Ion sampling and transport in Inductively Coupled Plasma Mass Spectrometry

NASA Astrophysics Data System (ADS)

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.

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

PubMed

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.

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

NASA Astrophysics Data System (ADS)

Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J. M.; García Alonso, J. I.

2015-06-01

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

Matrix effects in inductively coupled plasma mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen, Xiaoshan

1995-07-07

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 "Fassel" 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,more » 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.« less

Final Report on Jobin Yvon Contained Inductively Coupled Plasma Emission Spectrometer

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pennebaker, F.M.

2003-03-17

A new Inductively Coupled Plasma -- Emission Spectrometer (ICP-ES) was recently purchased and installed in Lab B-147/151 at SRTC. The contained JY Model Ultima 170-C ICP-ES has been tested and compared to current ADS ICP-ES instrumentation. The testing has included both performance tests to evaluate instrumental ability, and the measurement of matrix standards commonly analyzed by ICP-ES at Savannah River. In developing operating procedures for this instrument, we have implemented the use of internal standards and off-peak background subtraction. Both of these techniques are recommended by EPA SW-846 ICP-ES methods and are common to current ICP-ES operations. Based on themore » testing and changes, the JY Model Ultima 170-C ICP-ES provides improved performance for elemental analysis of radioactive samples in the Analytical Development Section.« less

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

PubMed

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 <4% transformation over more than two months. High ionic strengths matrices (>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.

Spectral interferences in the determination of rhenium in molybdenum and copper concentrates by inductively coupled plasma optical emission spectrometry (ICP-OES)

NASA Astrophysics Data System (ADS)

Karadjov, Metody; Velitchkova, Nikolaya; Veleva, Olga; Velichkov, Serafim; Markov, Pavel; Daskalova, Nonka

2016-05-01

This paper deals with spectral interferences of complex matrix containing Mo, Al, Ti, Fe, Mg, Ca and Cu in the determination of rhenium in molybdenum and copper concentrates by inductively coupled plasma optical emission spectrometry (ICP-OES). By radial viewing 40.68 MHz ICP equipped with a high resolution spectrometer (spectral bandwidth = 5 pm) the hyperfine structure (HFS) of the most prominent lines of rhenium (Re II 197.248 nm, Re II 221.426 nm and Re II 227.525 nm) was registered. The HFS components under high resolution conditions were used as separate prominent line in order to circumvent spectral interferences. The Q-concept was applied for quantification of spectral interferences. The quantitative databases for the type and the magnitude of the spectral interferences in the presence of above mentioned matrix constituents were obtained by using a radial viewing 40.68 MHz ICP with high resolution and an axial viewing 27.12 MHz ICP with middle resolution. The data for the both ICP-OES systems were collected chiefly with a view to spectrochemical analysis for comparing the magnitude of line and wing (background) spectral interference and the true detection limits with spectroscopic apparatus with different spectral resolution. The sample pretreatment methods by sintering with magnesium oxide and oxidizing agents as well as a microwave acid digestion were applied. The feasibility, accuracy and precision of the analytical results were experimentally demonstrated by certified reference materials.

Quantitative aspects of inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Bulska, Ewa; Wagner, Barbara

2016-10-01

Accurate determination of elements in various kinds of samples is essential for many areas, including environmental science, medicine, as well as industry. Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful tool enabling multi-elemental analysis of numerous matrices with high sensitivity and good precision. Various calibration approaches can be used to perform accurate quantitative measurements by ICP-MS. They include the use of pure standards, matrix-matched standards, or relevant certified reference materials, assuring traceability of the reported results. This review critically evaluates the advantages and limitations of different calibration approaches, which are used in quantitative analyses by ICP-MS. Examples of such analyses are provided. This article is part of the themed issue 'Quantitative mass spectrometry'.

Quantification of Al2O3 nanoparticles in human cell lines applying inductively coupled plasma mass spectrometry (neb-ICP-MS, LA-ICP-MS) and flow cytometry-based methods

NASA Astrophysics Data System (ADS)

Böhme, Steffi; Stärk, Hans-Joachim; Meißner, Tobias; Springer, Armin; Reemtsma, Thorsten; Kühnel, Dana; Busch, Wibke

2014-09-01

In order to quantify and compare the uptake of aluminum oxide nanoparticles of three different sizes into two human cell lines (skin keratinocytes (HaCaT) and lung epithelial cells (A549)), three analytical methods were applied: digestion followed by nebulization inductively coupled plasma mass spectrometry (neb-ICP-MS), direct laser ablation ICP-MS (LA-ICP-MS), and flow cytometry. Light and electron microscopy revealed an accumulation and agglomeration of all particle types within the cell cytoplasm, whereas no particles were detected in the cell nuclei. The internalized Al2O3 particles exerted no toxicity in the two cell lines after 24 h of exposure. The smallest particles with a primary particle size ( x BET) of 14 nm (Alu1) showed the lowest sedimentation velocity within the cell culture media, but were calculated to have settled completely after 20 h. Alu2 ( x BET = 111 nm) and Alu3 ( x BET = 750 nm) were calculated to reach the cell surface after 7 h and 3 min, respectively. The internal concentrations determined with the different methods lay in a comparable range of 2-8 µg Al2O3/cm2 cell layer, indicating the suitability of all methods to quantify the nanoparticle uptake. Nevertheless, particle size limitations of analytical methods using optical devices were demonstrated for LA-ICP-MS and flow cytometry. Furthermore, the consideration and comparison of particle properties as parameters for particle internalization revealed the particle size and the exposure concentration as determining factors for particle uptake.

Quantitative aspects of inductively coupled plasma mass spectrometry

PubMed Central

Wagner, Barbara

2016-01-01

Accurate determination of elements in various kinds of samples is essential for many areas, including environmental science, medicine, as well as industry. Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful tool enabling multi-elemental analysis of numerous matrices with high sensitivity and good precision. Various calibration approaches can be used to perform accurate quantitative measurements by ICP-MS. They include the use of pure standards, matrix-matched standards, or relevant certified reference materials, assuring traceability of the reported results. This review critically evaluates the advantages and limitations of different calibration approaches, which are used in quantitative analyses by ICP-MS. Examples of such analyses are provided. This article is part of the themed issue ‘Quantitative mass spectrometry’. PMID:27644971

Flow-field differences and electromagnetic-field properties of air and N2 inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Yu, Minghao; Yamada, Kazuhiko; Takahashi, Yusuke; Liu, Kai; Zhao, Tong

2016-12-01

A numerical model for simulating air and nitrogen inductively coupled plasmas (ICPs) was developed considering thermochemical nonequilibrium and the third-order electron transport properties. A modified far-field electromagnetic model was introduced and tightly coupled with the flow field equations to describe the Joule heating and inductive discharge phenomena. In total, 11 species and 49 chemical reactions of air, which include 5 species and 8 chemical reactions of nitrogen, were employed to model the chemical reaction process. The internal energy transfers among translational, vibrational, rotational, and electronic energy modes of chemical species were taken into account to study thermal nonequilibrium effects. The low-Reynolds number Abe-Kondoh-Nagano k-ɛ turbulence model was employed to consider the turbulent heat transfer. In this study, the fundamental characteristics of an ICP flow, such as the weak ionization, high temperature but low velocity in the torch, and wide area of the plasma plume, were reproduced by the developed numerical model. The flow field differences between the air and nitrogen ICP flows inside the 10-kW ICP wind tunnel were made clear. The interactions between the electromagnetic and flow fields were also revealed for an inductive discharge.

Isotope dilution inductively coupled plasma mass spectrometry (ID ICP-MS) for the certification of lead and cadmium in environmental standard reference materials.

PubMed

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.

High intensity ion beams from an atmospheric pressure inductively coupled plasma

NASA Astrophysics Data System (ADS)

Al Moussalami, S.; Chen, W.; Collings, B. A.; Douglas, D. J.

2002-02-01

This work is directed towards substantially improving the sensitivity of an inductively coupled plasma mass spectrometer (ICP-MS). Ions produced in the ICP at atmospheric pressure have been extracted with comparatively high current densities. The conventional approach to ion extraction, based on a skimmed molecular beam, has been abandoned, and a high extraction field arrangement has been adopted. Although the new approach is not optimized, current densities more than 180 times greater than that of a conventional interface have been extracted and analyte sensitivities ˜10-100× greater than those reported previously for quadrupole ICP-MS have been measured.

Method validation for simultaneous determination of chromium, molybdenum and selenium in infant formulas by ICP-OES and ICP-MS.

PubMed

Khan, Naeem; Jeong, In Seon; Hwang, In Min; Kim, Jae Sung; Choi, Sung Hwa; Nho, Eun Yeong; Choi, Ji Yeon; Kwak, Byung-Man; Ahn, Jang-Hyuk; Yoon, Taehyung; Kim, Kyong Su

2013-12-15

This study aimed to validate the analytical method for simultaneous determination of chromium (Cr), molybdenum (Mo), and selenium (Se) in infant formulas available in South Korea. Various digestion methods of dry-ashing, wet-digestion and microwave were evaluated for samples preparation and both inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS) were compared for analysis. The analytical techniques were validated by detection limits, precision, accuracy and recovery experiments. Results showed that wet-digestion and microwave methods were giving satisfactory results for sample preparation, while ICP-MS was found more sensitive and effective technique than ICP-OES. The recovery (%) of Se, Mo and Cr by ICP-OES were 40.9, 109.4 and 0, compared to 99.1, 98.7 and 98.4, respectively by ICP-MS. The contents of Cr, Mo and Se in infant formulas by ICP-MS were found in good nutritional values in accordance to nutrient standards for infant formulas CODEX values. Copyright © 2013 Elsevier Ltd. All rights reserved.

Comparison method for uranium determination in ore sample by inductively coupled plasma optical emission spectrometry (ICP-OES).

PubMed

Sert, Şenol

2013-07-01

A comparison method for the determination (without sample pre-concentration) of uranium in ore by inductively coupled plasma optical emission spectrometry (ICP-OES) has been performed. The experiments were conducted using three procedures: matrix matching, plasma optimization, and internal standardization for three emission lines of uranium. Three wavelengths of Sm were tested as internal standard for the internal standardization method. The robust conditions were evaluated using applied radiofrequency power, nebulizer argon gas flow rate, and sample uptake flow rate by considering the intensity ratio of the Mg(II) 280.270 nm and Mg(I) 285.213 nm lines. Analytical characterization of method was assessed by limit of detection and relative standard deviation values. The certificated reference soil sample IAEA S-8 was analyzed, and the uranium determination at 367.007 nm with internal standardization using Sm at 359.260 nm has been shown to improve accuracy compared with other methods. The developed method was used for real uranium ore sample analysis.

Diagnostic studies of ion beam formation in inductively coupled plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jacobs, Jenee L.

2015-01-01

This dissertation describes a variety of studies focused on the plasma and the ion beam in inductively coupled plasma mass spectrometry (ICP-MS). The ability to use ICP-MS for measurements of trace elements in samples requires the analytes to be efficiently ionized. Updated ionization efficiency tables are discussed for ionization temperatures of 6500 K and 7000 K with an electron density of 1 x 10 15 cm -3. These values are reflective of the current operating parameters of ICP-MS instruments. Calculations are also discussed for doubly charged (M 2+) ion formation, neutral metal oxide (MO) ionization, and metal oxide (MO +)more » ion dissociation for similar plasma temperature values. Ionization efficiency results for neutral MO molecules in the ICP have not been reported previously.« less

[Study on the determination of 28 inorganic elements in sunflower seeds by ICP-OES/ICP-MS].

