United States)

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

2013-01-01

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

Small-Volume U-Pb Zircon Geochronology by Laser Ablation-Multicollector-ICP-MS

Science.gov (United States)

2008-11-03

Ecstall pluton in the Coast Mountains of British Columbia: Evidence for local deformation rather than large-scale transport. Journal of Geophysical...Journal of Metamorphic Geology 18, 719–735. Kalsbeek, F., Jepsen, H.F., Nutman, A.P., 2001. From source migmatites to plutons : tracking the origin of

ICP-MS Workshop

Energy Technology Data Exchange (ETDEWEB)

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

2014-11-01

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

Evaluation of lead isotope compositions of NIST NBS 981 measured by thermal ionization mass spectrometer and multiple-collector inductively coupled plasma mass spectrometer

Directory of Open Access Journals (Sweden)

Honglin Yuan

2016-09-01

Full Text Available Because Pb isotopes can be used for tracing, they are widely used in many disciplines. The detection and analysis of Pb isotopes of bulk samples are usually conducted using thermal ionization mass spectrometer (TIMS and multiple-collector inductively coupled plasma mass spectrometer (MC-ICP-MS, both of which need external reference materials with known isotopic compositions to correct for the mass discrimination effect produced during analysis. NIST NBS 981 is the most widely used reference material for Pb isotope analysis; however, the isotopic compositions reported by various analytical laboratories, especially those using TIMS, vary from each other. In this study, we statistically evaluated 229 reported TIMS analysis values collected by GeoReM in the last 30 years, 176 reported MC-ICP-MS analysis values, and 938 MC-ICP-MS analysis results from our laboratory in the last five years. After careful investigation, only 40 TIMS results were found to have double or triple spikes. The ratios of the overall weighted averages, 206Pb/204Pb, 207Pb/204Pb, and 208Pb/204Pb, obtained from 40 spiked TIMS reports and 1114 MC-ICP-MS results of NIST NBS 981 isotopes were 16.9406 ± 0.0003 (2s, 15.4957 ± 0.0002 (2s, and 36.7184 ± 0.0007 (2s, respectively.

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

International Nuclear Information System (INIS)

Oliveira, Thiago Cesar de

2014-01-01

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

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

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

Determination of Mg/Ca ratio of stalagmite by laser multicollector inductively coupled plasma mass spectrometry

International Nuclear Information System (INIS)

He Xuexian; Zhu Xiangkun; Tang Suohan; Yang Chun; Cai Junjun; Li Shizhen; Li Zhihong

2005-01-01

A method for determining Mg/Ca of stalagmite by LA-MC-ICPMS is studied. 24 Mg/ 44 Ca (Mass 22, intensity of 44C a 2+ , collected by ion counting and mass 24, intensity of 24 Mg + , collected by Faraday cup) ratios were measured in replace of Mg/Ca ratios. Both diameter of laser sampling spot and laser moving increment were 2- μm. The curve of Mg/Ca vs. distance directly was obtained. The result indicates that relative Mg/Ca ratios changed from 0.5 to 2.0 this stalagmite and it is enough to reflect environmental factors act. (authors)

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

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

International Nuclear Information System (INIS)

Beuvier, Ludovic

2015-01-01

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

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

Science.gov (United States)

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

2013-03-01

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

Application of ICP-QMS for the determination of ultratrace-levels of 226Ra in geothermal water and sediment samples

International Nuclear Information System (INIS)

Tsuey-Lin Tsai; Tsung-Yuan Wang; Hwa-Jou Wei; Lee-Chung Men; Chun-Chih Lin

2010-01-01

A rapid, accurate and less labor intensive approach to determining 226 Ra in environmental samples was examined; this utilized quadrupole-based inductively coupled plasma mass spectrometry (ICP-QMS). The procedure used chemical separation by ion exchange chromatography to remove most of the matrices after coprecipitation with BaSO 4 . The average chemical recovery of the NIST SRM preparation method ranged from 60.5 to 85.9% using 133 Ba as internal tracer by gamma counting. This technique was capable of completing a 226 Ra measurement within 3 min. It did not require an in-growth period to allow radon and its progeny to achieve secular equilibrium with the parent 226 Ra as is needed for liquid scintillation analyzer (LSA). The method detection limits for the determination of 226 Ra in geothermal water and sediment samples were 0.02 mBq L -1 (0.558 fg L -1 ) and 0.10 Bq kg -1 (2.79 fg g -1 ), respectively. The results obtained with various natural samples and the suitability of the method when applied to various environmental matrices such as geothermal water and sediment are discussed. When ICP-QMS was compared to double-focusing magnetic sector field inductively coupled plasma mass spectrometry (ICP-SFMS), good agreement was obtained with a correlation coefficient, r 2 = 0.982. (author)

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

International Nuclear Information System (INIS)

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

2014-01-01

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

Effect of postural changes on ICP in healthy and ill subjects

DEFF Research Database (Denmark)

Petersen, Lonnie G; Juhler, Marianne

2015-01-01

to distinguish normal human physiology from disease entities such as idiopathic intracranial hypertension and normal pressure hydrocephalus, we investigated ICP in different body postures in both normal and ill subjects. METHODS: Thirty-one patients were included: four normal patients following complete removal......: upright standing, sitting in a chair, supine and right lateral lumbar puncture position. RESULTS: Linear regression of median ICP based on patient posture, group, and purpose of monitoring presented a significant model (p ... of differences in median ICP between body postures and supine ICP as the baseline, presented a highly significant model (p posture (p postures enabled...

Plutonium determination in urine by techniques of mass spectrometry

International Nuclear Information System (INIS)

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

2013-10-01

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

Method for separation of Cs from acid solution dissolving radionuclides and microanalysis of solution with ICP-AES

International Nuclear Information System (INIS)

Kanazawa, Toru; Hidaka, Akihide; Kudo, Tamotsu; Nakamura, Takehiko; Fuketa, Toyoshi

2004-06-01

The VEGA (Verification Experiments of radionuclides Gas/Aerosol release) program is being performed at JAERI to understand mechanisms of radionuclides release from irradiated fuel during severe accidents. As a part of evaluation in the program, the mass balances of released and deposited FP (Fission Products) onto the test apparatus are estimated from gamma ray measurement for acid solution leached from the apparatus, but short-life nuclides are difficult to be measured because those in the VEGA fuel have been mostly depleted due to cooling for several years. Moreover, the radionuclides without emitting gamma rays and very small quantity of elements cannot be quantified by gamma ray measurement. Therefore, a microanalysis by ICP-AES (Inductively Coupled Plasma - Atomic Emission Spectrometry) for the acid solution leached from VEGA apparatuses is being applied to evaluate the released and deposited masses for those elements. Since Cs-134 and -137, which are major FP dissolved in the solution, have high intensity of gamma ray spectrum, they have to be removed from the solution before the microanalysis in order to avoid contamination of ICP system and to decrease exposure to gamma ray. In this report, methods for separation of Cs from acid solution were reviewed and the applicability of them to the ICP-AES analysis was discussed. The method for Cs separation using the inorganic ion exchanger, AMP (Ammonium Molybdate Phosphate) was applied to the solutions of cold and hot test and the effectiveness was examined. The results showed that more than 99.9% of Cs could be removed from the test solutions, and once removed Sb by AMP was recovered by using a complexing agent such as citric acid. Next, the method was applied to an acid solution leached from VEGA-3 apparatus, and ICP-AES analysis was performed for it. The analysis showed that amount of U, Sr and Zr were successfully quantified. Most of elements to be analyzed were measurable except for Sb, Ag and Sn, although

Cu isotopic signature in blood serum of liver transplant patients: a follow-up study

Science.gov (United States)

Lauwens, Sara; Costas-Rodríguez, Marta; van Vlierberghe, Hans; Vanhaecke, Frank

2016-07-01

End-stage liver disease (ESLD) is life-threatening and liver transplantation (LTx) is the definitive treatment with good outcomes. Given the essential role of hepatocytes in Cu homeostasis, the potential of the serum Cu isotopic composition for monitoring a patient’s condition post-LTx was evaluated. For this purpose, high-precision Cu isotopic analysis of blood serum of ESLD patients pre- and post-LTx was accomplished via multi-collector ICP-mass spectrometry (MC-ICP-MS). The Cu isotopic composition of the ESLD patients was fractionated in favour of the lighter isotope (by about -0.50‰). Post-LTx, a generalized normalization of the Cu isotopic composition was observed for the patients with normal liver function, while it remained light when this condition was not reached. A strong decrease in the δ65Cu value a longer term post-LTx seems to indicate the recurrence of liver failure or cancer. The observed trend in favour of the heavier Cu isotopic composition post-LTx seems to be related with the restored biosynthetic capacity of the liver, the restored hepatic metabolism and/or the restored biliary secretion pathways. Thus, Cu isotopic analysis could be a valuable tool for the follow-up of liver transplant patients and for establishing the potential recurrence of liver failure.

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

International Nuclear Information System (INIS)

Kasprzak, L.M.

2007-01-01

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

Isotope dilution ICP-MS with laser-assisted sample introduction for direct determination of sulfur in petroleum products.

Science.gov (United States)

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

2005-08-01

Inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with direct laser-assisted introduction of isotope-diluted samples into the plasma, using a laser ablation system with high ablation rates, was developed for accurate sulfur determinations in different petroleum products such as 'sulfur-free' premium gasoline, diesel fuel, and heating oil. Two certified gas oil reference materials were analyzed for method validation. Two different 34S-enriched spike compounds, namely, elementary sulfur dissolved in xylene and dibenzothiophene in hexane, were synthesized and tested for their usefulness in this isotope dilution technique. The isotope-diluted sample was adsorbed on a filter-paper-like material, which was fixed in a special holder for irradiation by the laser beam. Under these conditions no time-dependent spike/analyte fractionation was only observed for the dibenzothiophene spike during the laser ablation process, which means that the measured 34S/32S isotope ratio of the isotope-diluted sample remained constant-a necessary precondition for accurate results with the isotope dilution technique. A comparison of LA-ICP-IDMS results with the certified values of the gas oil reference materials and with results obtained from ICP-IDMS analyses with wet sample digestion demonstrated the accuracy of the new LA-ICP-IDMS method in the concentration range of 9.2 microg g(-1) ('sulfur-free' premium gasoline) to 10.4 mg g(-1) (gas oil reference material BCR 107). The detection limit for sulfur by LA-ICP-IDMS is 0.04 microg g(-1) and the analysis time is only about 10 min, which therefore also qualifies this method for accurate determinations of low sulfur contents in petroleum products on a routine level.

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-07-01

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

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

Science.gov (United States)

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

2018-04-01

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

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

Science.gov (United States)

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

2014-09-01

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

Surface modification of ceramic materials induced by irradiation of high power pulsed ICP

International Nuclear Information System (INIS)

Ishigaki, Takamasa; Okada, Nobuhiro; Ohashi, Naoki; Haneda, Hajime

2003-01-01

Newly developed pulse-modulated high-power inductively coupled plasma [ICP] is expected to offer the unique physico-chemical condition, such as the increased concentration of chemically reactive species, as well as the appropriate heat flux for materials processing. Two kinds of oxide materials, titanium and zinc oxide, were placed at the downstream of Ar-H 2 ICP and irradiated in the plasma of continuous [CN] and pulse-modulated [PM] modes. The CN-ICP irradiation at the position close to the plasma tail gave rise to the thermal reduction of oxides. In the PM-ICP irradiation, the degree of thermal reduction depended on the lower power level during pulse-off time, as well as the total electric power. Irradiation in PM-ICP led to the increased formation of oxygen vacancies in titanium dioxide. In the case of zinc oxide, the UV emission efficiency was improved by PM-ICP irradiation, while the green emission became predominant by CN-ICP irradiation at the appropriate position. Induced effects in the two oxides by PM-ICP would be related to the high concentration of hydrogen radicals in the plasma. (author)

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

Energy Technology Data Exchange (ETDEWEB)

Boue-Bigne, F

2000-08-20

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

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

International Nuclear Information System (INIS)

Boue-Bigne, F.

2000-01-01

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

Determination of osmium concentrations and (187)Os/(188)Os of crude oils and source rocks by coupling high-pressure, high-temperature digestion with sparging OsO(4) into a multicollector inductively coupled plasma mass spectrometer.