PubMed

Liu, Hong-Wei; Qin, Zong-Hui; Xie, Hua-Lin; Cao, Shu

2013-01-01

The present paper describes a simple method for the determination of trace elements in sunflower seeds by using inductively coupled plasma optical emission spectrometry (ICP-OES) and inductively coupled plasma spectrometry (ICP-MS). HNO3 + H2O2 were used to achieve the complete decomposition of the organic matrix in a closed-vessel microwave oven. The contents of 10 trace elements (Al, B, Ca, Fe, K, Mg, Na, Si, P and S) in sunflower seeds were determined by ICP-OES while 18 trace elements (As, Ba, Cd, Co, Cr, Cu, Li, Mn, Mo, Ni, Pb, Rb, Sr, Sn, Sb, Ti, V and Zn) were determined by ICP-MS. The rice reference material (GBW10045) was used as standard reference materials. The results showed a good agreement between measured and certified values for all analytes. The concentrations of necessary micro elements Ca, K, Mg, P and S were higher. This method was simple, sensitive and precise and can perform simultaneous multi-elements determination of sunflower seeds.

Bioimaging of metals in brain tissue by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and metallomics.

PubMed

Becker, J Sabine; Matusch, Andreas; Palm, Christoph; Salber, Dagmar; Morton, Kathryn A; Becker, J Susanne

2010-02-01

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been developed and established as an emerging technique in the generation of quantitative images of metal distributions in thin tissue sections of brain samples (such as human, rat and mouse brain), with applications in research related to neurodegenerative disorders. A new analytical protocol is described which includes sample preparation by cryo-cutting of thin tissue sections and matrix-matched laboratory standards, mass spectrometric measurements, data acquisition, and quantitative analysis. Specific examples of the bioimaging of metal distributions in normal rodent brains are provided. Differences to the normal were assessed in a Parkinson's disease and a stroke brain model. Furthermore, changes during normal aging were studied. Powerful analytical techniques are also required for the determination and characterization of metal-containing proteins within a large pool of proteins, e.g., after denaturing or non-denaturing electrophoretic separation of proteins in one-dimensional and two-dimensional gels. LA-ICP-MS can be employed to detect metalloproteins in protein bands or spots separated after gel electrophoresis. MALDI-MS can then be used to identify specific metal-containing proteins in these bands or spots. The combination of these techniques is described in the second section.

Liquid chromatography coupled with inductively coupled plasma mass spectrometry in the pharmaceutical industry: selected examples.

PubMed

Marshall, Peter S; Leavens, Bill; Heudi, Olivier; Ramirez-Molina, Cesar

2004-11-12

Both LC and capillary LC (CapLC) have been successfully interfaced with inductively coupled plasma mass spectrometry (ICP-MS). Gradients of acetonitrile and aqueous based solvents have been employed to separate several compounds of pharmaceutical interest. This paper will describe four application areas in the pharmaceutical industry, and examples will be shown where CapLC, LC and gel electrophoresis via laser ablation have been coupled with ICP-MS. The four areas highlighted in this paper are: (1) the use of derivatisation reactions to "make the invisible visible". Methods involving derivatisations with copper and iron will be described that can be used for the analysis of amines and carboxylic acids by ICP-MS. (2) The profiling of metal ion content (in particular bromine) in biological samples such as human plasma, this study will focus on the metabolism of bromine-labelled peptides (e.g. substance P). (3) The analysis of materials derived from single, solid-phase beads used in combinatorial chemistry, and (4) also discussed will be our findings from investigations into the use of laser ablation ICP-MS on the determination of protein phosphorylation on electrophoresis gel blots.

Starter for inductively coupled plasma tube

DOEpatents

Hull, Donald E.; Bieniewski, Thomas M.

1988-01-01

A starter assembly is provided for use with an inductively coupled plasma (ICP) tube to reliably initate a plasma at internal pressures above about 30 microns. A conductive probe is inserted within the inductor coil about the tube and insulated from the tube shield assembly. A capacitive circuit is arranged for momentarily connecting a high voltage radio-frequency generator to the probe while simultaneously energizing the coil. When the plasma is initiated the probe is disconnected from the generator and electrically connected to the shield assembly for operation.

Starter for inductively coupled plasma tube

DOEpatents

Hull, D.E.; Bieniewski, T.M.

1988-08-23

A starter assembly is provided for use with an inductively coupled plasma (ICP) tube to reliably initiate a plasma at internal pressures above about 30 microns. A conductive probe is inserted within the inductor coil about the tube and insulated from the tube shield assembly. A capacitive circuit is arranged for momentarily connecting a high voltage radio-frequency generator to the probe while simultaneously energizing the coil. When the plasma is initiated the probe is disconnected from the generator and electrically connected to the shield assembly for operation. 1 fig.

Gas and liquid chromatography with inductively coupled plasma mass spectrometry detection for environmental speciation analysis — advances and limitations

NASA Astrophysics Data System (ADS)

Szpunar, Joanna; McSheehy, Shona; Połeć, Kasia; Vacchina, Véronique; Mounicou, Sandra; Rodriguez, Isaac; Łobiński, Ryszard

2000-07-01

Recent advances in the coupling of gas chromatography (GC) and high performance liquid chromatography (HPLC) with inductively coupled plasma mass spectrometry (ICP MS) and their role in trace element speciation analysis of environmental materials are presented. The discussion is illustrated with three research examples concerning the following topics: (i) development and coupling of multicapillary microcolumn GC with ICP MS for speciation of organotin in sediment and biological tissue samples; (ii) speciation of arsenic in marine algae by size-exclusion-anion-exchange HPLC-ICP MS; and (iii) speciation of cadmium in plant cell cultures by size-exclusion HPLC-ICP MS. Particular attention is paid to the problem of signal identification in ICP MS chromatograms; the potential of electrospray MS/MS for this purpose is highlighted.

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

PubMed

Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente; Sturup, Stefan; Nielsen, Camilla

2006-02-24

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, the resolution of the test substances was only slightly affected when the linear flow velocity was increased from 0.5 to 1.9 mm s(-1). However, the sensitivity of ICP-MS detection decreased when the linear flow velocity was increased from 0.5 to 1.9 mm s(-1). Analytical figures of merit were determined 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 and quantification were better than 3.3 and 11 microg BrL(-1), respectively. The analysis time was reduced to 2.7 min when the flow rate was increased to 90 microL min(-1) and limits of detection and quantification were better than 20 and 65 microg BrL(-1), respectively. The method was applied for quantitative analysis of bromine-containing preservatives in commercially available cosmetic products.

Effect of neutral gas heating in argon radio frequency inductively coupled plasma

NASA Astrophysics Data System (ADS)

Chin, O. H.; Jayapalan, K. K.; Wong, C. S.

2014-08-01

Heating of neutral gas in inductively coupled plasma (ICP) is known to result in neutral gas depletion. In this work, this effect is considered in the simulation of the magnetic field distribution of a 13.56 MHz planar coil ICP. Measured electron temperatures and densities at argon pressures of 0.03, 0.07 and 0.2 mbar were used in the simulation whilst neutral gas temperatures were heuristically fitted. The simulated results showed reasonable agreement with the measured magnetic field profile.

Capillary electrophoresis-high resolution sector field inductively coupled plasma mass spectrometry.

PubMed

Sonke, Jeroen E; Salters, Vincent J M

2007-08-03

The background and applications of high resolution sector field inductively coupled plasma mass spectrometry (HR-ICP-MS) as a detector for capillary (CE) and gel electrophoretic separations are reviewed. Notable progress has been made in the fields of bioinorganic and environmental (geo-) chemistry. Metallomics, the study of metal species interactions and functions in biological systems, puts substantial technical demands on speciation analysis. The combination of high species resolving power (CE) and high sensitivity-high mass resolving power (HR-ICP-MS) provides a solid base to meet such demands.

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

NASA Astrophysics Data System (ADS)

Becker, Johanna Sabine

2002-12-01

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

Investigation of large-area multicoil inductively coupled plasma sources using three-dimensional fluid model

NASA Astrophysics Data System (ADS)

Brcka, Jozef

2016-07-01

A multi inductively coupled plasma (ICP) system can be used to maintain the plasma uniformity and increase the area processed by a high-density plasma. This article presents a source in two different configurations. The distributed planar multi ICP (DM-ICP) source comprises individual ICP sources that are not overlapped and produce plasma independently. Mutual coupling of the ICPs may affect the distribution of the produced plasma. The integrated multicoil ICP (IMC-ICP) source consists of four low-inductance ICP antennas that are superimposed in an azimuthal manner. The identical geometry of the ICP coils was assumed in this work. Both configurations have highly asymmetric components. A three-dimensional (3D) plasma model of the multicoil ICP configurations with asymmetric features is used to investigate the plasma characteristics in a large chamber and the operation of the sources in inert and reactive gases. The feasibility of the computational calculation, the speed, and the computational resources of the coupled multiphysics solver are investigated in the framework of a large realistic geometry and complex reaction processes. It was determined that additional variables can be used to control large-area plasmas. Both configurations can form a plasma, that azimuthally moves in a controlled manner, the so-called “sweeping mode” (SM) or “polyphase mode” (PPM), and thus they have the potential for large-area and high-density plasma applications. The operation in the azimuthal mode has the potential to adjust the plasma distribution, the reaction chemistry, and increase or modulate the production of the radicals. The intrinsic asymmetry of the individual coils and their combined operation were investigated within a source assembly primarily in argon and CO gases. Limited investigations were also performed on operation in CH4 gas. The plasma parameters and the resulting chemistry are affected by the geometrical relation between individual antennas. The aim of

Quantification and visualization of glutathione S-transferase omega 1 in cells using inductively coupled plasma mass spectrometry (ICP-MS) and fluorescence microscopy.

PubMed

Liang, Yong; Jiang, Xin; Tang, Nannan; Yang, Limin; Chen, Haifeng; Wang, Qiuquan

2015-03-01

We report a novel activity-based and Cu-free click chemistry (CC) mediated methodology for glutathione S-transferase omega 1 (GSTO1) quantification using species-unspecific isotope dilution inductively coupled plasma mass spectrometry (SUID ICP-MS), in which dibenzylcyclooctyne-modified 2-chloroacetamide (DBCO-ChAcA) was designed and synthesized, meanwhile, as a navigator towards GSTO1 for subsequent N3-DOTA-Eu-tagging via Cu-free CC. Using (153)Eu-SUID ICP-MS coupled with size exclusion chromatography (SEC), the LOD (3σ) of GSTO1 reached 6.9 fmol with an RSD of 2.4% at the 0.1 μM level (n = 5) considering the recovery of GSTO1 on the SEC was 96.5 ± 2.4%. The GSTO1 contents in the cells of human hepatocellular carcinoma C7721 and breast carcinoma MCF-7 as well as normal hepatic C7701 without or with cis-platin administration were quantified to be from 1.2 μg/10,000 cells (n = 3, RSD = 4.5%) corresponding to 1.2 × 10(-2) ng per cell to 4.76 μg/10,000 cells (n = 3, RSD = 2.9%) corresponding to 4.76 × 10(-2) ng per cell. For a comparative study, DBCO-ChAcA-fluor 488-based fluorescence microscopy could not alone visualize GSTO1 in the cells but could together with those from the small SH-containing molecules such as GSH and that from extra N3-fluor 488 in the cells. This activity-based CC-mediated tagging/labeling strategy provided an opportunity for ICP-MS-based targeted protein quantification, and is very much expected to find its applications in biological mechanism study and the subsequent drug design.

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.

PubMed

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

Tissue gadolinium deposition in renally impaired rats exposed to different gadolinium-based MRI contrast agents: evaluation with inductively coupled plasma mass spectrometry (ICP-MS).

PubMed

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.

Predictions of ion energy distributions and radical fluxes in radio frequency biased inductively coupled plasma etching reactors

NASA Astrophysics Data System (ADS)

Hoekstra, Robert J.; Kushner, Mark J.

1996-03-01

Inductively coupled plasma (ICP) reactors are being developed for low gas pressure (<10s mTorr) and high plasma density ([e]≳1011 cm-3) microelectronics fabrication. In these reactors, the plasma is generated by the inductively coupled electric field while an additional radio frequency (rf) bias is applied to the substrate. One of the goals of these systems is to independently control the magnitude of the ion flux by the inductively coupled power deposition, and the acceleration of ions into the substrate by the rf bias. In high plasma density reactors the width of the sheath above the wafer may be sufficiently thin that ions are able to traverse it in approximately 1 rf cycle, even at 13.56 MHz. As a consequence, the ion energy distribution (IED) may have a shape typically associated with lower frequency operation in conventional reactive ion etching tools. In this paper, we present results from a computer model for the IED incident on the wafer in ICP etching reactors. We find that in the parameter space of interest, the shape of the IED depends both on the amplitude of the rf bias and on the ICP power. The former quantity determines the average energy of the IED. The latter quantity controls the width of the sheath, the transit time of ions across the sheath and hence the width of the IED. In general, high ICP powers (thinner sheaths) produce wider IEDs.

Developments in ICP-MS: electrochemically modulated liquid chromatography for the clean-up of ICP-MS blanks and reduction of matrix effects by flow injection ICP-MS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gross, Cory Thomas

2008-01-01

The focus of this dissertation is the development of techniques with which to enhance the existing abilities of inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS is a powerful technique for trace metal analysis in samples of many types, but like any technique it has certain strengths and weaknesses. Attempts are made to improve upon those strengths and to overcome certain weaknesses.

Provenance establishment of coffee using solution ICP-MS and ICP-AES.

PubMed

Valentin, Jenna L; Watling, R John

2013-11-01

Statistical interpretation of the concentrations of 59 elements, determined using solution based inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma emission spectroscopy (ICP-AES), was used to establish the provenance of coffee samples from 15 countries across five continents. Data confirmed that the harvest year, degree of ripeness and whether the coffees were green or roasted had little effect on the elemental composition of the coffees. The application of linear discriminant analysis and principal component analysis of the elemental concentrations permitted up to 96.9% correct classification of the coffee samples according to their continent of origin. When samples from each continent were considered separately, up to 100% correct classification of coffee samples into their countries, and plantations of origin was achieved. This research demonstrates the potential of using elemental composition, in combination with statistical classification methods, for accurate provenance establishment of coffee. Copyright © 2013 Elsevier Ltd. All rights reserved.

Simultaneous quantification of 17 trace elements in blood by dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS) equipped with a high-efficiency sample introduction system.

PubMed

D'Ilio, S; Violante, N; Di Gregorio, M; Senofonte, O; Petrucci, F

2006-10-10

A quadrupole inductively coupled plasma mass spectrometer (Q-ICP-MS) equipped with a dynamic reaction cell (DRC) and coupled with a desolvating nebulization system (APEX-IR) was employed to determine 17 elements (Al, As, Ba, Cd, Co, Cr, Li, Mn, Mo, Ni, Pb, Sb, Se, Sn, Sr, V, and Zr) in blood samples. Ammonia (for Al, Cr, Mn, and V) and O2 (for As and Se) were used as reacting gases. Selection of the best flow rate of the gases and optimization of the quadrupole dynamic bandpass tuning parameter (RPq) were carried out, using digested blood diluted 1+9 with deionized water and spiked with 1 microg L(-1) of Al, Cr, Mn, V and 5 microgL(-1) of As and Se. Detection limits were determined in digested blood using the 3sigma criterion. The desolvating system allowed a sufficient sensitivity to be achieved to determine elements at levels of ng L(-1) without detriment of signal stability. The accuracy of the method was tested with the whole blood certified reference material (CRM), certified for Al, As, Cd, Co, Cr, Mn, Mo, Ni, Pb, Sb, Se, and V, and with indicative values for Ba, Li, Sn, Sr, and Zr. The addition calibration approach was chosen for analysis. In order to confirm the DRC data, samples were also analyzed by means of sector field inductively coupled plasma mass spectrometry (SF-ICP-MS), operating in medium (m/Deltam=4000) and high (m/Deltam=10,000) resolution mode and achieving a good agreement between the two techniques.

Si-compatible cleaning process for graphene using low-density inductively coupled plasma.

PubMed

Lim, Yeong-Dae; Lee, Dae-Yeong; Shen, Tian-Zi; Ra, Chang-Ho; Choi, Jae-Young; Yoo, Won Jong

2012-05-22

We report a novel cleaning technique for few-layer graphene (FLG) by using inductively coupled plasma (ICP) of Ar with an extremely low plasma density of 3.5 × 10(8) cm(-3). It is known that conventional capacitively coupled plasma (CCP) treatments destroy the planar symmetry of FLG, giving rise to the generation of defects. However, ICP treatment with extremely low plasma density is able to remove polymer resist residues from FLG within 3 min at a room temperature of 300 K while retaining the carbon sp(2)-bonding of FLG. It is found that the carrier mobility and charge neutrality point of FLG are restored to their pristine defect-free state after the ICP treatment. Considering the application of graphene to silicon-based electronic devices, such a cleaning method can replace thermal vacuum annealing, electrical current annealing, and wet-chemical treatment due to its advantages of being a low-temperature, large-area, high-throughput, and Si-compatible process.

Plasma characteristics of direct current enhanced cylindrical inductively coupled plasma source

NASA Astrophysics Data System (ADS)

Yue, HUA; Jian, SONG; Zeyu, HAO; Chunsheng, REN

2018-06-01

Experimental results of a direct current enhanced inductively coupled plasma (DCE-ICP) source which consists of a typical cylindrical ICP source and a plate-to-grid DC electrode are reported. With the use of this new source, the plasma characteristic parameters, namely, electron density, electron temperature and plasma uniformity, are measured by Langmuir floating double probe. It is found that DC discharge enhances the electron density and decreases the electron temperature, dramatically. Moreover, the plasma uniformity is obviously improved with the operation of DC and radio frequency (RF) hybrid discharge. Furthermore, the nonlinear enhancement effect of electron density with DC + RF hybrid discharge is confirmed. The presented observation indicates that the DCE-ICP source provides an effective method to obtain high-density uniform plasma, which is desirable for practical industrial applications.

Inductively Coupled Plasma Optical Emission Spectrometry for Rare Earth Elements Analysis

NASA Astrophysics Data System (ADS)

He, Man; Hu, Bin; Chen, Beibei; Jiang, Zucheng

2017-01-01

Inductively coupled plasma optical emission spectrometry (ICP-OES) merits multielements capability, high sensitivity, good reproducibility, low matrix effect and wide dynamic linear range for rare earth elements (REEs) analysis. But the spectral interference in trace REEs analysis by ICP-OES is a serious problem due to the complicated emission spectra of REEs, which demands some correction technology including interference factor method, derivative spectrum, Kalman filtering algorithm and partial least-squares (PLS) method. Matrix-matching calibration, internal standard, correction factor and sample dilution are usually employed to overcome or decrease the matrix effect. Coupled with various sample introduction techniques, the analytical performance of ICP-OES for REEs analysis would be improved. Compared with conventional pneumatic nebulization (PN), acid effect and matrix effect are decreased to some extent in flow injection ICP-OES, with higher tolerable matrix concentration and better reproducibility. By using electrothermal vaporization as sample introduction system, direct analysis of solid samples by ICP-OES is achieved and the vaporization behavior of refractory REEs with high boiling point, which can easily form involatile carbides in the graphite tube, could be improved by using chemical modifier, such as polytetrafluoroethylene and 1-phenyl-3-methyl-4-benzoyl-5-pyrazone. Laser ablation-ICP-OES is suitable for the analysis of both conductive and nonconductive solid samples, with the absolute detection limit of ng-pg level and extremely low sample consumption (0.2 % of that in conventional PN introduction). ICP-OES has been extensively employed for trace REEs analysis in high-purity materials, and environmental and biological samples.

Determination of glyphosate and AMPA in surface and waste water using high-performance ion chromatography coupled to inductively coupled plasma dynamic reaction cell mass spectrometry (HPIC-ICP-DRC-MS).

PubMed

Popp, Maximilian; Hann, Stephan; Mentler, Axel; Fuerhacker, Maria; Stingeder, Gerhard; Koellensperger, Gunda

2008-05-01

A novel method employing high-performance cation chromatography in combination with inductively coupled plasma dynamic reaction cell mass spectrometry (ICP-DRC-MS) for the simultaneous determination of the herbicide glyphosate (N-phosphonomethylglycine) and its main metabolite aminomethyl phosphonic acid (AMPA) is presented. P was measured as (31)P(16)O(+) using oxygen as reaction gas. For monitoring the stringent target value of 0.1 μg L(-1) for glyphosate, applicable for drinking and surface water within the EU, a two-step enrichment procedure employing Chelex 100 and AG1-X8 resins was applied prior to HPIC-ICP-MS analysis. The presented approach was validated for surface water, revealing concentrations of 0.67 μg L(-1) glyphosate and 2.8 μg L(-1) AMPA in selected Austrian river water samples. Moreover, investigations at three waste water-treatment plants showed that elimination of the compounds at the present concentration levels was not straightforward. On the contrary, all investigated plant effluents showed significant amounts of both compounds. Concentration levels ranged from 0.5-2 μg L(-1) and 4-14 μg L(-1) for glyphosate and AMPA, respectively.

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

NASA Astrophysics Data System (ADS)

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).

Atlas of Atomic Spectral Lines of Neptunium Emitted by Inductively Coupled Plasma

DOE Office of Scientific and Technical Information (OSTI.GOV)

DeKalb, E.L. and Edelson, M. C.

1987-08-01

Optical emission spectra from high-purity Np-237 were generated with a glovebox-enclosed inductively coupled plasma (ICP) source. Spectra covering the 230-700 nm wavelength range are presented along with general commentary on the methodology used in collecting the data. The Ames Laboratory Nuclear Safeguards and Security Program has been charged with the task of developing optical spectroscopic methods to analyze the composition of spent nuclear fuels. Such materials are highly radioactive even after prolonged 'cooling' and are chemically complex. Neptunium (Np) is a highly toxic by-product of nuclear power generation and is found, in low abundance, in spent nuclear fuels. This atlasmore » of the optical emission spectrum of Np, as produced by an inductively coupled plasma (ICP) spectroscopic source, is part of a general survey of the ICP emission spectra of the actinide elements. The ICP emission spectrum of the actinides originates almost exclusively from the electronic relaxation of excited, singly ionized species. Spectral data on the Np ion emission spectrum (i.e., the Np II spectrum) have been reported by Tomkins and Fred [1] and Haaland [2]. Tomkins and Fred excited the Np II spectrum with a Cu spark discharge and identified 114 Np lines in the 265.5 - 436.3 nm spectral range. Haaland, who corrected some spectral line misidentifications in the work of Tomkins and Fred, utilized an enclosed Au spark discharge to excite the Np II spectrum and reported 203 Np lines within the 265.4 - 461.0 nm wavelength range.« less

The potential of inductively coupled plasma mass spectrometry (ICP-MS) for the simultaneous determination of trace elements in whole blood, plasma and serum.