Science.gov (United States)

Sen, Indra S; Peucker-Ehrenbrink, Bernhard

2014-03-18

The (187)Os/(188)Os ratio that is based on the β(-)-decay of (187)Re to (187)Os (t1/2 = 41.6 billion years) is widely used to investigate petroleum system processes. Despite its broad applicability to studies of hydrocarbon deposits worldwide, a suitable matrix-matched reference material for Os analysis does not exist. In this study, a method that enables Os isotope measurement of crude oil with in-line Os separation and purification from the sample matrix is proposed. The method to analyze Os concentration and (187)Os/(187)Os involves sample digestion under high pressure and high temperature using a high pressure asher (HPA-S, Anton Paar), sparging of volatile osmium tetroxide from the sample solution, and measurements using multicollector inductively coupled plasma mass spectrometry (MC-ICPMS). This methods significantly reduced the total procedural time compared to conventional Carius tube digestion followed by Os separation and purification using solvent extraction, microdistillation and N-TIMS analysis. The method yields Os concentration (28 ± 4 pg g(-1)) and (187)Os/(188)Os (1.62 ± 0.15) of commercially available crude oil reference material NIST 8505 (1 S.D., n = 6). The reference material NIST 8505 is homogeneous with respect to Os concentration at a test portion size of 0.2 g. Therefore, (187)Os/(188)Os composition and Os concentration of NIST 8505 can serve as a matrix-matched reference material for Os analysis. Data quality was assessed by repeated measurements of the USGS shale reference material SCo-1 (sample matrix similar to petroleum source rock) and the widely used Liquid Os Standard solution (LOsSt). The within-laboratory reproducibility of (187)Os/(188)Os for a 5 pg of LOsSt solution, analyzed with this method over a period of 12 months was ∼1.4% (1 S.D., n = 26), respectively.

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

International Nuclear Information System (INIS)

Arslan, Zikri; Paulson, Anthony J.

2003-01-01

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

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

International Nuclear Information System (INIS)

Pitois, A.

2006-04-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Bruneau, F

1999-07-01

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

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

Science.gov (United States)

Jantzi, Sarah C; Almirall, José R

2014-01-01

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

Multicollector High Precision Resolution of Primordial Kr and Xe in Mantle CO2 Well Gases

Science.gov (United States)

Holland, G.; Ballentine, C.; Cassidy, M.

2008-12-01

Noble gas isotopes in magmatic CO2 well gases provide a unique insight into mantle volatile origin and dynamics [1-3]. Previous work has resolved mantle 20Ne/22Ne ratios consistent with a solar wind irradiated meteoritic source for mantle He and Ne [1]. This is distinct from Solar Wind values that might be expected if the primary mechanism of terrestrial mantle volatile acquisition was through the gravitational capture of solar nebula gases [see 4]. Within the CO2 well gases a primordial component has also been resolved in the non- radiogenic Xe isotopic composition [2,3]. Using multicollector mass spectrometry we have observed a 124Xe/130Xe excess of 1.85 percent over air plus/minus 0.17 percent for the least air contaminated samples. At this level of precision we are for the first time able to differentiate between a trapped meteoritic origin (average carbonaceous chondrite or Q Xe) rather than Solar Wind origin as the primordial Xe component. The well gases also contain Kr which, in the least air contaminated sample, have a correlated 86Kr/82Kr excess of 0.55 percent over air plus/minus 0.04 percent. Whilst mass dependent fractionation can theoretically produce correlated excesses in 124Xe-128Xe and 82Kr-86Kr isotopes, no fractionation from air is observed in 38Ar/36Ar [3] and the Kr excesses are in the opposite sense to that of Xe. From 136Xe excesses, Kr fission yield from Pu and U can be calculated and subtracted from the Kr isotopic signature. This fission-corrected signature is most reasonably explained as a primordial component. This is the first time that primordial Kr has ever been resolved in a terrestrial sample. The primordial Kr isotopic signature is distinct from Solar Wind Kr and is consistent with the primordial Kr also originating as a trapped component within meteorites. We are now able to demonstrate that both the light (He and Ne) and Heavy (Kr and Xe) noble gas origin in the terrestrial mantle is consistent with a trapped component during the

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

DEFF Research Database (Denmark)

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

2016-01-01

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

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

NARCIS (Netherlands)

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

2018-01-01

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

Imaging of metal bioaccumulation in Hay-scented fern (Dennstaedtia punctilobula) rhizomes growing on contaminated soils by laser ablation ICP-MS

International Nuclear Information System (INIS)

Koelmel, Jeremy; Amarasiriwardena, Dulasiri

2012-01-01

Understanding Pb removal from the translocation stream is vital to engineering Pb hyperaccumulation in above ground organs, which would enhance the economic feasibility of Pb phytoextraction technologies. We investigated Cu, Pb, Sb and Zn distributions in Hay-scented fern (Dennstaedtia punctilobula) rhizomes on shooting range soils by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), analyzing digested rhizomes, stems, and fronds using ICP-MS. Nutrients Cu and Zn concentrated in fronds while toxic elements Pb and Sb did not, showing potential Pb and Sb sequestration in the rhizome. Frond and rhizome concentration of Pb was 0.17 ± 0.10% and 0.32 ± 0.21% of dry biomass, respectively. The 208 Pb/ 13 C and 121 Sb/ 13 C determined by LA-ICP-MS increased from inner sclerotic cortex to the epidermis, while Pb concentrated in the starchy cortex only in contaminated sites. These results suggest that concentration dependent bioaccumulation in the rhizome outer cortex removes Pb from the vascular transport stream. - Highlights: ► Bioimaged Cu, Pb, Sb, Zn across fern rhizomes from shooting ranges using LA-ICP-MS. ► Pb levels were highest in the outer starchy cortex. ► Pb seemed to displace nutrients Cu and Zn in contaminated site rhizomes. ► [Pb] and [Sb] were correlated across organs suggesting similar transport factors. - Using LA-ICP-MS we determined elemental distributions in Hay-scented fern rhizomes including concentration dependent Pb sequestration patterns in the outer cortex.

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

Science.gov (United States)

Kamar, Veysi; Dağalp, Rukiye; Taştekin, Mustafa

2017-12-28

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

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

Science.gov (United States)

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

2017-05-01

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

Comparison between INAA and ICP-OES: analysis of Sudanese medicinal plants

International Nuclear Information System (INIS)

Sheikhaldin, Elsadig Abdelmoniem

2014-07-01

The aim of this study was to provide elemental concentrations in medicinal plants and mainly to compare the two different determination methods (INAA and ICP-OES after wet digestion) elemental analysis of 14 Sudanese medicinal plants was carried out using INAA and ICP-OES techniques. The selection of reported elements was done according to intersection of elements determined by both techniques. This intersecting element list contained Ca, K, Fe, Mn, Mg, Sr, Zn, Cu, Co, and Cr. INAA correlated well with ICP-OES measurements of the same plants as long as concentrations were sufficiently above LoQ. Correlation coefficients (R 2 ) in this case is close to 1. Generally, INAA results tended to be higher compared to ICP-OES. The performance and possible source of errors of both techniques was discussed also with respect to measurements of certified reference materials. INAA provided the advantage of having both, faster and non destructive sample preparation than ICP-OES. Therefore, INAA may be technique of choice for Ca, K, Zn, and Mg elements specifically when samples are needed for further investigations. Regarding the low concentrations e.g for Cr, Ni or Cu, ICP-OES is the superior technique over INAA due to the sufficiently low limits of determination and thus gaining more detectable results at low concentrations. (author)

Salpeterzuurdestructie en ICP-MS analyse van biotisch materiaal en voeding

NARCIS (Netherlands)

Velde-Koerts T van der; LAC

2000-01-01

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

Fundamental and applied measurements in ICP MS

International Nuclear Information System (INIS)

Carter, Julian Robert

2002-01-01

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

Isotope dilution ICP-MS with laser-assisted sample introduction for direct determination of sulfur in petroleum products

Energy Technology Data Exchange (ETDEWEB)

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

2005-08-01

Inductively coupled plasma isotope dilution mass spectrometry (ICP-IDMS) with direct laser-assisted introduction of isotope-diluted samples into the plasma, using a laser ablation system with high ablation rates, was developed for accurate sulfur determinations in different petroleum products such as 'sulfur-free' premium gasoline, diesel fuel, and heating oil. Two certified gas oil reference materials were analyzed for method validation. Two different {sup 34}S-enriched spike compounds, namely, elementary sulfur dissolved in xylene and dibenzothiophene in hexane, were synthesized and tested for their usefulness in this isotope dilution technique. The isotope-diluted sample was adsorbed on a filter-paper-like material, which was fixed in a special holder for irradiation by the laser beam. Under these conditions no time-dependent spike/analyte fractionation was only observed for the dibenzothiophene spike during the laser ablation process, which means that the measured {sup 34}S/{sup 32}S isotope ratio of the isotope-diluted sample remained constant - a necessary precondition for accurate results with the isotope dilution technique. A comparison of LA-ICP-IDMS results with the certified values of the gas oil reference materials and with results obtained from ICP-IDMS analyses with wet sample digestion demonstrated the accuracy of the new LA-ICP-IDMS method in the concentration range of 9.2 {mu}g g{sup -1} ('sulfur-free' premium gasoline) to 10.4 mg g{sup -1} (gas oil reference material BCR 107). The detection limit for sulfur by LA-ICP-IDMS is 0.04 {mu}g g{sup -1} and the analysis time is only about 10 min, which therefore also qualifies this method for accurate determinations of low sulfur contents in petroleum products on a routine level. (orig.)

Environmental application of XRF, ICP-AES and INAA on biological matrix

International Nuclear Information System (INIS)

Zararsiz, A.; Dogangun, A.; Tuncel, S.

2004-01-01

Full text: It is very important to determine trace quantities of metals in different matrices with high accuracy since the metals are used as markers for different sources in air pollution studies. In this study, the analytical capabilities of XRF, ICP-AES and INM techniques on a biological matrix namely lichens, which are widely used as bio monitoring organisms for the pollutants mapping in the atmosphere, were tested. Lichen samples were collected in Aegean Region of Turkey where pollution is an important issue. 9 elements were determined by XRF, 14 elements by ICP-AES and 13 elements by INM. Quality assurance was achieved using lichen SRM (IAEA-336) and Orchard leaves SRM (NIST- 1571). Produced data are subjected to statistical tests, like t-test, Q-test in order to determine the accuracy and precision of each technique. A recommendation list of the proper analytical technique is obtained for determination of each specific element considering analytical capabilities of ICP-AES, XRF and INM. As a result we can recommend that the first choice for Cd, Cu, Mg is ICP-AES, for In, K, Rb is INAA, for Br is XRF, if the concentrations are not close to the detection limit of XRF. For V, Cr, AI, Na, Fe ICP-AES and INM are both well, for Pb ICP-AES and XRF are both well, if the concentrations are not close to the detection limit of XRF, for Mn and Ca INM, XRF and ICP-AES are all give similar results for this type of biological matrix

Assessment of Hg Pollution Released from a WWII Submarine Wreck (U-864) by Hg Isotopic Analysis of Sediments and Cancer pagurus Tissues.

Science.gov (United States)

Rua-Ibarz, Ana; Bolea-Fernandez, Eduardo; Maage, Amund; Frantzen, Sylvia; Valdersnes, Stig; Vanhaecke, Frank

2016-10-04

Hg pollution released from the U-864 submarine sunk during WWII and potential introduction of that Hg into the marine food chain have been studied by a combination of quantitative Hg and MeHg determination and Hg isotopic analysis via cold vapor generation multicollector inductively coupled plasma-mass spectrometry (CVG-MC-ICP-MS) in sediment and Cancer pagurus samples. The sediment pollution could be unequivocally linked with the metallic Hg present in the wreck. Crabs were collected at the wreck location and 4 nmi north and south, and their brown and claw meat were analyzed separately. For brown meat, the δ 202 Hg values of the individuals from the wreck location were shifted toward the isotopic signature of the sediment and, thus, the submarine Hg. Such differences were not found for claw meat. The isotope ratio results suggest direct ingestion of metallic Hg by C. pagurus but do not offer any proof for any other introduction of the submarine Hg into the marine food chain.

Direct determination of platinum group elements and their distributions in geological and environmental samples at the ng g(-1) level using LA-ICP-IDMS.