PubMed

Krachler, M; Irgolic, K J

1999-11-01

The advantages accruing to biochemical and clinical investigations from a method that allows the simultaneous quantification (RSD < or = 10%) of many elements in blood, plasma, and serum at concentrations equal to one-hundredth of the lower limits of the normal ranges are undeniable. The suitability of inductively coupled argon plasma low-resolution quadrupole mass spectrometry (ICP-MS), a simultaneous method with low detection limits, is evaluated for the quantification of inorganic constituents in whole blood, plasma, and serum with consideration of the dilution associated with the mineralization of the samples, of isobaric and polyatomic interferences and of normal ranges. Of the 3 bulk elements, the 3 major electrolytes, the 15 essential elements, the 8 toxic elements, the 4 therapeutic elements, and the 14 elements of potential interest (total of 47 elements) only 7 elements (Ca, Cu, K, Mg, Rb, Sr, Zn) can be simultaneously quantified under these rigorous conditions in serum and only 8 elements (additional element Pb) in whole blood. Quantification of elements in the Seronorm Standards "Whole Blood" and "Serum" showed, that this list of simultaneously determinable elements in these matrices is reasonable. Although this list is disappointingly short, the number of elements determinable simultaneously by ICP-MS is still larger than that by ICP-AES or GFAAS. Improved detectors, more efficient nebulizers, avoidance of interferences, better instrument design, and high-resolution mass spectrometers promise to increase the number of elements that can be determined simultaneously.

Use of a parallel path nebulizer for capillary-based microseparation techniques coupled with an inductively coupled plasma mass spectrometer for speciation measurements

NASA Astrophysics Data System (ADS)

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

2004-06-01

A low flow, parallel path Mira Mist CE nebulizer designed for capillary electrophoresis (CE) was evaluated as a function of make-up solution flow rate, composition, and concentration, as well as the nebulizer gas flow rate. This research was conducted in support of a project related to the separation and quantification of cobalamin (vitamin B-12) species using microseparation techniques combined with inductively coupled plasma mass spectrometry (ICP-MS) detection. As such, Co signals were monitored during the nebulizer characterization process. Transient effects in the ICP were studied to evaluate the suitability of using gradients for microseparations and the benefit of using methanol for the make-up solution was demonstrated. Co signal response changed significantly as a function of changing methanol concentrations of the make-up solution and maximum signal enhancement was seen at 20% methanol with a 15 μl/min flow rate. Evaluation of the effect of changing the nebulizer gas flow rates showed that argon flows from 0.8 to 1.2 l/min were equally effective. The Mira Mist CE parallel path nebulizer was then evaluated for interfacing capillary microseparation techniques including capillary electrophoresis (CE) and micro high performance liquid chromatography (μHPLC) to inductively coupled plasma mass spectrometry (ICP-MS). A mixture of four cobalamin species standards (cyanocobalamin, hydroxocobalamin, methylcobalamin, and 5' deoxyadenosylcobalamin) and the corrinoid analogue cobinamide dicyanide were successfully separated using both CE-ICP-MS and μHPLC-ICP-MS using the parallel path nebulizer with a make-up solution containing 20% methanol with a flow rate of 15 μl/min.

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

NASA Astrophysics Data System (ADS)

Vašinová Galiová, Michaela; Čopjaková, Renata; Škoda, Radek; Štěpánková, Kateřina; Vaňková, Michaela; Kuta, Jan; Prokeš, Lubomír; Kynický, Jindřich; Kanický, Viktor

2014-10-01

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

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

PubMed Central

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

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

USGS Publications Warehouse

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.

Imaging Metals in Brain Tissue by Laser Ablation - Inductively Coupled Plasma - Mass Spectrometry (LA-ICP-MS)

PubMed Central

Hare, Dominic J.; Kysenius, Kai; Paul, Bence; Knauer, Beate; Hutchinson, Robert W.; O'Connor, Ciaran; Fryer, Fred; Hennessey, Tom P.; Bush, Ashley I.; Crouch, Peter J.; Doble, Philip A.

2017-01-01

Metals are found ubiquitously throughout an organism, with their biological role dictated by both their chemical reactivity and abundance within a specific anatomical region. Within the brain, metals have a highly compartmentalized distribution, depending on the primary function they play within the central nervous system. Imaging the spatial distribution of metals has provided unique insight into the biochemical architecture of the brain, allowing direct correlation between neuroanatomical regions and their known function with regard to metal-dependent processes. In addition, several age-related neurological disorders feature disrupted metal homeostasis, which is often confined to small regions of the brain that are otherwise difficult to analyze. Here, we describe a comprehensive method for quantitatively imaging metals in the mouse brain, using laser ablation - inductively coupled plasma - mass spectrometry (LA-ICP-MS) and specially designed image processing software. Focusing on iron, copper and zinc, which are three of the most abundant and disease-relevant metals within the brain, we describe the essential steps in sample preparation, analysis, quantitative measurements and image processing to produce maps of metal distribution within the low micrometer resolution range. This technique, applicable to any cut tissue section, is capable of demonstrating the highly variable distribution of metals within an organ or system, and can be used to identify changes in metal homeostasis and absolute levels within fine anatomical structures. PMID:28190025

External control of electron energy distributions in a dual tandem inductively coupled plasma

NASA Astrophysics Data System (ADS)

Liu, Lei; Sridhar, Shyam; Zhu, Weiye; Donnelly, Vincent M.; Economou, Demetre J.; Logue, Michael D.; Kushner, Mark J.

2015-08-01

The control of electron energy probability functions (EEPFs) in low pressure partially ionized plasmas is typically accomplished through the format of the applied power. For example, through the use of pulse power, the EEPF can be modulated to produce shapes not possible under continuous wave excitation. This technique uses internal control. In this paper, we discuss a method for external control of EEPFs by transport of electrons between separately powered inductively coupled plasmas (ICPs). The reactor incorporates dual ICP sources (main and auxiliary) in a tandem geometry whose plasma volumes are separated by a grid. The auxiliary ICP is continuously powered while the main ICP is pulsed. Langmuir probe measurements of the EEPFs during the afterglow of the main ICP suggests that transport of hot electrons from the auxiliary plasma provided what is effectively an external source of energetic electrons. The tail of the EEPF and bulk electron temperature were then elevated in the afterglow of the main ICP by this external source of power. Results from a computer simulation for the evolution of the EEPFs concur with measured trends.

Determination of the rare-earth elements in geological materials by inductively coupled plasma mass spectrometry

USGS Publications Warehouse

Lichte, F.E.; Meier, A.L.; Crock, J.G.

1987-01-01

A method of analysis of geological materials for the determination of the rare-earth elements using the Inductively coupled plasma mass spectrometric technique (ICP-MS) has been developed. Instrumental parameters and factors affecting analytical results have been first studied and then optimized. Samples are analyzed directly following an acid digestion, without the need for separation or preconcentration with limits of detection of 2-11 ng/g, precision of ?? 2.5% relative standard deviation, and accuracy comparable to inductively coupled plasma emission spectrometry and instrumental neutron activation analysis. A commercially available ICP-MS instrument is used with modifications to the sample introduction system, torch, and sampler orifice to reduce the effects of high salt content of sample solutions prepared from geologic materials. Corrections for isobaric interferences from oxide ions and other diatomic and triatomic ions are made mathematically. Special internal standard procedures are used to compensate for drift in metahmetal oxide ratios and sensitivity. Reference standard values are used to verify the accuracy and utility of the method.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ebert, Christopher Hysjulien

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 thatmore » 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.« less

Development and Validation of an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Method for Quantitative Analysis of Platinum in Plasma, Urine, and Tissues.

PubMed

Zhang, Ti; Cai, Shuang; Forrest, Wai Chee; Mohr, Eva; Yang, Qiuhong; Forrest, M Laird

2016-09-01

Cisplatin, a platinum chemotherapeutic, is one of the most commonly used chemotherapeutic agents for many solid tumors. In this work, we developed and validated an inductively coupled plasma mass spectrometry (ICP-MS) method for quantitative determination of platinum levels in rat urine, plasma, and tissue matrices including liver, brain, lungs, kidney, muscle, heart, spleen, bladder, and lymph nodes. The tissues were processed using a microwave accelerated reaction system (MARS) system prior to analysis on an Agilent 7500 ICP-MS. According to the Food and Drug Administration guidance for industry, bioanalytical validation parameters of the method, such as selectivity, accuracy, precision, recovery, and stability were evaluated in rat biological samples. Our data suggested that the method was selective for platinum without interferences caused by other presenting elements, and the lower limit of quantification was 0.5 ppb. The accuracy and precision of the method were within 15% variation and the recoveries of platinum for all tissue matrices examined were determined to be 85-115% of the theoretical values. The stability of the platinum-containing solutions, including calibration standards, stock solutions, and processed samples in rat biological matrices was investigated. Results indicated that the samples were stable after three cycles of freeze-thaw and for up to three months. © The Author(s) 2016.

Development and Validation of an Inductively Coupled Plasma Mass Spectrometry (ICP-MS) Method for Quantitative Analysis of Platinum in Plasma, Urine, and Tissues

PubMed Central

Zhang, Ti; Cai, Shuang; Forrest, Wai Chee; Mohr, Eva; Yang, Qiuhong; Forrest, M. Laird

2016-01-01

Cisplatin, a platinum chemotherapeutic, is one of the most commonly used chemotherapeutic agents for many solid tumors. In this work, we developed and validated an inductively coupled plasma mass spectrometry (ICP-MS) method for quantitative determination of platinum levels in rat urine, plasma, and tissue matrices including liver, brain, lungs, kidney, muscle, heart, spleen, bladder, and lymph nodes. The tissues were processed using a microwave accelerated reaction system (MARS) system prior to analysis on an Agilent 7500 ICP-MS. According to the Food and Drug Administration guidance for industry, bioanalytical validation parameters of the method, such as selectivity, accuracy, precision, recovery, and stability were evaluated in rat biological samples. Our data suggested that the method was selective for platinum without interferences caused by other presenting elements, and the lower limit of quantification was 0.5 ppb. The accuracy and precision of the method were within 15% variation and the recoveries of platinum for all tissue matrices examined were determined to be 85–115% of the theoretical values. The stability of the platinum-containing solutions, including calibration standards, stock solutions, and processed samples in rat biological matrices was investigated. Results indicated that the samples were stable after three cycles of freeze–thaw and for up to three months. PMID:27527103

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

NASA Astrophysics Data System (ADS)

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.

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

PubMed

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

2015-01-15

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

Statistical evaluation of an inductively coupled plasma atomic emission spectrometric method for routine water quality testing

USGS Publications Warehouse

Garbarino, J.R.; Jones, B.E.; Stein, G.P.

1985-01-01

In an interlaboratory test, inductively coupled plasma atomic emission spectrometry (ICP-AES) was compared with flame atomic absorption spectrometry and molecular absorption spectrophotometry for the determination of 17 major and trace elements in 100 filtered natural water samples. No unacceptable biases were detected. The analysis precision of ICP-AES was found to be equal to or better than alternative methods. Known-addition recovery experiments demonstrated that the ICP-AES determinations are accurate to between plus or minus 2 and plus or minus 10 percent; four-fifths of the tests yielded average recoveries of 95-105 percent, with an average relative standard deviation of about 5 percent.

Fluorescence quenching and the "ring-mode" to "red-mode" transition in alkali inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Huang, M.; Bazurto, R.; Camparo, J.

2018-01-01

The ring-mode to red-mode transition in alkali metal inductively coupled plasmas (ICPs) (i.e., rf-discharge lamps) is perhaps the most important physical phenomenon affecting these devices as optical pumping light sources for atomic clocks and magnetometers. It sets the limit on useful ICP operating temperature, thereby setting a limit on ICP light output for atomic-clock/magnetometer signal generation, and it is a temperature region of ICP operation associated with discharge instability. Previous work has suggested that the mechanism driving the ring-mode to red-mode transition is associated with radiation trapping, but definitive experimental evidence validating that hypothesis has been lacking. Based on that hypothesis, one would predict that the introduction of an alkali-fluorescence quenching gas (i.e., N2) into the ICP would increase the ring-mode to red-mode transition temperature. Here, we test that prediction, finding direct evidence supporting the radiation-trapping hypothesis.

Boron detection from blood samples by ICP-AES and ICP-MS during boron neutron capture therapy.

PubMed

Linko, S; Revitzer, H; Zilliacus, R; Kortesniemi, M; Kouri, M; Savolainen, S

2008-01-01

The concept of boron neutron capture therapy (BNCT) involves infusion of a (10)B containing tracer into the patient's bloodstream followed by local neutron irradiation(s). Accurate estimation of the blood boron level for the treatment field before irradiation is required. Boron concentration can be quantified by inductively coupled plasma atomic emission spectrometry (ICP-AES), mass spectrometry (ICP-MS), spectrofluorometric and direct current atomic emission spectrometry (DCP-AES) or by prompt gamma photon detection methods. The blood boron concentrations were analysed and compared using ICP-AES and ICP-MS to ensure congruency of the results if the analysis had to be changed during the treatment, e.g. for technical reasons. The effect of wet-ashing on the results was studied in addition. The mean of all samples analysed with ICP-MS was 5.8 % lower than with ICP-AES coupled to wet-ashing (R (2) = 0.88). Without wet-ashing, the mean of all samples analysed with ICP-MS was 9.1 % higher than with ICP-AES (R (2) = 0.99). Boron concentration analysed from whole blood samples with ICP-AES correlated well with the values of ICP-MS with wet-ashing of the sample matrix, which is generally considered the reference method. When using these methods in parallel at certain intervals during the treatments, reliability of the blood boron concentration values remains satisfactory, taking into account the required accuracy of dose determination in the irradiation of cancer patients.

A study of GaN-based LED structure etching using inductively coupled plasma

NASA Astrophysics Data System (ADS)

Wang, Pei; Cao, Bin; Gan, Zhiyin; Liu, Sheng

2011-02-01

GaN as a wide band gap semiconductor has been employed to fabricate optoelectronic devices such as light-emitting diodes (LEDs) and laser diodes (LDs). Recently several different dry etching techniques for GaN-based materials have been developed. ICP etching is attractive because of its superior plasma uniformity and strong controllability. Most previous reports emphasized on the ICP etching characteristics of single GaN film. In this study dry etching of GaN-based LED structure was performed by inductively coupled plasmas (ICP) etching with Cl2 as the base gas and BCl3 as the additive gas. The effects of the key process parameters such as etching gases flow rate, ICP power, RF power and chamber pressure on the etching properties of GaN-based LED structure including etching rate, selectivity, etched surface morphology and sidewall was investigated. Etch depths were measured using a depth profilometer and used to calculate the etch rates. The etch profiles were observed with a scanning electron microscope (SEM).

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.

PubMed

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.

Differentiating the Bishop ash bed and related tephra layers by elemental-based similarity coefficients of volcanic glass shards using solution inductively coupled plasma-mass spectrometry (S-ICP-MS)

USGS Publications Warehouse

Knott, J.R.; Sarna-Wojcicki, A. M.; Montanez, I.P.; Wan, E.

2007-01-01

Volcanic glass samples from the same volcanic center (intra-source) often have a similar major-element composition. Thus, it can be difficult to distinguish between individual tephra layers, particularly when using similarity coefficients calculated from electron microprobe major-element measurements. Minor/trace element concentrations in glass can be determined by solution inductively coupled plasma mass spectrometry (S-ICP-MS), but have not been shown as suitable for use in large tephrochronologic databases. Here, we present minor/trace-element concentrations measured by S-ICP-MS and compare these data by similarity coefficients, the method commonly used in large databases. Trial samples from the Bishop Tuff, the upper and lower tuffs of Glass Mountain and the tuffs of Mesquite Spring suites from eastern California, USA, which have an indistinguishable major-element composition, were analyzed using S-ICP-MS. The resulting minor/trace element similarity coefficients clearly separated the suites of tephra layers and, in most cases, individual tephra layers within each suite. Comparisons with previous instrumental neutron activation analysis (INAA) elemental measurements were marginally successful. This is important step toward quantitative correlation in large tephrochronologic databases to achieve definitive identification of volcanic glass samples and for high-resolution age determinations. ?? 2007 Elsevier Ltd and INQUA.

Inductively coupled plasma mass spectrometry and electrospray mass spectrometry for speciation analysis: applications and instrumentation

NASA Astrophysics Data System (ADS)

Rosen, Amy L.; Hieftje, Gary M.

2004-02-01

To gain an understanding of the function, toxicity and distribution of trace elements, it is necessary to determine not only the presence and concentration of the elements of interest, but also their speciation, by identifying and characterizing the compounds within which each is present. For sensitive detection of compounds containing elements of interest, inductively coupled plasma mass spectrometry (ICP-MS) is a popular method, and for identification of compounds via determination of molecular weight, electrospray ionization mass spectrometry (ESI-MS) is gaining increasing use. ICP-MS and ESI-MS, usually coupled to a separation technique such as chromatography or capillary electrophoresis, have already been applied to a large number of research problems in such diverse fields as environmental chemistry, nutritional science, and bioinorganic chemistry, but a great deal of work remains to be completed. Current areas of research to which ICP-MS and ESI-MS have been applied are discussed, and the existing instrumentation used to solve speciation problems is described.

Surface Modification of Polyimide for Improving Adhesion Strength by Inductively Coupled Plasma

NASA Astrophysics Data System (ADS)

Byun, Tae Joon; Kim, Sung Il; Kim, Youn Joon; Choi, Yoon Suk; Choi, In Sik; Setsuhara, Yuichi; Geon Han, Jeon

2009-08-01

This study examined the effect of an inductively coupled plasma (ICP) treatment using an argon and helium gas mixture on the adhesion between polyimide and a copper film. Optical emission spectroscopy (OES) of the ICP revealed the emission intensity of helium and argon at various intensities with the helium mixing ratio. The treated polyimide surface was analyzed using a contact angle analyzer, Atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The contact angle and RMS roughness ranged from 66 to 31° and 2.3 to 4.1 nm, respectively. XPS showed an increase in C-O bonding. The highest peel strength was 0.43 kgf/cm at a 40% of helium mixing ratio, which contained the highest level of activate species. Overall, an ICP treatment of a polyimide surface with a 40% helium gas mixture improves the adhesion strength between copper and polyimide significantly.

Observation of collisionless heating of low energy electrons in low pressure inductively coupled argon plasmas

NASA Astrophysics Data System (ADS)

Lee, Min-Hyong; Lee, Hyo-Chang; Chung, Chin-Wook

2008-12-01

Collisionless heating of low energy electrons was observed in low pressure argon rf-biased inductively coupled plasmas (ICPs) by measurement of the electron energy distribution function (EEDF). When only capacitive power (bias) was supplied, the EEDF in the discharge was a bi-Maxwellian distribution with two electron groups. It was found that the low energy electrons were heated up significantly even with a little inductive power (<20 W) even when the discharge was in E mode. Due to the low gas pressure and low temperature of low energy electrons (close to the energy of the Ramsauer minimum), the collisional heating of low energy electrons appears to be negligible. Therefore, this effective heating of the low energy electrons showed a direct experimental evidence of the collisionless heating by inductive field. The significant heating of low energy electrons in E mode indicates that collisionless heating in the skin layer is an important electron heating mechanism of low pressure ICP even when the discharge is in E mode.

Challenges in the quality assurance of elemental and isotopic analyses in the nuclear domain benefitting from high resolution ICP-OES and sector field ICP-MS.

PubMed

Krachler, Michael; Alvarez-Sarandes, Rafael; Van Winckel, Stefaan

Accurate analytical data reinforces fundamentally the meaningfulness of nuclear fuel performance assessments and nuclear waste characterization. Regularly lacking matrix-matched certified reference materials, quality assurance of elemental and isotopic analysis of nuclear materials remains a challenging endeavour. In this context, this review highlights various dedicated experimental approaches envisaged at the European Commission-Joint Research Centre-Institute for Transuranium Elements to overcome this limitation, mainly focussing on the use of high resolution-inductively coupled plasma-optical emission spectrometry (HR-ICP-OES) and sector field-inductively coupled plasma-mass spectrometry (SF-ICP-MS). However, also α- and γ-spectrometry are included here to help characterise extensively the investigated actinide solutions for their actual concentration, potential impurities and isotopic purity.

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

ERIC Educational Resources Information Center

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

2016-01-01

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

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.

PubMed

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

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(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. Copyright © 2015 Elsevier B.V. All rights reserved.

Direct determination of lead in biological samples by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) after furnace-fusion in the sample cuvette-tungsten boat furnace.

PubMed

Okamoto, Y

2000-06-01

The newly conceived electrothermal vaporization (ETV) system using a tungsten boat furnace (TBF) sample cuvette was designed for the direct analysis of solid samples with detection by inductively coupled plasma mass spectrometry (ICP-MS). Into this small sample cuvette, a solid mixture of the biological samples and diammonium hydrogenphosphate powder as a fusion flux was placed and situated on a TBF. Tetramethylammonium hydroxide solution was added to the mixture. After the on-furnace digestion had been completed, the analyte in the cuvette was vaporized and introduced into the ICP mass spectrometer. The solid samples were analyzed by using a calibration curve prepared from the aqueous standard solutions. The detection limit was estimated to be 5.1 pg of lead, which corresponds to 10.2 ng g(-1) of lead in solid samples when a prepared sample amount of 1.0 mg was applied. The relative standard deviation for 8 replicate measurements obtained with 100 pg of lead was calculated to be 6.5%. The analytical results for various biological samples are described.

Determination of arsenic in traditional Chinese medicine by microwave digestion with flow injection-inductively coupled plasma mass spectrometry (FI-ICP-MS).

PubMed

Ong, E S; Yong, Y L; Woo, S O

1999-01-01

A simple, rapid, and sensitive method with high sample throughput was developed for determining arsenic in traditional Chinese medicine (TCM) in the form of uncoated tablets, sugar-coated tablets, black pills, capsules, powders, and syrups. The method involves microwave digestion with flow injection-inductively coupled plasma mass spectrometry (FI-ICP-MS). Method precision was 2.7-10.1% (relative standard deviation, n = 6) for different concentrations of arsenic in different TCM samples analyzed by different analysts on different days. Method accuracy was checked with a certified reference material (sea lettuce, Ulva lactuca, BCR CRM 279) for external calibration and by spiking arsenic standard into different TCMs. Recoveries of 89-92% were obtained for the certified reference material and higher than 95% for spiked TCMs. Matrix interference was insignificant for samples analyzed by the method of standard addition. Hence, no correction equation was used in the analysis of arsenic in the samples studied. Sample preparation using microwave digestion gave results that were very similar to those obtained by conventional wet acid digestion using nitric acid.