Science.gov (United States)

Boulyga, Sergei F; Heumann, Klaus G

2005-10-01

Laser ablation inductively coupled plasma isotope dilution mass spectrometry (LA-ICP-IDMS) was applied to the direct and simultaneous determination of the platinum group elements (PGEs) Pt, Pd, Ru, and Ir in geological and environmental samples. A special laser ablation system with high ablation rates was used, along with sector field ICP-MS. Special attention was paid to deriving the distributions of PGEs in the pulverized samples. IDMS could not be applied to the (mono-isotopic) Rh, but the similar ablation behavior of Ru and Rh allowed Rh to be simultaneously determined via relative sensitivity coefficients. The laser ablation process produces hardly any oxide ions (which usually cause interference in PGE analysis with liquid sample injection), so the ICP-MS can be run in its low mass resolution but high-sensitivity mode. The detection limits obtained for the geological samples were 0.16 ng g(-1), 0.14 ng g(-1), 0.08 ng g(-1), 0.01 ng g(-1) and 0.06 ng g(-1) for Ru, Rh, Pd, Ir and Pt, respectively. LA-ICP-IDMS was applied to different geological reference materials (TDB-1, WGB-1, UMT-1, WMG-1, SARM-7) and the road dust reference material BCR-723, which are only certified for some of the PGEs. Comparisons with certified values as well as with indicative values from the literature demonstrated the validity of the LA-ICP-IDMS method. The PGE concentrations in subsamples of the road dust reference material correspond to a normal distribution, whereas the distributions in the geological reference materials TDB-1, WGB-1, UMT-1, WMG-1, and SARM-7 are more complex. For example, in the case of Ru, a logarithmic normal distribution best fits the analyzed concentrations in TDB-1 subsamples, whereas a pronounced nugget effect was found for Pt in most geological samples.

Sodium Bicarbonate for Control of ICP: A Systematic Review.

Science.gov (United States)

Zeiler, Frederick A; Sader, Nicholas; West, Michael; Gillman, Lawrence M

2018-01-01

Our goal was to perform a systematic review of the literature on the use of intravenous sodium bicarbonate for intracranial pressure (ICP) reduction in patients with neurologic illness. Data sources: articles from MEDLINE, BIOSIS, EMBASE, Global Health, Scopus, Cochrane Library, the International Clinical Trials Registry Platform (inception to April 2015), reference lists of relevant articles, and gray literature were searched. 2 reviewers independently extracted data including population characteristics and treatment characteristics. The strength of evidence was adjudicated using both the Oxford and Grading of Recommendation Assessment Development and Education methodology. Our search strategy produced a total 559 citations. Three original articles were included in the review. There were 2 prospective studies, 1 randomized control trial and 1 single arm, and 1 retrospective case report.Across all studies there were a total of 19 patients studied, with 31 episodes of elevated ICP being treated. Twenty-one of those episodes were treated with sodium bicarbonate infusion, with the remaining 10 treated with hypertonic saline in a control model. All elevated ICP episodes treated with sodium bicarbonate solution demonstrated a significant drop in ICP, without an elevation of serum partial pressure of carbon dioxide. No significant complications were described. There currently exists Oxford level 4, Grading of Recommendation Assessment Development and Education D evidence to support an ICP reduction effect with intravenous sodium bicarbonate in TBI. No comments on its impact in other neuropathologic states, or on patient outcomes, can be made at this time.

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)

Metal ion transport quantified by ICP-MS in intact cells

Science.gov (United States)

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

2016-01-01

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

Characterisation of an ion source on the Helix MC Plus noble gas mass spectrometer - pressure dependent mass discrimination

Science.gov (United States)

Zhang, X.

2017-12-01

Characterisation of an ion source on the Helix MC Plusnoble gas mass spectrometer - pressure dependent mass discrimination Xiaodong Zhang* dong.zhang@anu.edu.au Masahiko Honda Masahiko.honda@anu.edu.au Research School of Earth Sciences, The Australian National University, Canberra, Australia To obtain reliable measurements of noble gas elemental and isotopic abundances in a geological sample it is essential that the mass discrimination (instrument-induced isotope fractionation) of the mass spectrometer remain constant over the working range of noble gas partial pressures. It is known, however, that there are pressure-dependent variations in sensitivity and mass discrimination in conventional noble gas mass spectrometers [1, 2, 3]. In this study, we discuss a practical approach to ensuring that the pressure effect in the Helix MC Plus high resolution, multi-collector noble gas mass spectrometer is minimised. The isotopic composition of atmospheric Ar was measured under a range of operating conditions to test the effects of different parameters on Ar mass discrimination. It was found that the optimised ion source conditions for pressure independent mass discrimination for Ar were different from those for maximised Ar sensitivity. The optimisation can be achieved by mainly adjusting the repeller voltage. It is likely that different ion source settings will be required to minimise pressure-dependent mass discrimination for different noble gases. A recommended procedure for tuning an ion source to reduce pressure dependent mass discrimination will be presented. References: Honda M., et al., Geochim. Cosmochim. Acta, 57, 859 -874, 1993. Burnard P. G., and Farley K. A., Geochemistry Geophysics Geosystems, Volume 1, 2000GC00038, 2000. Mabry J., et al., Journal of Analytical Atomic Spectrometry, 27, 1012 - 1017, 2012.

Metal RIE 2: Unaxis SHUTTLELINE ICP

Data.gov (United States)

Federal Laboratory Consortium — Description:CORAL Name: Unaxis ICP EtcherChlorine-based system utilizing Boron Trichloride and Chlorine to etch metals and III-V group materials on planar substrates...

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-01-28

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

Air pollution studies using PIXE and ICP methods

International Nuclear Information System (INIS)

Stihi, Claudia; Bancuta, Anca; Popescu, I V; Virgolici, M; Cimpoca, V; Gugiu, M; Vlaicu, Gh

2006-01-01

In the present work the moss biomonitoring technique and the combination of two analytical techniques - Particle Induced X-ray Emission (PIXE) and Inductively Coupled Plasma (ICP) - were applied for assessing environmental situation from the point of view of air polluting along the transect from north to south of the Dambovita County. PIXE analysis at the Tandem Accelerator FN-8 of the National Institute of Nuclear Physics - Horia Hulubei of Magurele, Bucharest, allowed determination of P, S, Cl, K, Ca, Mn, Fe, Ni, Cu, Zn, As, Sr, Cd and Pb in samples. ICP analyses were made using a Baird ICP2070 - Sequential Plasma Spectrometer in Targoviste and we determined in samples the concentration of Li, B, Na, and Mg together with Cd and Pb. The obtained results will permit to determine the regional extent of heavy metals and toxic elements atmospheric pollution and to identify specially affected areas and local sources of

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

International Nuclear Information System (INIS)

Kallio, E.

1994-01-01

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

Application of ICP-MS in Environmental Sampling Analysis for Safeguards

International Nuclear Information System (INIS)

Eko Pudjadi; Petrus Zacharias; Budi Prayitno

2004-01-01

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

Some practical applications of an ICP-MS instrument

International Nuclear Information System (INIS)

Meddings, B.; Ng, R.

1987-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-01-01

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

Direct determination of platinum group elements and their distributions in geological and environmental samples at the ng g{sup -1} level using LA-ICP-IDMS

Energy Technology Data Exchange (ETDEWEB)

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

2005-10-01

Laser ablation inductively coupled plasma isotope dilution mass spectrometry (LA-ICP-IDMS) was applied to the direct and simultaneous determination of the platinum group elements (PGEs) Pt, Pd, Ru, and Ir in geological and environmental samples. A special laser ablation system with high ablation rates was used, along with sector field ICP-MS. Special attention was paid to deriving the distributions of PGEs in the pulverized samples. IDMS could not be applied to the (mono-isotopic) Rh, but the similar ablation behavior of Ru and Rh allowed Rh to be simultaneously determined via relative sensitivity coefficients. The laser ablation process produces hardly any oxide ions (which usually cause interference in PGE analysis with liquid sample injection), so the ICP-MS can be run in its low mass resolution but high-sensitivity mode. The detection limits obtained for the geological samples were 0.16 ng g{sup -1}, 0.14 ng g{sup -1}, 0.08 ng g{sup -1}, 0.01 ng g{sup -1} and 0.06 ng g{sup -1} for Ru, Rh, Pd, Ir and Pt, respectively. LA-ICP-IDMS was applied to different geological reference materials (TDB-1, WGB-1, UMT-1, WMG-1, SARM-7) and the road dust reference material BCR-723, which are only certified for some of the PGEs. Comparisons with certified values as well as with indicative values from the literature demonstrated the validity of the LA-ICP-IDMS method. The PGE concentrations in subsamples of the road dust reference material correspond to a normal distribution, whereas the distributions in the geological reference materials TDB-1, WGB-1, UMT-1, WMG-1, and SARM-7 are more complex. For example, in the case of Ru, a logarithmic normal distribution best fits the analyzed concentrations in TDB-1 subsamples, whereas a pronounced nugget effect was found for Pt in most geological samples. (orig.)

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

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

2017-05-01

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

Applications of ICP-MS in marine analytical chemistry

Energy Technology Data Exchange (ETDEWEB)

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

1990-07-01

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

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

Science.gov (United States)

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

2017-01-01

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

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

Science.gov (United States)

Ko, Jung Aa; Lim, H B

2016-09-28

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

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

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

2017-05-05

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

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

Science.gov (United States)

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

2017-09-25

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

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

Science.gov (United States)

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

2017-04-01

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

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

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Emmanuelle Cordeau

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

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

Science.gov (United States)

2012-01-01

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

Reassessment of 239Pu on planchets from human urine samples at ultra-trace levels using Aridus-ICP-SFMS and AMS

International Nuclear Information System (INIS)

Hernandez-Mendoza, H.; Chamizo, E.; Delgado, A.; Garcia-Leon, M.; Yllera, A.

2012-01-01

New analytical methods developed at the facilities here, based on two ultra-sensitive mass spectrometry (MS) techniques, inductively coupled plasma sector field mass spectrometer with a desolvator system (Aridus-ICP-SFMS) and accelerator MS (AMS), have been applied in this work for the reassessment of 239 Pu in alpha spectrometry (AS) planchets corresponding to spiked human urine samples. The obtained 239 Pu minimum detectable activities (MDAs) values by Aridus-ICP-SFMS and AMS were 3 fg (∼6.92 μBq) and 0.4 fg (∼0.92 μBq), respectively, per sample, which are much better than those attainable by AS [50 fg (∼115.3 μBq) of 239 Pu per sample, approximately]. Therefore, it is demonstrated that the MS techniques employed in this work are very powerful tools for internal dosimetry studies in human urine samples, giving excellent results when the reassessment of AS planchets is needed (samples with a Pu concentration below or at the MDA levels measurable by AS). This work is the continuation of an article published in J. Anal. At. Spectrom. 25 (1410-1415) 2010. (authors)

The baseline pressure of intracranial pressure (ICP) sensors can be altered by electrostatic discharges.

Science.gov (United States)

Eide, Per K; Bakken, André

2011-08-22

The monitoring of intracranial pressure (ICP) has a crucial role in the surveillance of patients with brain injury. During long-term monitoring of ICP, we have seen spontaneous shifts in baseline pressure (ICP sensor zero point), which are of technical and not physiological origin. The aim of the present study was to explore whether or not baseline pressures of ICP sensors can be affected by electrostatics discharges (ESD's), when ESD's are delivered at clinically relevant magnitudes. We performed bench-testing of a set of commercial ICP sensors. In our experimental setup, the ICP sensor was placed in a container with 0.9% NaCl solution. A test person was charged 0.5-10 kV, and then delivered ESD's to the sensor by touching a metal rod that was located in the container. The continuous pressure signals were recorded continuously before/after the ESD's, and the pressure readings were stored digitally using a computerized system A total of 57 sensors were tested, including 25 Codman ICP sensors and 32 Raumedic sensors. When charging the test person in the range 0.5-10 kV, typically ESD's in the range 0.5-5 kV peak pulse were delivered to the ICP sensor. Alterations in baseline pressure ≥ 2 mmHg was seen in 24 of 25 (96%) Codman sensors and in 17 of 32 (53%) Raumedic sensors. Lasting changes in baseline pressure > 10 mmHg that in the clinical setting would affect patient management, were seen frequently for both sensor types. The changes in baseline pressure were either characterized by sudden shifts or gradual drifts in baseline pressure. The baseline pressures of commercial solid ICP sensors can be altered by ESD's at discharge magnitudes that are clinically relevant. Shifts in baseline pressure change the ICP levels visualised to the physician on the monitor screen, and thereby reveal wrong ICP values, which likely represent a severe risk to the patient.

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

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

Science.gov (United States)

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

2018-05-09

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

Application of CE-ICP-MS and CE-ESI-MS/MS for identification of Zn-binding ligands in Goji berries extracts.