Application of isotope dilution inductively coupled plasma mass spectrometry to the analysis of marine sediments

DOE Office of Scientific and Technical Information (OSTI.GOV)

McLaren, J.W.; Beauchemin, D.; Berman, S.S.

1987-02-15

Isotope dilution inductively coupled plasma mass spectrometry (ICP-MS) has been applied to the determination of 11 trace elements (Cr, Ni, Zn, Sr, Mo, Cd, Sn, Sb, Tl, Pb, and U) in the marine sediment reference materials MESS-1 and BCSS-1. Accuracy and, especially, precision are better than those that can be easily achieved by other ICP-MS calibration strategies, as long as isotopic equilibration is achieved and the isotopes used for the ratio measurement are free of isobaric interferences by molecular species. The measurement of the isotope ratios on unspiked samples provides a sensitive diagnostic of such interferences.

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

USGS Publications Warehouse

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

2014-01-01

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

Laser ablation inductively coupled plasma mass spectrometry for direct isotope ratio measurements on solid samples

NASA Astrophysics Data System (ADS)

Pickhardt, Carola; Dietze, Hans-Joachim; Becker, J. Sabine

2005-04-01

Isotope ratio measurements have been increasingly used in quite different application fields, e.g., for the investigation of isotope variation in nature, in geoscience (geochemistry and geochronology), in cosmochemistry and planetary science, in environmental science, e.g., in environmental monitoring, or by the application of the isotope dilution technique for quantification purposes using stable or radioactive high-enriched isotope tracers. Due to its high sensitivity, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) is today a challenging mass spectrometric technique for the direct determination of precise and accurate isotope ratios in solid samples. In comparison to laser ablation quadrupole ICP-MS (LA-ICP-QMS), laser ablation coupled to a double-focusing sector field ICP-MS (LA-ICP-SFMS) with single ion detection offers a significant improvement of sensitivity at low mass resolution, whereby isotope ratios can be measured with a precision to 0.1% relative standard deviation (R.S.D.). In LA-ICP-SFMS, many disturbing isobaric interferences of analyte and molecular ions can be separated at the required mass resolution (e.g., 40Ar16O+ and 56Fe+ for iron isotope ratio measurements). The precision on isotope ratio measurements was improved by one order of magnitude via the simultaneous detection of mass-separated ion currents of isotopes using multiple ion collectors in LA-ICP-MS (LA-MC-ICP-MS). The paper discusses the state of the art, the challenges and limits in isotope ratio measurements by LA-ICP-MS using different instrumentations at the trace and ultratrace level in different fields of application as in environmental and biological research, geochemistry and geochronology with respect to their precision and accuracy.

High-Resolution Inductively Coupled Plasma Optical Emission Spectrometry for (234)U/(238)Pu Age Dating of Plutonium Materials and Comparison to Sector Field Inductively Coupled Plasma Mass Spectrometry.

PubMed

Krachler, Michael; Alvarez-Sarandes, Rafael; Rasmussen, Gert

2016-09-06

Employing a commercial high-resolution inductively coupled plasma optical emission spectrometry (HR-ICP-OES) instrument, an innovative analytical procedure for the accurate determination of the production age of various Pu materials (Pu powder, cardiac pacemaker battery, (242)Cm heat source, etc.) was developed and validated. This undertaking was based on the fact that the α decay of (238)Pu present in the investigated samples produced (234)U and both mother and daughter could be identified unequivocally using HR-ICP-OES. Benefiting from the high spectral resolution of the instrument (<5 pm) and the isotope shift of the emission lines of both nuclides, (234)U and (238)Pu were selectively and directly determined in the dissolved samples, i.e., without a chemical separation of the two analytes from each other. Exact emission wavelengths as well as emission spectra of (234)U centered around λ = 411.590 nm and λ = 424.408 nm are reported here for the first time. Emission spectra of the isotopic standard reference material IRMM-199, comprising about one-third each of (233)U, (235)U, and (238)U, confirmed the presence of (234)U in the investigated samples. For the assessment of the (234)U/(238)Pu amount ratio, the emission signals of (234)U and (238)Pu were quantified at λ = 424.408 nm and λ = 402.148 nm, respectively. The age of the investigated samples (range: 26.7-44.4 years) was subsequently calculated using the (234)U/(238)Pu chronometer. HR-ICP-OES results were crossed-validated through sector field inductively coupled plasma mass spectrometry (SF-ICPMS) analysis of the (234)U/(238)Pu amount ratio of all samples applying isotope dilution combined with chromatographic separation of U and Pu. Available information on the assumed ages of the analyzed samples was consistent with the ages obtained via the HR-ICP-OES approach. Being based on a different physical detection principle, HR-ICP-OES provides an alternative strategy to the well-established mass

Precise ruthenium fission product isotopic analysis using dynamic reaction cell inductively coupled plasma mass spectrometry (DRC-ICP-MS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Brown, Christopher F.; Dresel, P. Evan; Geiszler, Keith N.

2006-05-09

99Tc is a subsurface contaminant of interest at numerous federal, industrial, and international facilities. However, as a mono-isotopic fission product, 99Tc lacks the ability to be used as a signature to differentiate between the different waste disposal pathways that could have contributed to subsurface contamination at these facilities. Ruthenium fission-product isotopes are attractive analogues for the characterization of 99Tc sources because of their direct similarity to technetium with regard to subsurface mobility, and their large fission yields and low natural background concentrations. We developed an inductively coupled plasma mass spectrometry (ICP-MS) method capable of measuring ruthenium isotopes in groundwater samplesmore » and extracts of vadose zone sediments. Samples were analyzed directly on a Perkin Elmer ELAN DRC II ICP-MS after a single pass through a 1-ml bed volume of Dowex AG 50W-X8 100-200 mesh cation exchange resin. Precise ruthenium isotopic ratio measurements were achieved using a low-flow Meinhard-type nebulizer and long sample acquisition times (150,000 ms). Relative standard deviations of triplicate replicates were maintained at less than 0.5% when the total ruthenium solution concentration was 0.1 ng/ml or higher. Further work was performed to minimize the impact caused by mass interferences using the dynamic reaction cell (DRC) with O2 as the reaction gas. The aqueous concentrations of 96Mo and 96Zr were reduced by more than 99.7% in the reaction cell prior to injection of the sample into the mass analyzer quadrupole. The DRC was used in combination with stable-mass correction to quantitatively analyze samples containing up to 2-orders of magnitude more zirconium and molybdenum than ruthenium. The analytical approach documented herein provides an efficient and cost-effective way to precisely measure ruthenium isotopes and quantitate total ruthenium (natural vs. fission-product) in aqueous matrixes.« less

A comparison of lead-isotope measurements on exploration-type samples using inductively coupled plasma and thermal ionization mass spectrometry

USGS Publications Warehouse

Gulson, B.L.; Meier, A.L.; Church, S.E.; Mizon, K.J.

1989-01-01

Thermal ionization mass spectrometry (TI-MS) has long been the method of choice for Pb-isotope determinations. More recently, however, inductively coupled plasma mass spectrometry (ICP-MS) has been used to determine Pb-isotope ratios for mineral exploration. The ICP-MS technique, although not as precise as TI-MS, may promote a wider application of Ph-isotope ratio methods because it allows individual isotopes to be determined more rapidly, generally without need for chemical separation (e.g., Smith et al., 1984; Hinners et al., 1987). To demonstrate the utility of the ICP-MS method, we have conducted a series of Pb-isotope measurements on several suites of samples using both TI-MS and ICP-MS. ?? 1989.

Iron-Isotopic Fractionation Studies Using Multiple Collector Inductively Coupled Plasma Mass Spectrometry

NASA Technical Reports Server (NTRS)

Anbar, A. D.; Zhang, C.; Barling, J.; Roe, J. E.; Nealson, K. H.

1999-01-01

The importance of Fe biogeochemistry has stimulated interest in Fe isotope fractionation. Recent studies using thermal ionization mass spectrometry (TIMS) and a "double spike" demonstrate the existence of biogenic Fe isotope effects. Here, we assess the utility of multiple-collector inductively-coupled plasma mass spectrometry(MC-ICP-MS) with a desolvating sample introduction system for Fe isotope studies, and present data on Fe biominerals produced by a thermophilic bacterium. Additional information is contained in the original extended abstract.

Inductively coupled plasma mass spectrometry for stable isotope metabolic tracer studies of living systems

DOE Office of Scientific and Technical Information (OSTI.GOV)

Luong, Elise

1999-05-10

This dissertation focuses on the development of methods for stable isotope metabolic tracer studies in living systems using inductively coupled plasma single and dual quadrupole mass spectrometers. Sub-nanogram per gram levels of molybdenum (Mo) from human blood plasma are isolated by the use of anion exchange alumina microcolumns. Million-fold more concentrated spectral and matrix interferences such as sodium, chloride, sulfate, phosphate, etc. in the blood constituents are removed from the analyte. The recovery of Mo from the alumina column is 82 ± 5% (n = 5). Isotope dilution inductively coupled plasma mass spectrometry (ID-ICP-MS) is utilized for the quantitative ultra-tracemore » concentration determination of Mo in bovine and human blood samples. The average Mo concentration in reference bovine serum determined by this method is 10.2 ± 0.4 ng/g, while the certified value is 11.5 ± 1.1 ng/g (95% confidence interval). The Mo concentration of one pool of human blood plasma from two healthy male donors is 0.5 ± 0.1 ng/g. The inductively coupled plasma twin quadrupole mass spectrometer (ICP-TQMS) is used to measure the carbon isotope ratio from non-volatile organic compounds and bio-organic molecules to assess the ability as an alternative analytical method to gas chromatography combustion isotope ratio mass spectrometry (GC-combustion-IRMS). Trytophan, myoglobin, and β-cyclodextrin are chosen for the study, initial observation of spectral interference of 13C + with 12C 1H + comes from the incomplete dissociation of myoglobin and/or β-cyclodextrin.« less

Invention of the Annular Inductively Coupled Plasma as a Spectroscopic Source

NASA Astrophysics Data System (ADS)

Greenfield, Stanley

2000-05-01

This paper shows how experiments with electrical discharges from the 18th century onward led to their use as sources in atomic spectroscopy and how the invention of the annular inductively coupled plasma (ICP) some 30 years ago arose from the need to solve a problem that necessitated the use of a high-temperature source. The search for such a source followed a fairly logical pattern involving dc plasma jets and an ICP such as had been used by T. B. Reed for crystal growing. The ellipsoidal plasma used by Reed was not entirely suitable as a spectroscopic source, since the analytical sample either mixed with the plasma gases or passed around the plasma, resulting in matrix effects and a diminution in the emission. It is shown how suitable modification of the plasma torch with attention to gas flows made it possible to produce an annular or tunnel plasma through which the sample aerosol could be passed, resulting in an annular ICP with greatly improved spectroscopic properties. The further refinements to the source and ancillary equipment are also discussed.

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

PubMed

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.