Science.gov (United States)

Ruzik, Lena; Kwiatkowski, Piotr

2018-06-01

The identification of groups of ligands binding metals is a crucial issue for the better understanding of their bioaccessibility. In the current study, we have intended an approach for identification of Zn-binding ligands based on using capillary electrophoresis combined with inductively coupled plasma mass spectrometry (CE-ICP-MS) and tandem electrospray ionization mass spectrometry (CE-ESI-MS/MS). The approach, which featured the use of the coupling of capillary electrophoresis with inductively coupled plasma mass spectrometry allows to separate and observe zinc ions present in complexes with respect to their size and charge and to identify nine compounds with zinc isotopic profile. CE-ICP-MS provides us with information about presence of zinc species and elemental information about zinc distribution. CE-ESI-MS/MS provide us with information about the most favorable Zn binding ligands: amino acids, flavonols, stilbenoids, fenolic acids and carotenoids. The presented work is the continuation of previous studies based on using LC-ESI-MS/MS, though, now we presented a new solutions with the possibility of changing detectors without changing the separation techniques, what is important without re-optimizing the method. The new presented method allows to identify the zinc-binding ligands in shorter time. Copyright © 2018 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

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

2018-01-01

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

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

Science.gov (United States)

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

2004-10-01

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

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

Science.gov (United States)

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

2014-08-01

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

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.

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)

Tracing lead pollution sources in abandoned mine areas using stable Pb isotope ratios.

Science.gov (United States)

Yoo, Eun-Jin; Lee, Jung-A; Park, Jae-Seon; Lee, Khanghyun; Lee, Won-Seok; Han, Jin-Seok; Choi, Jong-Woo

2014-02-01

This study focused on Pb isotope ratios of sediments in areas around an abandoned mine to determine if the ratios can be used as a source tracer. For pretreatment, sediment samples were dissolved with mixed acids, and a multi-collector inductively coupled plasma mass spectrometer (MC-ICP-MS, Nu plasma II) was used to investigate the Pb isotopic composition of the samples. The measured isotope ratios were then corrected for instrumental mass fractionation by measuring the (203)Tl/(205)Tl ratio. Repeated measurements with the NIST SRM 981 reference material showed that the precision of all ratios was below 104 ppm (±2σ) for 50 ng/g. The isotope ratios ((207)Pb/(206)Pb) found were 0.85073 ± 0.0004~0.85373 ± 0.0003 for the main stream, while they were 0.83736 ± 0.0010 for the tributary and 0.84393 ± 0.0002 for the confluence. A binary mixing equation for isotope ratios showed that the contributions of mine lead to neighboring areas were up to 60%. Therefore, Pb isotope ratios can be a good source tracer for areas around abandoned mines.

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

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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.

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

Czech Academy of Sciences Publication Activity Database

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

2013-01-01

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

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

Science.gov (United States)

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

2017-11-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2011-07-01

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

Species and life-history affects the utility of otolith chemical composition to determine natal stream-of-origin in Pacific salmon

Science.gov (United States)

Zimmerman, Christian E.; Swanson, Heidi K.; Volk, Eric C.; Kent, Adam J.R.

2013-01-01

To test the utility of otolith chemical composition as a tool for determining the natal stream of origin for salmon, we examined water chemistry and otoliths of juvenile and adult Chum Salmon Oncorhynchus keta and Coho Salmon O. kisutch from three watersheds (five rivers) in the Norton Sound region of Alaska. The two species are characterized by different life histories: Coho Salmon rear in freshwater for up to 3 years, whereas Chum Salmon emigrate from freshwater shortly after emergence. We used laser ablation (LA) inductively coupled plasma (ICP) mass spectrometry (MS) to quantify element: Ca ratios for Mg, Mn, Zn, Sr, and Ba, and we used multicollector LA-ICP-MS to determine 87Sr:86Sr ratios in otolith regions corresponding to the period of freshwater residence. Significant differences existed in both water and otolith elemental composition, suggesting that otolith composition could be used to discriminate the natal origin of Coho Salmon and Chum Salmon but only when 87Sr:86Sr ratios were included in the discriminant function analyses. The best discriminant model included 87Sr:86Sr ratios, and without 87Sr:86Sr ratios it was difficult to discriminate among watersheds and rivers. Classification accuracy was 80% for Coho Salmon and 68% for Chum Salmon, indicating that this method does not provide sufficient sensitivity to estimate straying rates of Pacific salmon at the scale we studied.

Development of pre-concentration procedure for the determination of Hg isotope ratios in seawater samples.

Science.gov (United States)

Štrok, Marko; Hintelmann, Holger; Dimock, Brian

2014-12-03

Hg concentrations in seawater are usually too low to allow direct (without pre-concentration and removal of salt matrix) measurement of its isotope ratios with multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS). Therefore, a new method for the pre-concentration of Hg from large volumes of seawater was developed. The final method allows for relatively fast (about 2.5Lh(-1)) and quantitative pre-concentration of Hg from seawater samples with an average Hg recovery of 98±6%. Using this newly developed method we determined Hg isotope ratios in seawater. Reference seawater samples were compared to samples potentially impacted by anthropogenic activity. The results show negative mass dependent fractionation relative to the NIST 3133 Hg standard with δ(202)Hg values in the range from -0.50‰ to -1.50‰. In addition, positive mass independent fractionation of (200)Hg was observed for samples from reference sites, while impacted sites did not show significant Δ(200)Hg values. Although the influence of the impacted sediments is limited to the seawater and particulate matter in very close proximity to the sediment, this observation may raise the possibility of using Δ(200)Hg to distinguish between samples from impacted and reference sites. Copyright © 2014 Elsevier B.V. All rights reserved.

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

Digital Repository Service at National Institute of Oceanography (India)

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

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

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

Online elemental analysis of process gases with ICP-OES: A case study on waste wood combustion

International Nuclear Information System (INIS)

Wellinger, Marco; Wochele, Joerg; Biollaz, Serge M.A.; Ludwig, Christian

2012-01-01

Highlights: ► Simultaneous measurements of 23 elements in process gases of a waste wood combustor. ► Mobile ICP spectrometer allows measurements of high quality at industrial plants. ► Continuous online measurements with high temporal resolution. ► Linear correlations among element concentrations in the raw flue gas were detected. ► Novel sampling and calibration methods for ICP-OES analysis of process gases. - Abstract: A mobile sampling and measurement system for the analysis of gaseous and liquid samples in the field was developed. An inductively coupled plasma optical emission spectrometer (ICP-OES), which is built into a van, was used as detector. The analytical system was calibrated with liquid and/or gaseous standards. It was shown that identical mass flows of either gaseous or liquid standards resulted in identical ICP-OES signal intensities. In a field measurement campaign trace and minor elements in the raw flue gas of a waste wood combustor were monitored. Sampling was performed with a highly transport efficient liquid quench system, which allowed to observe temporal variations in the elemental process gas composition. After a change in feedstock an immediate change of the element concentrations in the flue gas was detected. A comparison of the average element concentrations during the combustion of the two feedstocks showed a high reproducibility for matrix elements that are expected to be present in similar concentrations. On the other hand elements that showed strong differences in their concentration in the feedstock were also represented by a higher concentration in the flue gas. Following the temporal variations of different elements revealed strong correlations between a number of elements, such as chlorine with sodium, potassium and zinc, as well as arsenic with lead, and calcium with strontium.

Analysis of nanoparticles using the ICAP Q ICP-MS

DEFF Research Database (Denmark)

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

2014-01-01

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

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

International Nuclear Information System (INIS)

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

1998-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Conde, E.; Navarro, N.; Fernández, M.

2015-07-01

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

Early Implementation of THAM for ICP Control: Therapeutic Hypothermia Avoidance and Reduction in Hypertonics/Hyperosmotics

Directory of Open Access Journals (Sweden)

F. A. Zeiler

2014-01-01

Full Text Available Background. Tromethamine (THAM has been demonstrated to reduce intracranial pressure (ICP. Early consideration for THAM may reduce the need for other measures for ICP control. Objective. To describe 4 cases of early THAM therapy for ICP control and highlight the potential to avoid TH and paralytics and achieve reduction in sedation and hypertonic/hyperosmotic agent requirements. Methods. We reviewed the charts of 4 patients treated with early THAM for ICP control. Results. We identified 2 patients with aneurysmal subarachnoid hemorrhage (SAH and 2 with traumatic brain injury (TBI receiving early THAM for ICP control. The mean time to initiation of THAM therapy was 1.8 days, with a mean duration of 5.3 days. In all patients, after 6 to 12 hours of THAM administration, ICP stability was achieved, with reduction in requirements for hypertonic saline and hyperosmotic agents. There was a relative reduction in mean hourly hypertonic saline requirements of 89.1%, 96.1%, 82.4%, and 97.0% for cases 1, 2, 3, and 4, respectively, comparing pre- to post-THAM administration. Mannitol, therapeutic hypothermia, and paralytics were avoided in all patients. Conclusions. Early administration of THAM for ICP control could potentially lead to the avoidance of other ICP directed therapies. Prospective studies of early THAM administration are warranted.

Fundamental and applied measurements in ICP MS

Energy Technology Data Exchange (ETDEWEB)

Carter, Julian Robert

2002-07-01

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

Quality and Safety of Home ICP Monitoring Compared with In-Hospital Monitoring

DEFF Research Database (Denmark)

Andresen, Morten; Juhler, Marianne; Munch, Tina Nørgaard

2012-01-01

Introduction: Intracranial pressure (ICP) monitoring is usually conducted in-hospital using stationary devices. Modern mobile ICP monitoring systems present new monitoring possibilities more closely following the patients' daily life. We reviewed patient safety, quality of technical data...

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

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

Science.gov (United States)

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

2015-04-01

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

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.

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.

Elemental analysis of coal by tandem laser induced breakdown spectroscopy and laser ablation inductively coupled plasma time of flight mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Dong, Meirong [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China); Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Oropeza, Dayana [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Chirinos, José [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Escuela de Química, Facultad de Ciencias, Universidad Central de Venezuela, Caracas 1041a (Venezuela, Bolivarian Republic of); González, Jhanis J. [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Lu, Jidong [School of Electric Power, South China University of Technology, Guangzhou, Guangdong 510640 (China); Mao, Xianglei [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States); Russo, Richard E., E-mail: RERusso@lbl.gov [Lawrence Berkeley National Laboratory, University of California, Berkeley, CA 94720 (United States)

2015-07-01

The capabilities and analytical benefits of combined LIBS and LA-ICP-MS were evaluated for the analysis of coal samples. The ablation system consisted of a Nd:YAG laser operated 213 nm. A Czerny-turner spectrograph with ICCD detector and time-of-flight based mass spectrometer were utilized for LIBS and ICP-MS detection, respectively. This tandem approach allows simultaneous determination of major and minor elements (C, Si, Ca, Al, Mg), and trace elements (V, Ba, Pb, U, etc.) in the coal samples. The research focused on calibration strategies, specifically the use of univariate and multivariate data analysis on analytical performance. Partial least square regression (PLSR) was shown to minimize and compensate for matrix effects in the emission and mass spectra improving quantitative analysis by LIBS and LA-ICP-MS, respectively. The correlation between measurements from these two techniques demonstrated that mass spectral data combined with LIBS emission measurements by PLSR improved the accuracy and precision for quantitative analysis of trace elements in coal. - Highlights: • Tandem LIBS LA-ICP-MS • Simultaneous determination of major and minor elements and trace elements in the coal samples. • Extended Dynamic Range • Correlation between LIBS with LA-ICP-MS demonstrated improved the accuracy and precision for quantitative analysis of coal.

Elemental analysis of coal by tandem laser induced breakdown spectroscopy and laser ablation inductively coupled plasma time of flight mass spectrometry

International Nuclear Information System (INIS)

Dong, Meirong; Oropeza, Dayana; Chirinos, José; González, Jhanis J.; Lu, Jidong; Mao, Xianglei; Russo, Richard E.

2015-01-01

The capabilities and analytical benefits of combined LIBS and LA-ICP-MS were evaluated for the analysis of coal samples. The ablation system consisted of a Nd:YAG laser operated 213 nm. A Czerny-turner spectrograph with ICCD detector and time-of-flight based mass spectrometer were utilized for LIBS and ICP-MS detection, respectively. This tandem approach allows simultaneous determination of major and minor elements (C, Si, Ca, Al, Mg), and trace elements (V, Ba, Pb, U, etc.) in the coal samples. The research focused on calibration strategies, specifically the use of univariate and multivariate data analysis on analytical performance. Partial least square regression (PLSR) was shown to minimize and compensate for matrix effects in the emission and mass spectra improving quantitative analysis by LIBS and LA-ICP-MS, respectively. The correlation between measurements from these two techniques demonstrated that mass spectral data combined with LIBS emission measurements by PLSR improved the accuracy and precision for quantitative analysis of trace elements in coal. - Highlights: • Tandem LIBS LA-ICP-MS • Simultaneous determination of major and minor elements and trace elements in the coal samples. • Extended Dynamic Range • Correlation between LIBS with LA-ICP-MS demonstrated improved the accuracy and precision for quantitative analysis of coal

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

International Nuclear Information System (INIS)

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

2007-01-01

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

Identification of Marchfeld asparagus using Sr isotope ratio measurements by MC-ICP-MS.

Science.gov (United States)

Swoboda, S; Brunner, M; Boulyga, S F; Galler, P; Horacek, M; Prohaska, T

2008-01-01

This work focuses on testing and application of Sr isotope signatures for the fast and reliable authentication and traceability of Asparagus officinalis originating from Marchfeld, Austria, using multicollector inductively coupled plasma mass spectrometry after optimised Rb/Sr separation. The major sample pool comprises freeze-dried and microwave-digested asparagus samples from Hungary and Slovakia which are compared with Austrian asparagus originating from the Marchfeld region, which is a protected geographical indication. Additional samples from Peru, The Netherlands and Germany were limited in number and allowed therefore only restricted statistical evaluation. Asparagus samples from Marchfeld were harvested within two subsequent years in order to investigate the annual variation. The results show that the Sr isotope ratio is consistent within these 2 years of investigation. Moreover, the Sr isotope ratio of total Sr in soil was found to be significantly higher than in an NH4NO3 extract, reflecting the mobile (bioavailable) phase. The isotope composition in the latter extract corresponds well to the range found in the asparagus samples in Marchfeld, even though the concentration of Sr in asparagus shows no direct correlation to the concentration of Sr in the mobile phase of the soil. The major question was whether the 'Marchfelder Spargel' can be distinguished from samples from the neighbouring countries of Hungary and Slovakia. According to our findings, they can be clearly (100%) singled out from the Hungarian samples and can be distinguished from the Slovakian asparagus samples with a probability of more than 80%.

Direct determination of uranium in human urine by Icp-SFMS; Determinacion directa de uranio en orina humana por ICP-SFMS

Energy Technology Data Exchange (ETDEWEB)

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

2013-10-15

The success of the measurement and the evaluation of the internal exposure are highly dependent of the effective capacities for the radiation measurement in biological samples (mainly urine and the feces). Usually, during the samples bioassay of human urine, a pre-concentration and purification of the radionuclides is carried out previously to the quantitative analysis. These stages, as the analysis time are the main source of uncertainty in the measurement process. In the uranium case, this is not necessary when are used mass spectrometry techniques, in particular, Mass Spectrometry of Magnetic Sector with Inductively Coupled Plasma (Icp-SFMS). This work presents the results obtained for the uranium analysis in samples of human urine during the participation in the inter-comparison exercises of the Association pour la Promotion de Controle de Qualite des Analyses de Biologie Medicale en Radiotoxicologie (PROCORAD) in the period 2010 and 2011. The analyses were realized directly in the diluted urine samples (dilution factor 1:20) in 5% of HNO{sub 3}. The obtained results, were normalized to the total urine sample (V = 0.5 L), these values coincide with the waited reference values of uranium in the urine sample. Additionally, were calculated the detection limits of {sup 235}U= 0.049 x 10{sup -3} μg L{sup -1} and {sup 238}U= 7.37 x 10{sup -3} μg L{sup -1}. (author)

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)

Inductively coupled plasma- mass spectrometry. Chapter 13

International Nuclear Information System (INIS)

Mahalingam, T.R.

1997-01-01

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

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

Science.gov (United States)

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

2011-12-07

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

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

Science.gov (United States)

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

1996-06-01

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

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

International Nuclear Information System (INIS)

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

1997-01-01

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

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

C-terminal region of herpes simplex virus ICP8 protein needed for intranuclear localization

International Nuclear Information System (INIS)

Taylor, Travis J; Knipe, David M.

2003-01-01

The herpes simplex virus single-stranded DNA-binding protein, ICP8, localizes initially to structures in the nucleus called prereplicative sites. As replication proceeds, these sites mature into large globular structures called replication compartments. The details of what signals or proteins are involved in the redistribution of viral and cellular proteins within the nucleus between prereplicative sites and replication compartments are poorly understood; however, we showed previously that the dominant-negative d105 ICP8 does not localize to prereplicative sites and prevents the localization of other viral proteins to prereplicative sites (J. Virol. 74 (2000) 10122). Within the residues deleted in d105 (1083 to 1168), we identified a region between amino acid residues 1080 and 1135 that was predicted by computer models to contain two α-helices, one with considerable amphipathic nature. We used site-specific and random mutagenesis techniques to identify residues or structures within this region that are required for proper ICP8 localization within the nucleus. Proline substitutions in the predicted helix generated ICP8 molecules that did not localize to prereplicative sites and acted as dominant-negative inhibitors. Other substitutions that altered the charged residues in the predicted α-helix to alanine or leucine residues had little or no effect on ICP8 intranuclear localization. The predicted α-helix was dispensable for the interaction of ICP8 with the U L 9 origin-binding protein. We propose that this C-terminal α-helix is required for localization of ICP8 to prereplicative sites by binding viral or cellular factors that target or retain ICP8 at specific intranuclear sites

Simultaneous measurement of 239Pu, 240Pu, 241Pu, and 242Pu by high resolution inductively coupled plasma mass spectrometer (HR ICP-MS) in marine sediments

International Nuclear Information System (INIS)

Bruneau, F.

1999-01-01

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

Registration of TLS and MLS Point Cloud Combining Genetic Algorithm with ICP

Directory of Open Access Journals (Sweden)

YAN Li

2018-04-01

Full Text Available Large scene point cloud can be quickly acquired by mobile laser scanning (MLS technology,which needs to be supplemented by terrestrial laser scanning (TLS point cloud because of limited field of view and occlusion.MLS and TLS point cloud are located in geodetic coordinate system and local coordinate system respectively.This paper proposes an automatic registration method combined genetic algorithm (GA and iterative closed point ICP to achieve a uniform coordinate reference frame.The local optimizer is utilized in ICP.The efficiency of ICP is higher than that of GA registration,but it depends on a initial solution.GA is a global optimizer,but it's inefficient.The combining strategy is that ICP is enabled to complete the registration when the GA tends to local search.The rough position measured by a built-in GPS of a terrestrial laser scanner is used in the GA registration to limit its optimizing search space.To improve the GA registration accuracy,a maximum registration model called normalized sum of matching scores (NSMS is presented.The results for measured data show that the NSMS model is effective,the root mean square error (RMSE of GA registration is 1~5 cm and the registration efficiency can be improved by about 50% combining GA with ICP.

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.

Characterization of Elements Regulating the Nuclear-to-Cytoplasmic Translocation of ICP0 in Late Herpes Simplex Virus 1 Infection.

Science.gov (United States)

Samrat, Subodh Kumar; Ha, Binh L; Zheng, Yi; Gu, Haidong

2018-01-15

Infected cell protein 0 (ICP0) of herpes simplex virus 1 (HSV-1) is an immediate early protein containing a RING-type E3 ubiquitin ligase. It targets several host factors for proteasomal degradation and subsequently activates viral expression. ICP0 has a nuclear localization sequence and functions in the nucleus early during infection. However, later in infection, ICP0 is found solely in the cytoplasm. The molecular mechanism and biological function of the ICP0 nuclear-to-cytoplasmic translocation are not well understood. In this study, we sought to characterize elements important for this translocation. We found that (i) in human embryonic lung fibroblast (HEL) cells, ICP0 C-terminal residues 741 to 775 were necessary but not sufficient for the nuclear-to-cytoplasmic translocation; (ii) the loss of ICP0 E3 ubiquitin ligase activity, which led to defective viral replication in nonpermissive cells, also caused mutant ICP0 to be retained in the nucleus of HEL cells; (iii) in permissive U2OS cells, however, ICP0 lacking E3 ligase activity was translocated to the cytoplasm at a pace faster than that of wild-type ICP0, suggesting that nuclear retention of ICP0 occurs in an ICP0 E3 ligase-dependent manner; and (iv) the ICP0 C terminus and late viral proteins cooperate in order to overcome nuclear retention and stimulate ICP0 cytoplasmic translocation. Taken together, less ICP0 nuclear retention may contribute to the permissiveness of U2OS cells to HSV-1 in the absence of functional ICP0. IMPORTANCE A distinct characteristic for eukaryotes is the compartmentalization of cell metabolic pathways, which allows greater efficiency and specificity of cellular functions. ICP0 of HSV-1 is a multifunctional viral protein that travels through different compartments as infection progresses. Its main regulatory functions are carried out in the nucleus, but it is translocated to the cytoplasm late during HSV-1 infection. To understand the biological significance of cytoplasmic ICP0 in

Comparative evaluation of ICP sample introduction systems to be used in the metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS.

Science.gov (United States)

Klencsár, Balázs; Sánchez, Carlos; Balcaen, Lieve; Todolí, José; Lynen, Frederic; Vanhaecke, Frank

2018-05-10

A systematic evaluation of four different ICP sample introduction systems to be used in the context of metabolite profiling of chlorine-containing pharmaceuticals via HPLC-ICP-MS was carried out using diclofenac and its major metabolite, 4'-hydroxy-diclofenac, as model compounds. The strict requirements for GMP validation of chromatographic methods in the pharmaceutical industry were adhered to in this context. The final aim of this investigation is an extension of the applicability and validatability of HPLC-ICP-MS in the field of pharmaceutical R&D. Five different gradient programmes were tested while the baseline peak width (w b ), peak capacity (P), USP tailing factor (A s ) and USP signal-to-noise ratio (USP S/N) were determined as major indicators of the chromatographic performance and the values obtained were compared to the corresponding FDA recommendations (if applicable). Four different ICP-MS sample introductions systems were investigated involving two units typically working at higher flow rates (∼1.0 mL min -1 ) and another two systems working at lower flow rates (∼0.1 mL min -1 ). Optimal conditions with potential for applicability under GMP conditions were found at a mobile phase flow rate of 1.0 mL min -1 by using a pneumatic micro-flow LC nebulizer mounted onto a Peltier-cooled cyclonic spray chamber cooled to -1 °C for sample introduction. Under these conditions, HPLC-ICP-MS provided a chromatographic performance similar to that of HPLC with UV detection. The peak shape (USP tailing factor = 1.1-1.4) was significantly improved compared to that obtained with the Peltier-cooled Scott-type spray chamber. Two alternative sample introduction systems - a POINT ® and a High-Temperature Torch-Integrated Sample Introduction System (hTISIS) - were also tested at a flow rate of 0.1 mL min -1 using a chromatographic column with 1.0 mm ID. Although these systems allowed the peak shape to be improved compared to that obtained with

Determination of organic phosphorous in oil production waters by ICP-AES and ICP-MS after preconcentration on silica immobilized C{sub 18}; Determinacao de fosforo organico em aguas de producao petrolifera por ICP-AES e ICP-MS apos pre-concentracao em coluna de silica C{sub 18}

Energy Technology Data Exchange (ETDEWEB)

Rocha, Anderson Araujo; Miekeley, Norbert; Silveira, Carmem Lucia Porto da [Pontificia Univ. Catolica do Rio de Janeiro, RJ (Brazil). Dept. de Quimica; Bezerra, Maria Carmem Moreira [PETROBRAS, Rio de Janeiro, RJ (Brazil). Centro de Pesquisas

1998-10-01

Results on the optimization analytical methods for the determination of phosphorous in phosphino-poly carboxylate (PPCA), used frequently as scale inhibitor during oil production, by ICP-AES and ICP-MS are presented. Due to the complex matrix of production waters (brines) and their high concentration in inorganic phosphorus, the separation of organic phosphorus prior to its determination in necessary. In this work, mini columns of silica immobilized C{sub 18} were used. Optimization of the separation step resulted in the following working conditions: (1) pre washing of the column with methanol (80% v/v); (2) use of a flow rate of 5 m L/min and 10 m L/min, respectively, for the preconditioning step and for percolation of the water sample; (3) final elution of organic phosphorus with 7 m L of buffer of H{sub 3} BO{sub 3}/Na OH (0.05 M, p H 9) with a flow rate of 1 m L/min. Sample detection limits (3{sigma}) for different combinations of nebulizers and spectrometric methods, based on 10 m L water aliquots, are: ICP-AES-Cross flow (47 mg/L) and Ultrasonic (18 {mu}g/L); ICP-M S-Cross flow (1.2 {mu}g/L) and Ultrasonic (0.5 {mu}g/L). Typical recoveries of organic phosphorous are between 90 and 95% and the repeatability of the whole procedure is better than 10%. The developed methodology was applied successfully to samples from the oil-well N A 46, platform PNA 2, Campos basin, Brazil. Assessment of the PPCA inhibitor was possible at lower concentrations than achieved by current analytical methods., resulting in benefits such as reduced cost of chemicals, postponed oil production and lower environmental impacts. (author)

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.)