Comparative performance study of different sample introduction techniques for rapid and precise selenium isotope ratio determination using multi-collector inductively coupled plasma mass spectrometry (MC-ICP/MS).

PubMed

Elwaer, Nagmeddin; Hintelmann, Holger

2007-11-01

The analytical performance of five sample introduction systems, a cross flow nebulizer spray chamber, two different solvent desolvation systems, a multi-mode sample introduction system (MSIS), and a hydride generation (LI2) system were compared for the determination of Se isotope ratio measurements using multi-collector inductively coupled plasma mass spectrometry (MC-ICP/MS). The optimal operating parameters for obtaining the highest Se signal-to-noise (S/N) ratios and isotope ratio precision for each sample introduction were determined. The hydride generation (LI2) system was identified as the most suitable sample introduction method yielding maximum sensitivity and precision for Se isotope ratio measurement. It provided five times higher S/N ratios for all Se isotopes compared to the MSIS, 20 times the S/N ratios of both desolvation units, and 100 times the S/N ratios produced by the conventional spray chamber sample introduction method. The internal precision achieved for the (78)Se/(82)Se ratio at 100 ng mL(-1) Se with the spray chamber, two desolvation, MSIS, and the LI2 systems coupled to MC-ICP/MS was 150, 125, 114, 13, and 7 ppm, respectively. Instrument mass bias factors (K) were calculated using an exponential law correction function. Among the five studied sample introduction systems the LI2 showed the lowest mass bias of -0.0265 and the desolvation system showed the largest bias with -0.0321.

Determination of Metal Levels in Shamma (Smokeless Tobacco) with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) in Najran, Saudi Arabia

PubMed

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 < 0.05) among Shamma types. Moreover, Pb levels are higher in red and yellow Shamma, which could be due to use (PbCrO4) as yellow colouring agent and lead tetroxide, Pb3O4 as a red colouring agent. The findings from this study can be used to raise public awareness about the safety and health effects of Shamma, which is clearly a source of oral exposure to metals. Creative Commons Attribution License

Phosphorus doped graphene by inductively coupled plasma and triphenylphosphine treatments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shin, Dong-Wook, E-mail: shindong37@skku.edu; Kim, Tae Sung; Yoo, Ji-Beom, E-mail: jbyoo@skku.edu

Highlights: • Substitution doping is a promising method for opening the energy band gap of graphene. • Substitution doping with phosphorus in the graphene lattice has numerous advantage such as high band gap, low formation energy, and high net charge density compared to nitrogen. • V{sub dirac} of Inductively coupled plasma (ICP) and triphenylphosphine (TPP) treated graphene was −57 V, which provided clear evidence of n-type doping. • Substitutional doping of graphene with phosphorus is verified by the XPS spectra of P 2p core level and EELS mapping of phosphorus. • The chemical bonding between P and graphene is verymore » stable for a long time in air (2 months). - Abstract: Graphene is considered a host material for various applications in next-generation electronic devices. However, despite its excellent properties, one of the most important issues to be solved as an electronic material is the creation of an energy band gap. Substitution doping is a promising method for opening the energy band gap of graphene. Herein, we demonstrate the substitutional doping of graphene with phosphorus using inductively coupled plasma (ICP) and triphenylphosphine (TPP) treatments. The electrical transfer characteristics of the phosphorus doped graphene field effect transistor (GFET) have a V{sub dirac} of ∼ − 54 V. The chemical bonding between P and C was clearly observed in XPS spectra, and uniform distribution of phosphorus within graphene domains was confirmed by EELS mapping. The capability for substitutional doping of graphene with phosphorus can significantly promote the development of graphene based electronic devices.« less

Effects of Inductively Coupled Plasma Hydrogen on Long-Wavelength Infrared HgCdTe Photodiodes

NASA Astrophysics Data System (ADS)

Boieriu, P.; Buurma, C.; Bommena, R.; Blissett, C.; Grein, C.; Sivananthan, S.

2013-12-01

Bulk passivation of semiconductors with hydrogen continues to be investigated for its potential to improve device performance. In this work, hydrogen-only inductively coupled plasma (ICP) was used to incorporate hydrogen into long-wavelength infrared HgCdTe photodiodes grown by molecular-beam epitaxy. Fully fabricated devices exposed to ICP showed statistically significant increases in zero-bias impedance values, improved uniformity, and decreased dark currents. HgCdTe photodiodes on Si substrates passivated with amorphous ZnS exhibited reductions in shunt currents, whereas devices on CdZnTe substrates passivated with polycrystalline CdTe exhibited reduced surface leakage, suggesting that hydrogen passivates defects in bulk HgCdTe and in CdTe.

Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry

PubMed Central

Ornatsky, Olga I.; Kinach, Robert; Bandura, Dmitry R.; Lou, Xudong; Tanner, Scott D.; Baranov, Vladimir I.; Nitz, Mark; Winnik, Mitchell A.

2008-01-01

Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for elemental tagging of antibodies, immunostaining of live and fixed human leukemia cells, and preparation of samples for ICP-MS analysis. Quantitative analysis of surface antigens on model cell lines using a cocktail of seven lanthanide labeled antibodies demonstrated high specificity and concordance with conventional immunophenotyping. PMID:19122859

Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry.

PubMed

Ornatsky, Olga I; Kinach, Robert; Bandura, Dmitry R; Lou, Xudong; Tanner, Scott D; Baranov, Vladimir I; Nitz, Mark; Winnik, Mitchell A

2008-01-01

Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for elemental tagging of antibodies, immunostaining of live and fixed human leukemia cells, and preparation of samples for ICP-MS analysis. Quantitative analysis of surface antigens on model cell lines using a cocktail of seven lanthanide labeled antibodies demonstrated high specificity and concordance with conventional immunophenotyping.

[Study on microwave digestion of gypsum for the determination of multielement by ICP-OES and ICP-MS].

PubMed

Wang, Hui; Song, Qiang; Yang, Rui-ming; Yao, Qiang; Chen, Chang-he

2010-09-01

Three acids (HNO3, HNO3/HF and HNO3 /HF+ H3BO3) were used to decompose gypsum with microwave digestion system. The contents of 10 mineral elements (Al, Ca, Mg, Fe, K, Na, S, Ti, Si and Sr) in gypsum were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES) while 6 heavy metals (V, Cr, Mn, Zn, Se and Ce) were determined by inductively coupled plasma-mass spectrometry (ICP-MS). GBW03109a, GBW03110 and FGD-2 were used as gypsum standard reference materials. The results showed that two-step microwave digestion with HNO3/HF at 210 degrees C and then adding H3BO3 for the removal of HF and fluorides completely decomposed the gypsums, while this method achieved good recoveries for all elements in the three gypsum standard reference materials. The recovery was from 88% to 112% and the RSD of tests was below 3%. The method was applied to the elemental analysis for flue gas desulfurization gypsums from three coal-fired power plants.

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

PubMed

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

2016-01-01

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

Behavior of microorganisms in drinking water treatment by inductively coupled plasma system: Case study in ground water

NASA Astrophysics Data System (ADS)

Desmiarti, Reni; Hazmi, Ariadi; Martynis, Munas; Sutopo, Ulung Muhammad; Li, Fusheng

2018-02-01

Pathogenic bacteria, such as total coliforms (TC), fecal coliforms (FC) and other coliforms (OC), were removed from groundwater by inductively coupled plasma system treatment in continuous flow experiments. The objective of this study is to investigate the effect of flowrate and frequency on the behavior of microorganisms in drinking water treatment using inductively coupled plasma system (ICPS). The results showed that after 120 minutes of ICPS treatment, the removal efficiency with respect to TC, FC and OC decreased with increasing flowrate. The removal efficiency of FC was achieved at 100% in all runs. Compared to FC, the removal efficiencies with respect to TC and FC were lower than those with respect to TC and OC in the following order: FC >OC> TC. The disinfection yield of TC and OC significantly increased when the removal efficiency increased. The electromagnetic flux varied from 8.08±0.46 to 10.54±0.19 W/cm2. The results in the present work can be used to design a new technology for drinking water treatment to remove all pathogenic bacteria without using hazardous chemicals.

Low pressure laser ablation coupled to inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Fliegel, Daniel; Günther, Detlef

2006-07-01

The particle size distribution in laser ablation inductively coupled plasma mass spectrometry is known to be a critical parameter for complete vaporization of particles. Any strategy to reduce the particle size distribution of laser generated aerosols has the potential to increase the ion signal intensity and to reduce fractionation effects. Due to the fact that vapor generation, nucleation, condensation, and agglomeration take place within an extremely short period of time, ablation under atmospheric pressure might not allow influencing these processes while under reduced pressure condition the cooling of the aerosol and therefore the condensation is expected to be slower. In this study, a low pressure laser ablation cell for the generation of laser aerosols was coupled to an ICP-MS. In contrast to the previously developed trapped ablation mode, the newly designed cell allows the adjustment of the pressure in the ablation cell between 20 and 1400 mbar prior to the ablation. Ablation experiments carried out using this configuration showed a dependence of the aerosol properties (size distribution and particle structure) on the ablation cell pressure. The intensity ratio U/Th measured as a figure of merit for complete vaporization within the ICP indicated a change in the aerosol structure at approximately 500 mbar toward smaller particle size. A significant difference between low pressure and at ambient pressure ablated aerosol was observed. The intensity ratios (U/Th) of the ablated sample moves closer to the bulk composition at lower pressures at the expense of sensitivity. Therefore the decrease in the ICP-MS signal intensity in the low pressure cell can be attributed to vapor deposition within the ablation cell walls. Moreover, scanning electron microscope images of aerosols collected on filters after the low pressure ablation cell suggest the possibility of a slower cooling velocity of the aerosol, which was observed in the condensed material on the surface of

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).

PubMed

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%.

Analytical performance of a low-gas-flow torch optimized for inductively coupled plasma atomic emission spectrometry

USGS Publications Warehouse

Montaser, A.; Huse, G.R.; Wax, R.A.; Chan, S.-K.; Golightly, D.W.; Kane, J.S.; Dorrzapf, A.F.

1984-01-01

An inductively coupled Ar plasma (ICP), generated in a lowflow torch, was investigated by the simplex optimization technique for simultaneous, multielement, atomic emission spectrometry (AES). The variables studied included forward power, observation height, gas flow (outer, intermediate, and nebulizer carrier) and sample uptake rate. When the ICP was operated at 720-W forward power with a total gas flow of 5 L/min, the signal-to-background ratios (S/B) of spectral lines from 20 elements were either comparable or inferior, by a factor ranging from 1.5 to 2, to the results obtained from a conventional Ar ICP. Matrix effect studies on the Ca-PO4 system revealed that the plasma generated in the low-flow torch was as free of vaporizatton-atomizatton interferences as the conventional ICP, but easily ionizable elements produced a greater level of suppression or enhancement effects which could be reduced at higher forward powers. Electron number densities, as determined via the series until line merging technique, were tower ht the plasma sustained in the low-flow torch as compared with the conventional ICP. ?? 1984 American Chemical Society.