[Effect of the chelator Zn-DTPA on the excretion of lead in lead intoxication mice detected with ICP-MS].

Science.gov (United States)

Li, Chen; Lu, Kai-zhi; Zhou, Qi; Wang, Qiong; Zeng, Yu-liang; Yin, Hong-jun; He, Xuan-hui; Tian, Ying; Dong, Jun-Xing

2014-11-01

To study the lead excretion effect of the chelator Zn-DTPA on the lead intoxication mice, inductively coupled plasma mass spectrometry (ICP-MS) was applied to detect the lead content of biological samples. The acute lead intoxication mice model was established by injecting lead acetate intraperitoneally with the dose of 1 mg. Zn-DTPA was administered intraperitoneally to mice once daily for five consecutive days 4 h after intoxication. Control group, model group, combination of Zn-DTPA and Ca-DTPA group were evaluated at the same time. The urine was collected every day. The mice were sacrificed in batches in the 2rd, 4th, 6th day. Biological samples including urine, whole blood, femur and brain were prepared and nitrated. Lead concentration was detected by ICP-MS. The result showed that Zn-DTPA could increase lead content in urine markedly and reduce lead content in blood, femur and brain.

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

International Nuclear Information System (INIS)

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

2003-01-01

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

Identification of TRIM27 as a novel degradation target of herpes simplex virus 1 ICP0.

Science.gov (United States)

Conwell, Sara E; White, Anne E; Harper, J Wade; Knipe, David M

2015-01-01

The herpes simplex virus 1 (HSV-1) immediate early protein ICP0 performs many functions during infection, including transactivation of viral gene expression, suppression of innate immune responses, and modification and eviction of histones from viral chromatin. Although these functions of ICP0 have been characterized, the detailed mechanisms underlying ICP0's complex role during infection warrant further investigation. We thus undertook an unbiased proteomic approach to identifying viral and cellular proteins that interact with ICP0 in the infected cell. Cellular candidates resulting from our analysis included the ubiquitin-specific protease USP7, the transcriptional repressor TRIM27, DNA repair proteins NBN and MRE11A, regulators of apoptosis, including BIRC6, and the proteasome. We also identified two HSV-1 early proteins involved in nucleotide metabolism, UL39 and UL50, as novel candidate interactors of ICP0. Because TRIM27 was the most statistically significant cellular candidate, we investigated the relationship between TRIM27 and ICP0. We observed rapid, ICP0-dependent loss of TRIM27 during HSV-1 infection. TRIM27 protein levels were restored by disrupting the RING domain of ICP0 or by inhibiting the proteasome, arguing that TRIM27 is a novel degradation target of ICP0. A mutant ICP0 lacking E3 ligase activity interacted with endogenous TRIM27 during infection as demonstrated by reciprocal coimmunoprecipitation and supported by immunofluorescence data. Surprisingly, ICP0-null mutant virus yields decreased upon TRIM27 depletion, arguing that TRIM27 has a positive effect on infection despite being targeted for degradation. These results illustrate a complex interaction between TRIM27 and viral infection with potential positive or negative effects of TRIM27 on HSV under different infection conditions. During productive infection, a virus must simultaneously redirect multiple cellular pathways to replicate itself while evading detection by the host's defenses. To

Transition metal analysis. A comparison between ICP-AES and deuteron activation

International Nuclear Information System (INIS)

Pillay, A.E.; Williams, J.R.; Hassan, S.M.; Al-Hamdi, A.; El Mardi, M.O.

2002-01-01

The analytical capabilities of ICP-AES (ICP) and deuteron activation (associated with prompt gamma-rays and delayed X-rays) for the determination of certain transition metals, were investigated. The sensitivities of the three methods are given, and the general applicability of each technique is evaluated. In the case of ICP, numerical data were obtained from aqueous solutions containing digested plant material. These experimental results were assessed against minimum detectable limits attained in relevant solid matrices that were subjected to prompt gamma-ray and delayed X-ray spectrometry using 5 MeV 2 H + ions. The analytically useful lines originated mainly from (d,p) and (d,n) reactions. The potential of the three techniques for routine analysis is discussed and detailed methodologies are presented. (author)

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

High-Precision Measurement of Eu/Eu* in Geological Glasses via LA-ICP-MS Analysis

Science.gov (United States)

Tang, Ming; McDonough, William F.; Arevalo, Ricardo, Jr.

2014-01-01

Elemental fractionation during laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) analysis has been historically documented between refractory and volatile elements. In this work, however, we observed fractionation between light rare earth elements (LREEs) and heavy rare earth elements (HREEs) when using ablation strategies involving large spot sizes (greater than 100 millimeters) and line scanning mode. In addition: (1) ion yields decrease when using spot sizes above 100 millimeters; (2) (Eu/Eu*)(sub raw) (i.e. Europium anomaly) positively correlates with carrier gas (He) flow rate, which provides control over the particle size distribution of the aerosol reaching the ICP; (3) (Eu/Eu*)(sub raw) shows a positive correlation with spot size, and (4) the changes in REE signal intensity, induced by the He flow rate change, roughly correlate with REE condensation temperatures. The REE fractionation is likely driven by the slight but significant difference in their condensation temperatures. Large particles may not be completely dissociated in the ICP and result in preferential evaporation of the less refractory LREEs and thus non-stoichiometric particle-ion conversion. This mechanism may also be responsible for Sm-Eu-Gd fractionation as Eu is less refractory than Sm and Gd. The extent of fractionation depends upon the particle size distribution of the aerosol, which in turn is influenced by the laser parameters and matrix. Ablation pits and lines defined by low aspect ratios produce a higher proportion of large particles than high aspect ratio ablation, as confirmed by measurements of particle size distribution in the laser induced aerosol. Therefore, low aspect ratio ablation introduces particles that cannot be decomposed and/or atomized by the ICP and thus results in exacerbated elemental fractionation. Accurate quantification of REE concentrations and Eu/Eu* requires reduction of large particle production during laser ablation. For the reference

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

DEFF Research Database (Denmark)

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

2016-01-01

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

Radiochronological Age of a Uranium Metal Sample from an Abandoned Facility

Energy Technology Data Exchange (ETDEWEB)

Meyers, L A; Williams, R W; Glover, S E; LaMont, S P; Stalcup, A M; Spitz, H B

2012-03-16

A piece of scrap uranium metal bar buried in the dirt floor of an old, abandoned metal rolling mill was analyzed using multi-collector inductively coupled plasma mass spectroscopy (MC-ICP-MS). The mill rolled uranium rods in the 1940s and 1950s. Samples of the contaminated dirt in which the bar was buried were also analyzed. The isotopic composition of uranium in the bar and dirt samples were both the same as natural uranium, though a few samples of dirt also contained recycled uranium; likely a result of contamination with other material rolled at the mill. The time elapsed since the uranium metal bar was last purified can be determined by the in-growth of the isotope {sup 230}Th from the decay of {sup 234}U, assuming that only uranium isotopes were present in the bar after purification. The age of the metal bar was determined to be 61 years at the time of this analysis and corresponds to a purification date of July 1950 {+-} 1.5 years.

Radiochronological age of a uranium metal sample from an abandoned facility

International Nuclear Information System (INIS)

Meyers, L.A.; Stalcup, A.M.; Glover, S.E.; Spitz, H.B.

2013-01-01

A piece of scrap uranium metal bar buried in the dirt floor of an old, abandoned metal rolling mill was analyzed using multi-collector inductively coupled plasma mass spectroscopy (MC-ICP-MS). The mill rolled uranium rods in the 1940 and 1950s. Samples of the contaminated dirt in which the bar was buried were also analyzed. The isotopic composition of uranium in the bar and dirt samples were both the same as natural uranium, though a few samples of dirt also contained recycled uranium; likely a result of contamination with other material rolled at the mill. The time elapsed since the uranium metal bar was last purified can be determined by the in-growth of the isotope 230 Th from the decay of 234 U, assuming that only uranium isotopes were present in the bar after purification. The age of the metal bar was determined to be 61 years at the time of this analysis and corresponds to a purification date of July 1950 ± 1.5 years. (author)

Radiochronological Age of a Uranium Metal Sample from an Abandoned Facility

International Nuclear Information System (INIS)

Meyers, L.A.; Williams, R.W.; Glover, S.E.; LaMont, S.P.; Stalcup, A.M.; Spitz, H.B.

2012-01-01

A piece of scrap uranium metal bar buried in the dirt floor of an old, abandoned metal rolling mill was analyzed using multi-collector inductively coupled plasma mass spectroscopy (MC-ICP-MS). The mill rolled uranium rods in the 1940s and 1950s. Samples of the contaminated dirt in which the bar was buried were also analyzed. The isotopic composition of uranium in the bar and dirt samples were both the same as natural uranium, though a few samples of dirt also contained recycled uranium; likely a result of contamination with other material rolled at the mill. The time elapsed since the uranium metal bar was last purified can be determined by the in-growth of the isotope 230 Th from the decay of 234 U, assuming that only uranium isotopes were present in the bar after purification. The age of the metal bar was determined to be 61 years at the time of this analysis and corresponds to a purification date of July 1950 ± 1.5 years.

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

International Nuclear Information System (INIS)

Pedreira Filho, Walter dos Reis

2000-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2005-12-17

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

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

International Nuclear Information System (INIS)

Nygren, U.; Baxter, D.C.

2002-01-01

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

Zinc, lead and copper in human teeth measured by induced coupled argon plasma atomic emission spectroscopy (ICP-AES)

Energy Technology Data Exchange (ETDEWEB)

Chew, L.T.; Bradley, D.A. E-mail: D.A.Bradley@exeter.ac.uk; Mohd, Y.; Jamil, M

2000-11-15

Inductively Coupled Argon Plasma Atomic Emission Spectroscopy (ICP-AES) has been used to determine Pb, Zn and Cu levels in 47 exfoliated human teeth (all of which required extraction for orthodontic reasons). Lead concentrations for the group were 1.7 {mu}g (g tooth mass){sup -1} to 40.5 {mu}g (g tooth mass){sup -1}, with a median of 9.8 {mu}g (g tooth mass){sup -1}. A median lead level in excess of the group value was found for the teeth of six lorry drivers who were included in the study. A more significant enhancement was found for the seven subjects whose age was in excess of 60 years. The median values for Zn and Cu were 123.0 and 0.6 {mu}g (g tooth mass){sup -1} respectively. Present values for tooth-Zn are lower than published data for other ethnic groups.

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

Science.gov (United States)

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

2006-08-01

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

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

International Nuclear Information System (INIS)

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

2002-01-01

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

Redox speciation of final repository relevant elements using separation methods in combination with ICP mass spectrometry; Redoxspeziation von endlagerrelevanten Elementen mit Hilfe von Trennmethoden gekoppelt an ein Massenspektrometer mit induktiv gekoppeltem Plasma

Energy Technology Data Exchange (ETDEWEB)

Graser, Carl-Heinrich

2015-12-18

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

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.

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

Science.gov (United States)

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

2016-04-01

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

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)

David Price--Pioneer of digital ICP monitoring, neurosurgeon and teacher.

Science.gov (United States)

Czosnyka, Marek; Kirollos, Ramez; van Hille, Philip

2015-06-01

In early 1970s first personal desk-top computers started to be available in hospitals. Mr Price was one of the pioneers introducing his own software to identify Marmarou's model of CSF space during infusion studies to diagnose patients suffering from hydrocephalus. His closed-loop control system for infusion of mannitol to manage patients at risk of intracranial hypertension was designed in 1977. The system worked successfully for 10 years in Pinderfields Hospital in Wakefield, UK. In the middle 1980's he initiated international cooperation with Children's Health Centre in Poland in long-term computer-assisted monitoring and analysis of ICP. Software designed in a course of this cooperation paved the way for contemporary package of ICM+ (Intensive Care Monitor, University of Cambridge, UK). Our scientific portfolio from these years (1985-1995) contains hundreds of head injured patients with waveform ICP analysis, introduction of compensatory reserve index RAP, few highly cited papers. Now, we understand ICP much better thanks to David's personal passion and extremely friendly support.

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.

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

International Nuclear Information System (INIS)

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

2017-01-01

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

Determination of trace impurities in uranium-transition metal alloy fuels by ICP-MS using extended common analyte internal standardization (ECAIS) technique

International Nuclear Information System (INIS)

Saha, Abhijit; Deb, S.B.; Nagar, B.K.; Saxena, M.K.

2015-01-01

An analytical methodology was developed for the determination of eight trace impurities viz, Al, B, Cd, Co, Cu, Mg, Mn and Ni in three different uranium-transition metal alloy fuels (U-Me; Me = Ti, Zr and Mo) employing inductively coupled plasma mass spectrometry (ICP-MS). The well known common analyte internal standardization (CAIS) chemometric technique was modified and then employed to minimize and account for the matrix effect on analyte intensity. Standard addition of analytes to the pure synthetic U-Me sample solutions and subsequently their ≥ 94% recovery by the ICP-MS measurement validates the proposed methodology. One real sample of each of these alloys was analyzed by the developed analytical methodology and the %RSD observed was in the range of 5-8%. The method detection limits were found to be within 4-10 μg L -1 . (author)

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

DEFF Research Database (Denmark)

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

2003-01-01

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

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

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

The advantages of orthogonal acceleration in ICP time-of-flight mass spectrometry

International Nuclear Information System (INIS)

Gaal, Andrew

2004-01-01

The OptiMass 8000 incorporates an orthogonal acceleration time-of-flight mass spectrometer. A general schematic of the instrument is given. The continuous ion beam is chopped by an orthogonal accelerator. A push out pulse supply is coupled to the accelerator for providing repetitive push-out voltages at a frequency of 30 kHz. The ion packets that are sliced out of the beam then travel within the field free space towards the SMARTGATE ion blanker. Orthogonal accelerator parameters are set to enable temporal-spatial focusing at the SMARTGATE ion blanker, so that iso-mass ion packets are resolved in time. Any ion packets of unwanted specie are ejected from the direction of travel by supplying pulsed voltages onto the deflection plates of the SMARTGATE. The ions to be measured are let through SMARTGATE and travel further down the field free space, to enter the ion reflectron. The ion reflectron increases the resolution of the mass spectrometer by means of temporal-energy focussing. After reflection, the ions travel within the field free space towards the discrete-dynode detector. In comparison to other acceleration geometries used in elemental time-of-flight mass spectrometry the OptiMass 8000 orthogonal acceleration geometry ultimately leads to superior resolution. As the energy spread is about 3 orders of magnitude lower in the time-of-flight direction for an oaTOFMS in comparison to an on-axis system, aberration acquired in the initial stages of acceleration are much lower. As a result the orthogonal acceleration scheme provides superior resolution at the first spatial focus point and the detector. The orthogonal acceleration time-of-flight analyzer of the OptiMass 8000 is able to provide resolution of at least 1800 at mass 238. (author)

Application of SEC-ICP-MS for comparative analyses of metal-containing species in cancerous and healthy human thyroid samples.

Science.gov (United States)

Boulyga, Sergei F; Loreti, Valeria; Bettmer, Jörg; Heumann, Klaus G

2004-09-01

Size exclusion chromatography (SEC) was coupled on-line to inductively coupled plasma mass spectrometry (ICP-MS) for speciation study of trace metals in cancerous thyroid tissues in comparison to healthy thyroids aimed to estimation of changes in metalloprotein speciation in pathological tissue. The study showed a presence of species binding Cu, Zn, Cd and Pb in healthy thyroid tissue with a good reproducibility of chromatographic results, whereas the same species could not be detected in cancerous tissues. Thus, remarkable differences with respect to metal-binding species were revealed between healthy and pathological thyroid samples, pointing out a completely different distribution of trace metals in cancerous tissues. The metal-binding species could not be identified in the frame of this work because of a lack of appropriate standards. Nevertheless, the results obtained confirm the suitability of SEC-ICP-MS for monitoring of changes in trace metal distribution in cancerous tissue and will help to better understand the role of metal-containing species in thyroid pathology.

Contribution to the understanding of ion-gas reactions in ICP-MS collision reaction cells: application to the resolution of isobaric and polyatomic interferences

International Nuclear Information System (INIS)

Quemet, A.

2012-01-01

Inductively Coupled Plasma Mass Spectrometry (ICP-MS) emerged as the most essential technique in inorganic analytical chemistry thanks to its numerous assets, particularly its flexibility, its sensitivity and its reproducibility. As part of the elementary and isotopic analysis of irradiated fuel and transmutation target, the analyst is faced with a complex mass spectrum, due to the presence of many radionuclides. ICP-MS can not differentiate ions with the same mass, which induces isobaric and polyatomic interferences when the ions at the same mass are different chemical species. Last generations of ICP-MS have introduced collision reaction cells. It can in situ reduce these isobaric or polyatomic interferences. The cell is a multipole (quadrupole, hexapole or octupole) device filled with a collision and/or reaction gas. The gas molecules collide or possibly react with the ion beam, which eliminates or reduces interferences. Such resolution of interferences is based on the difference of chemical behaviours between the analyte and the interfering species: the choice of the gas is crucial. A better understanding of the 'ion - gas' reaction should help choosing the reacting gases. Three ICP-MS, with the different cell geometries, were used for this study: Perkin Elmer Elan DRC e (quadrupole), Thermo Fischer X serie II (hexapole) and Agilent Technologies 7700x (octupole). The effects of the cell geometry on different experimental parameters and on the resolution of the 56 Fe + / 40 Ar 16 O + polyatomic interferences were examined to measure iron at trace or ultra-trace level. This preliminary study was applied to measure iron as impurities in uranium oxide, the method was then validated with a Certified Reference Material. The reactivities of transition metals (Zr, Ru, Pd, Ag, Cd, Sn), lanthanides (La, Ce, Nd, Sm, Eu, Gd, Dy, Er and Yb) and actinides (U, Np, Pu, Am and Cm), elements of interest in the nuclear field, are studied with numerous gases (O 2 , CO, CO 2 , N 2

Identification of Marchfeld asparagus using Sr isotope ratio measurements by MC-ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Swoboda, S; Brunner, M; Boulyga, S F; Galler, P; Prohaska, T [University of Natural Resources and Applied Life Sciences, Department of Chemistry-VIRIS Project, Vienna (Austria); Horacek, M [Austrian Research Centers GmbH, Seibersdorf (Austria)

2008-01-15

This work focuses on testing and application of Sr isotope signatures for the fast and reliable authentication and traceability of Asparagus officinalis originating from Marchfeld, Austria, using multicollector inductively coupled plasma mass spectrometry after optimised Rb/Sr separation. The major sample pool comprises freeze-dried and microwave-digested asparagus samples from Hungary and Slovakia which are compared with Austrian asparagus originating from the Marchfeld region, which is a protected geographical indication. Additional samples from Peru, the Netherlands and Germany were limited in number and allowed therefore only restricted statistical evaluation. Asparagus samples from Marchfeld were harvested within two subsequent years in order to investigate the annual variation. The results show that the Sr isotope ratio is consistent within these 2 years of investigation. Moreover, the Sr isotope ratio of total Sr in soil was found to be significantly higher than in an NH{sub 4}NO{sub 3} extract, reflecting the mobile (bioavailable) phase. The isotope composition in the latter extract corresponds well to the range found in the asparagus samples in Marchfeld, even though the concentration of Sr in asparagus shows no direct correlation to the concentration of Sr in the mobile phase of the soil. The major question was whether the 'Marchfelder Spargel' can be distinguished from samples from the neighbouring countries of Hungary and Slovakia. According to our findings, they can be clearly (100%) singled out from the Hungarian samples and can be distinguished from the Slovakian asparagus samples with a probability of more than 80%. (orig.)

Identification of Marchfeld asparagus using Sr isotope ratio measurements by MC-ICP-MS

Energy Technology Data Exchange (ETDEWEB)

Swoboda, S.; Brunner, M.; Boulyga, S.F.; Galler, P.; Prohaska, T. [University of Natural Resources and Applied Life Sciences, Department of Chemistry-VIRIS Project, Vienna (Austria); Horacek, M. [Austrian Research Centers GmbH, Seibersdorf (Austria)

2008-01-15

This work focuses on testing and application of Sr isotope signatures for the fast and reliable authentication and traceability of Asparagus officinalis originating from Marchfeld, Austria, using multicollector inductively coupled plasma mass spectrometry after optimised Rb/Sr separation. The major sample pool comprises freeze-dried and microwave-digested asparagus samples from Hungary and Slovakia which are compared with Austrian asparagus originating from the Marchfeld region, which is a protected geographical indication. Additional samples from Peru, the Netherlands and Germany were limited in number and allowed therefore only restricted statistical evaluation. Asparagus samples from Marchfeld were harvested within two subsequent years in order to investigate the annual variation. The results show that the Sr isotope ratio is consistent within these 2 years of investigation. Moreover, the Sr isotope ratio of total Sr in soil was found to be significantly higher than in an NH{sub 4}NO{sub 3} extract, reflecting the mobile (bioavailable) phase. The isotope composition in the latter extract corresponds well to the range found in the asparagus samples in Marchfeld, even though the concentration of Sr in asparagus shows no direct correlation to the concentration of Sr in the mobile phase of the soil. The major question was whether the 'Marchfelder Spargel' can be distinguished from samples from the neighbouring countries of Hungary and Slovakia. According to our findings, they can be clearly (100%) singled out from the Hungarian samples and can be distinguished from the Slovakian asparagus samples with a probability of more than 80%. (orig.)

Forensic discrimination of aluminum foil by SR-XRF and ICP-AES

International Nuclear Information System (INIS)

Kasamatsu, Masaaki; Suzuki, Yasuhiro; Suzuki, Shinichi; Miyamoto, Naoki; Watanabe, Seiya; Shimoda, Osamu; Takatsu, Masahisa; Nakanishi, Toshio

2010-01-01

The application of synchrotron radiation X-ray fluorescence spectrometry (SR-XRF) was investigated for the forensic discrimination of aluminum foil by comparisons of the elemental components. Small fragments (1 x 1 mm) were taken from 4 kinds of aluminum foils produced by different manufactures and used for measurements of the XRF spectrum at BL37XU of SPring-8. A comparison of the XRF spectra was effective for the discrimination of aluminum foils from different sources, because significant differences were observed in the X-ray peak intensities of Fe, Cu, Zn, Ga, Zr and Sn. These elements, except for Zr and Sn in the aluminum foils and NIST SRM1258 (Aluminium Alloy 6011), were also determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The observed values of Fe, Cu, Zn and Ga in NIST standard samples by ICP-AES showed satisfactorily good agreements with the certified or information values with relative standard deviations from 1.1% for Zn to 6.7% for Ga. The observed values for the aluminum foils by ICP-AES were compared with those by SR-XRF. Correlation coefficients from 0.997 for Cu/Fe to 0.999 for Zn/Fe and Ga/Fe were obtained between the ratio of the elemental concentration by ICP-AES and normalized the X-ray intensity by SR-XRF. This result demonstrates that a comparison of the normalized X-ray intensity is nearly as effective for the discrimination of aluminum foils as quantitative analysis by ICP-AES. Comparisons of the analytical results by SR-XRF allow the discrimination of all aluminum foils using only a 1 mm 2 fragment with no destruction of the samples. (author)

Molecular Characterization of Prostate Cancer Cell Oncolysis by Herpes Simplex Virus ICP0 Mutants

National Research Council Canada - National Science Library

Mossman, Karen

2006-01-01

.... Briefly, the goals of the proposal were to characterize the oncolytic capacity of Herpes simplex virus type 1 ICP0 mutants in prostate cancer cells given the relationship between ICP0 and two tumor...

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

International Nuclear Information System (INIS)

Isoyama, Naohiko; Oikawa, Shinji; Misonoo, Jun

2008-01-01

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

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)

PIXE and ICP-MS Analysis of Andrographis Paniculata Medicinal Plant

Science.gov (United States)

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

2017-08-01

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

The herpes viral transcription factor ICP4 forms a novel DNA recognition complex

Science.gov (United States)

Tunnicliffe, Richard B.; Lockhart-Cairns, Michael P.; Levy, Colin; Mould, A. Paul; Jowitt, Thomas A.; Sito, Hilary; Baldock, Clair; Sandri-Goldin, Rozanne M.

2017-01-01

Abstract The transcription factor ICP4 from herpes simplex virus has a central role in regulating the gene expression cascade which controls viral infection. Here we present the crystal structure of the functionally essential ICP4 DNA binding domain in complex with a segment from its own promoter, revealing a novel homo-dimeric fold. We also studied the complex in solution by small angle X-Ray scattering, nuclear magnetic resonance and surface-plasmon resonance which indicated that, in addition to the globular domain, a flanking intrinsically disordered region also recognizes DNA. Together the data provides a rationale for the bi-partite nature of the ICP4 DNA recognition consensus sequence as the globular and disordered regions bind synergistically to adjacent DNA motifs. Therefore in common with its eukaryotic host, the viral transcription factor ICP4 utilizes disordered regions to enhance the affinity and tune the specificity of DNA interactions in tandem with a globular domain. PMID:28505309

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

OpenAIRE

Ugarte Baztán, Ana

2014-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Falk, K.

1999-09-01

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

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

International Nuclear Information System (INIS)

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

2018-01-01

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

Precision and accuracy of ST-EDXRF performance for As determination comparing with ICP-MS and evaluation of As deviation in the soil media.

Science.gov (United States)

Akbulut, Songul; Cevik, Ugur; Van, Aydın Ali; De Wael, Karolien; Van Grieken, Rene

2014-02-01

The present study was conducted to (i) determine the precision and accuracy of arsenic measurement in soil samples using ST-EDXRF by comparison with the results of ICP-MS analyses and (ii) identify the relationship of As concentration with soil characteristics. For the analysis of samples, inductively coupled plasma mass spectrometry (ICP-MS) and energy dispersive X-ray fluorescence spectrometry (EDXRF) were performed. According to the results found in the soil samples, the addition of HCl to HNO3, used for the digestion gave significant variations in the recovery of As. However, spectral interferences between peaks for As and Pb can affect detection limits and accuracy for XRF analysis. When comparing the XRF and ICP-MS results a correlation was observed with R(2)=0.8414. This means that using a ST-EDXRF spectrometer, it is possible to achieve accurate and precise analysis by the calibration of certified reference materials and choosing an appropriate secondary target. On the other hand, with regard to soil characteristics analyses, the study highlighted that As is mostly anthropogenically enriched in the studied area. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

Science.gov (United States)

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

2017-06-22

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

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

International Nuclear Information System (INIS)

Conde, E.; Navarro, N.; Fernández, M.

2015-01-01

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

Integrated care pathways for airway diseases (AIRWAYS-ICPs)

DEFF Research Database (Denmark)

Bousquet, J; Addis, A; Adcock, I

2014-01-01

The objective of Integrated Care Pathways for Airway Diseases (AIRWAYS-ICPs) is to launch a collaboration to develop multi-sectoral care pathways for chronic respiratory diseases in European countries and regions. AIRWAYS-ICPs has strategic relevance to the European Union Health Strategy...... and will add value to existing public health knowledge by: 1) proposing a common framework of care pathways for chronic respiratory diseases, which will facilitate comparability and trans-national initiatives; 2) informing cost-effective policy development, strengthening in particular those on smoking...... and environmental exposure; 3) aiding risk stratification in chronic disease patients, using a common strategy; 4) having a significant impact on the health of citizens in the short term (reduction of morbidity, improvement of education in children and of work in adults) and in the long-term (healthy ageing); 5...

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

Science.gov (United States)

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

2017-12-01

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

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

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.

PIXE analysis of human stones: comparison with data from ICP-AES

International Nuclear Information System (INIS)

Pougnet, M.A.B.; Peisach, M.; Pineda, C.A.; Rodgers, A.L.

1987-01-01

25 human stone samples previously analyzed by inductively coupled plasma atomic emission spectroscopy (ICP-AES) and the IAEA Animal Bone Standard Reference Material were used to evaluate trace element analysis by PIXE. Bombardment with 4 MeV protons was used for the determination of Mn, Fe, Cu, Pb, Br, Rb, Sr and Ca. PIXE and ICP-AES data gave correlation factors better than 0.97 for the elements Ca, Fe, Zn, Sr and Pb. (author) 9 refs.; 5 figs

Some aspects of ICP-AES analysis of high purity rare earths

International Nuclear Information System (INIS)

Murty, P.S.; Biswas, S.S.

1991-01-01

Inductively coupled plasma atomic emission spectrometry (ICP-AES) is a technique capable of giving high sensitivity in trace elemental analysis. While the technique possesses high sensitivity, it lacks high selectivity. Selectivity is important where substances emitting complex spectra are to be analysed for trace elements. Rare earths emit highly complex spectra in a plasma source and the determination of adjacent rare earths in a high purity rare earth matrix, with high sensitivity, is not possible due to the inadequate selectivity of ICP-AES. One approach that has yielded reasonably good spectral selectivity in the high purity rare earth analysis by ICP-AES is by employing a combination of wavelength modulation techniques and high resolution echelle grating. However, it was found that by using a high resolution monochromator senstitivities either comparable to or better than those reported by the wavelength modulation technique could be obtained. (author). 2 refs., 2 figs., 2 tabs

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

International Nuclear Information System (INIS)

Dufailly, Vincent; Noel, Laurent; Guerin, Thierry

2006-01-01

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

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

International Nuclear Information System (INIS)

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

2007-01-01

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

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

Science.gov (United States)

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

2007-10-01

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

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

Science.gov (United States)

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

2017-03-01

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

Identification of a divalent metal cation binding site in herpes simplex virus 1 (HSV-1) ICP8 required for HSV replication.

Science.gov (United States)

Bryant, Kevin F; Yan, Zhipeng; Dreyfus, David H; Knipe, David M

2012-06-01

Herpes simplex virus 1 (HSV-1) ICP8 is a single-stranded DNA-binding protein that is necessary for viral DNA replication and exhibits recombinase activity in vitro. Alignment of the HSV-1 ICP8 amino acid sequence with ICP8 homologs from other herpesviruses revealed conserved aspartic acid (D) and glutamic acid (E) residues. Amino acid residue D1087 was conserved in every ICP8 homolog analyzed, indicating that it is likely critical for ICP8 function. We took a genetic approach to investigate the functions of the conserved ICP8 D and E residues in HSV-1 replication. The E1086A D1087A mutant form of ICP8 failed to support the replication of an ICP8 mutant virus in a complementation assay. E1086A D1087A mutant ICP8 bound DNA, albeit with reduced affinity, demonstrating that the protein is not globally misfolded. This mutant form of ICP8 was also recognized by a conformation-specific antibody, further indicating that its overall structure was intact. A recombinant virus expressing E1086A D1087A mutant ICP8 was defective in viral replication, viral DNA synthesis, and late gene expression in Vero cells. A class of enzymes called DDE recombinases utilize conserved D and E residues to coordinate divalent metal cations in their active sites. We investigated whether the conserved D and E residues in ICP8 were also required for binding metal cations and found that the E1086A D1087A mutant form of ICP8 exhibited altered divalent metal binding in an in vitro iron-induced cleavage assay. These results identify a novel divalent metal cation-binding site in ICP8 that is required for ICP8 functions during viral replication.

Quantitative characterization of TiO2 nanoparticle release from textiles by conventional and single particle ICP-MS

Science.gov (United States)

Mackevica, Aiga; Olsson, Mikael Emil; Hansen, Steffen Foss

2018-01-01

TiO2 is ubiquitously present in a wide range of everyday items, both as an intentionally incorporated additive and naturally occurring constituent. It can be found in a wide range of consumer products, including personal care products, food contact materials, and textiles. Normal use of these products may lead to consumer and/or environmental exposure to TiO2, possibly in form of nanoparticles. The aim of this study is to perform a leaching test and apply state-of-the-art methods to investigate nano-TiO2 and total Ti release from five types of commercially available conventional textiles: table placemats, wet wipes, microfiber cloths, and two types of baby bodysuits, with Ti contents ranging from 2.63 to 1448 μg/g. Released particle analysis was performed using conventional and single particle inductively coupled plasma mass spectrometry (ICP-MS and spICP-MS), in conjunction with transmission electron microscopy (TEM), to measure total and particulate TiO2 release by mass and particle number, as well as size distribution. Less than 1% of the initial Ti content was released over 24 h of leaching, with the highest releases reaching 3.13 μg/g. The fraction of nano-TiO2 released varied among fabric types and represented 0-80% of total TiO2 release. Particle mode sizes were 50-75 nm, and TEM imaging revealed particles in sizes of 80-200 nm. This study highlights the importance of using a multi-method approach to obtain quantitative release data that is able to provide an indication regarding particle number, size distribution, and mass concentration, all of which can help in understanding the fate and exposure of nanoparticles.

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

Science.gov (United States)

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

2017-04-15

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

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

Science.gov (United States)

Horstwood, M.

2016-12-01

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

Role of mass spectrometry in nuclear forensic science

International Nuclear Information System (INIS)

Joseph, M.; Sivaraman, N.

2016-01-01

The present talk will focus on the role of mass spectrometry in NFS in general; besides that, the various chromatographic methods developed towards separation of actinides and lanthanide fission products and characterization of dissolver solutions of nuclear reactor fuels using TIMS and some applications of using ICP-MS as well

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)

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

Energy Technology Data Exchange (ETDEWEB)

Oliveira, Thiago Cesar de

2014-06-01

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

Identification of an ICP27-responsive element in the coding region of a herpes simplex virus type 1 late gene.

Science.gov (United States)

Sedlackova, Lenka; Perkins, Keith D; Meyer, Julia; Strain, Anna K; Goldman, Oksana; Rice, Stephen A

2010-03-01

During productive herpes simplex virus type 1 (HSV-1) infection, a subset of viral delayed-early (DE) and late (L) genes require the immediate-early (IE) protein ICP27 for their expression. However, the cis-acting regulatory sequences in DE and L genes that mediate their specific induction by ICP27 are unknown. One viral L gene that is highly dependent on ICP27 is that encoding glycoprotein C (gC). We previously demonstrated that this gene is posttranscriptionally transactivated by ICP27 in a plasmid cotransfection assay. Based on our past results, we hypothesized that the gC gene possesses a cis-acting inhibitory sequence and that ICP27 overcomes the effects of this sequence to enable efficient gC expression. To test this model, we systematically deleted sequences from the body of the gC gene and tested the resulting constructs for expression. In so doing, we identified a 258-bp "silencing element" (SE) in the 5' portion of the gC coding region. When present, the SE inhibits gC mRNA accumulation from a transiently transfected gC gene, unless ICP27 is present. Moreover, the SE can be transferred to another HSV-1 gene, where it inhibits mRNA accumulation in the absence of ICP27 and confers high-level expression in the presence of ICP27. Thus, for the first time, an ICP27-responsive sequence has been identified in a physiologically relevant ICP27 target gene. To see if the SE functions during viral infection, we engineered HSV-1 recombinants that lack the SE, either in a wild-type (WT) or ICP27-null genetic background. In an ICP27-null background, deletion of the SE led to ICP27-independent expression of the gC gene, demonstrating that the SE functions during viral infection. Surprisingly, the ICP27-independent gC expression seen with the mutant occurred even in the absence of viral DNA synthesis, indicating that the SE helps to regulate the tight DNA replication-dependent expression of gC.

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

NARCIS (Netherlands)

Krystek, Petra; Heumann, Klaus G.

1999-01-01

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

Analytical data and sample locality map for aqua-regia leachates of stream sediments analyzed by ICP, and emission spectrographic and ICP results for many NURE stream sediments from the Killik River Quadrangle, Alaska

International Nuclear Information System (INIS)

Motooka, J.M.; Adrian, B.M.; Church, S.E.; McDougal, C.M.; Fife, J.B.

1989-01-01

A U.S. Geological Survey report is presented giving analytical data and sample locality map for aqua-regia leachates of stream sediments analyzed by ICP, and emission spectrographic and ICP results for many NURE stream sediments from the Killik River Quadrangle, Alaska

ICP MS selection of radiopure materials for the GERDA experiment

Science.gov (United States)

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

2015-08-01

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

ICP MS selection of radiopure materials for the GERDA experiment

Energy Technology Data Exchange (ETDEWEB)

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

2015-08-17

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

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

International Nuclear Information System (INIS)

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

1999-01-01

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

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