Asymmetrical flow field-flow fractionation coupled to inductively coupled plasma mass spectrometry for sizing SeNPs for packaging applications

NASA Astrophysics Data System (ADS)

Palomo-Siguero, María; Vera, Paula; Echegoyen, Yolanda; Nerin, Cristina; Cámara, Carmen; Madrid, Yolanda

2017-06-01

This paper describes the application of Asymmetrical Flow Field-Flow Fractionation (AF4) coupled to diode array detector (DAD) and inductively coupled plasma mass spectrometry (AF4-UV-ICP-MS) to characterize selenium nanoparticles (SeNPs) in an aqueous acrylic adhesive to be used in a multilayer food packaging material. SeNPs were synthesized using a solution-phase approach based on the reduction of selenite with ascorbic acid in presence of different stabilizers compatible with food industry such as polysaccharides (chitosan (poly(D-glucosamine) and hydroxyethylcellulose (HEC)) and non-ionic surfactants (Triton X-100 (t-octylphenoxypolyethoxyethanol), 2,4,7,9-tetramethyl 5decyne-4,7-diol ethoxylate, and isotridecanol ethoxylate). Several parameters such as pH, ascorbic acid and stabilizers concentration, and compatibility of the stabilizer with the adhesive were evaluated. SeNPs suspensions with spherical morphology were obtained except when isotridecanol ethoxylate was employed which provides SeNPs with a nanorod morphology. AF4-DAD-ICP-MS was further applied for sizing the different SeNPs preparations. DAD was used as detector for selecting the best AF4 separation conditions before coupling to ICP-MS to ensure unequivocal identification of NPs. AF4 calibration with polystyrene latex (PSL) beads of known sizes allowed size determination of the different SeNPs. The following estimated hydrodynamic sizes (expressed as the mean ± standard deviation, n = 6 replicates) were found: chitosan-SeNPs- (26 ± 3 nm), TritonX100-SeNPs (22 ± 10 nm) HEC- SeNPs (91 ± 8 nm) and 2,4,7,9-tetramethyl 5decyne-4,7-diol ethoxylate- SeNPs (59 ± 4 nm). The proposed methodology was successfully applied to the characterization in terms of size of aqueous acrylic adhesives containing SeNPs Results from AF4-ICP-MS and TEM shown that only those SeNPs obtained with non-ionic surfactants and HEC were compatible with the adhesive. The results reported here evidence the usefulness of AF4-ICP

Use of Electrodeposition for Sample Preparation and Rejection Rate Prediction for Assay of Electroformed Ultra High Purity Copper for 232Th and 238U Prior to Inductively Coupled Plasma Mass Spectrometry (ICP/MS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoppe, Eric W.; Aalseth, Craig E.; Brodzinski, Ronald L.

The search for neutrinoless double beta decay in 76Ge has driven the need for ultra-low background Ge detectors shielded by electroformed copper of ultra-high radiopurity (<0.1µBq/kg). Although electrodeposition processes are almost sophisticated enough to produce copper of this purity, to date there are no methods sensitive enough to assay it. Inductively-coupled plasma mass spectrometry (ICP/MS) can detect thorium and uranium at femtogram levels, but in the past, this assay has been hindered by high copper concentrations in the sample. Electrodeposition of copper samples removes copper from the solution while selectively concentrating thorium and uranium contaminants to be assayed by ICP/MS.more » Spiking 232Th and 238U into the plating bath simulates low purity copper and allows for the calculation of the electrochemical rejection rate of thorium and uranium in the electroplating system. This rejection value will help to model plating bath chemistry.« less

Spectral emission from the alkali inductively-coupled plasma: Theory and experiment

NASA Astrophysics Data System (ADS)

Bazurto, R.; Huang, M.; Camparo, J.

2018-04-01

The weakly-ionized, alkali inductively-coupled plasma (ICP) has a long history as the light source for optical pumping. Today, its most significant application is perhaps in the rubidium atomic frequency standard (RAFS), arguably the workhorse of atomic timekeeping in space, where it is crucial to the RAFS' functioning and performance (and routinely referred to as the RAFS' "rf-discharge lamp"). In particular, the photon flux from the lamp determines the signal-to-noise ratio of the device, and variations in ICP brightness define the long-term frequency stability of the atomic clock as a consequence of the ac-Stark shift (i.e., the light-shift). Given the importance of Rb atomic clocks to diverse satellite navigation systems (e.g., GPS, Galileo, BeiDou) - and thereby the importance of alkali ICPs to these systems - it is somewhat surprising to find that the physical processes occurring within the discharge are not well understood. As a consequence, researchers do not understand how to improve the spectral emission from the lamp except at a trial-and-error level, nor do they fully understand the nonlinear mechanisms that result in ICP light instability. Here, we take a first step in developing an intuitive, semi-quantitative model of the alkali rf-discharge lamp, and we perform a series of experiments to validate the theory's predictions.

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.

PubMed

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.

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

DOEpatents

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

2010-08-03

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

Review of inductively coupled plasmas: Nano-applications and bistable hysteresis physics

NASA Astrophysics Data System (ADS)

Lee, Hyo-Chang

2018-03-01

Many different gas discharges and plasmas exhibit bistable states under a given set of conditions, and the history-dependent hysteresis that is manifested by intensive quantities of the system upon variation of an external parameter has been observed in inductively coupled plasmas (ICPs). When the external parameters (such as discharge powers) increase, the plasma density increases suddenly from a low- to high-density mode, whereas decreasing the power maintains the plasma in a relatively high-density mode, resulting in significant hysteresis. To date, a comprehensive description of plasma hysteresis and a physical understanding of the main mechanism underlying their bistability remain elusive, despite many experimental observations of plasma bistability conducted under radio-frequency ICP excitation. This fundamental understanding of mode transitions and hysteresis is essential and highly important in various applied fields owing to the widespread use of ICPs, such as semiconductor/display/solar-cell processing (etching, deposition, and ashing), wireless light lamp, nanostructure fabrication, nuclear-fusion operation, spacecraft propulsion, gas reformation, and the removal of hazardous gases and materials. If, in such applications, plasma undergoes a mode transition and hysteresis occurs in response to external perturbations, the process result will be strongly affected. Due to these reasons, this paper comprehensively reviews both the current knowledge in the context of the various applied fields and the global understanding of the bistability and hysteresis physics in the ICPs. At first, the basic understanding of the ICP is given. After that, applications of ICPs to various applied fields of nano/environmental/energy-science are introduced. Finally, the mode transition and hysteresis in ICPs are studied in detail. This study will show the fundamental understanding of hysteresis physics in plasmas and give open possibilities for applications to various applied

Numerical study of heating and evaporation processes of quartz particles in RF inductively coupled plasma

NASA Astrophysics Data System (ADS)

Grishin, Yu M.; Miao, Long

2017-05-01

Numerical simulations of heat and evaporation processes of quartz particles in Ar radio frequency inductively coupled plasma (ICP) are investigated. The quartz particles are supplied by the carrier gas into the ICP within gas-cooling. It is shown that with the increase of amplitude of discharge current above critical value there is a toroidal vortex in the ICP torch at the first coil. The conditions for the formation of vortex and the parameters of the vortex tube have been evaluated and determined. The influence of vortex, discharge current, coil numbers and feed rate of carrier gas on the evaporation efficiency of quartz particles have been demonstrated. It was found that the optimal discharge current is close to the critical value when the quartz particles with initial sizes up to 130 μm can be fully vaporized in the ICP torch with thermal power of 10kW. The heat and evaporation processes of quartz particles in the ICP torch have significant importance for the study of one-step plasma chemical reaction method directly producing silicon from silicide (SiO2) in the argon-hydrogen plasma.

Role of laser ablation-inductively coupled plasma-mass spectrometry in cultural heritage research: a review.

PubMed

Giussani, Barbara; Monticelli, Damiano; Rampazzi, Laura

2009-03-02

Cultural heritage represents a bridge between the contemporary society and the past populations, and a strong collaboration between archaeologists, art historians and analysts may lead to the decryption of the information hidden in an ancient object. Quantitative elemental compositional data play a key role in solving questions concerning dating, provenance, technology, use and the relationship of ancient cultures with the environment. Nevertheless, the scientific investigation of an artifact should be carried out complying with some important constraints: above all the analyses should be as little destructive as possible and performed directly on the object to preserve its integrity. Laser ablation sampling coupled to inductively coupled plasma-mass spectrometry (LA-ICP-MS) fulfils these requirements exhibiting comparably strong analytical performance in trace element determination. This review intends to show through the applications found in the literature how valuable is the contribution of LA-ICP-MS in the investigation of ancient materials such as obsidian, glass, pottery, human remains, written heritage, metal objects and miscellaneous stone materials. The main issues related to cultural heritage investigation are introduced, followed by a brief description of the features of this technique. An overview of the exploitation of LA-ICP-MS is then presented. Finally, advantages and drawbacks of this technique are critically discussed: the fit for purpose and prospects of the use of LA-ICP-MS are presented.

Effect of silane/hydrogen ratio on microcrystalline silicon thin films by remote inductively coupled plasma

NASA Astrophysics Data System (ADS)

Guo, Y. N.; Wei, D. Y.; Xiao, S. Q.; Huang, S. Y.; Zhou, H. P.; Xu, S.

2013-05-01

Hydrogenated microcrystalline silicon (μc-Si:H) thin films were prepared by remote low frequency inductively coupled plasma (ICP) chemical vapor deposition system, and the effect of silane/hydrogen ratio on the microstructure and electrical properties of μc-Si:H films was systematically investigated. As silane/hydrogen ratio increases, the crystalline volume fraction Fc decreases and the ratio of the intensity of (220) peak to that of (111) peak drops as silane flow rate is increased. The FTIR result indicates that the μc-Si:H films prepared by remote ICP have a high optical response with a low hydrogen content, which is in favor of reducing light-induced degradation effect. Furthermore, the processing window of the phase transition region for remote ICP is much wider than that for typical ICP. The photosensitivity of μc-Si:H films can exceed 100 at the transition region and this ensures the possibility of the fabrication of microcrystalline silicon thin film solar cells with a open-circuit voltage of about 700 mV.

Determination of trace-level haloacetic acids in drinking water by ion chromatography-inductively coupled plasma mass spectrometry.

PubMed

Liu, Yongjian; Mou, Shifen; Chen, Dengyun

2004-06-11

A new method for the determination of nine haloacetic acids (HAAs) with ion chromatography (IC) coupled to inductively coupled plasma mass spectrometry (ICP-MS) was developed. With the very hydrophilic anion-exchange column and steep gradient of sodium hydroxide, the nine HAAs could be well separated in 15 min. After suppression with an ASRS suppressor that was introduced in between IC and ICP-MS, the background was much decreased, the interference caused by sodium ion present in eluent was removed, and the sensitivities of HAAs were greatly improved. The chlorinated and brominated HAAs could be detected as 35ClO and 79Br without interference of the matrix due to the elemental selective ICP-MS. The detection limits for mono-, di-, trichloroacetic acids were between 15.6 and 23.6 microg/l. For the other six bromine-containing HAAs, the detection limits were between 0.34 and 0.99 microg/l. With the pretreatment of OnGuard Ag cartridge to remove high concentration of chloride in sample, the developed method could be applied to the determination of HAAs in many drinking water matrices.

Reduction of matrix effects in inductively coupled plasma mass spectrometry by flow injection with an unshielded torch.

PubMed

Gross, Cory T; McIntyre, Sally M; Houk, R S

2009-06-15

Solution samples with matrix concentrations above approximately 0.1% generally present difficulties for analysis by inductively coupled plasma mass spectrometry (ICP-MS) because of cone clogging and matrix effects. Flow injection (FI) is coupled to ICP-MS to reduce deposition from samples such as 1% sodium salts (as NaCl) and seawater (approximately 3% dissolved salts). Surprisingly, matrix effects are also less severe during flow injection, at least for some matrix elements on the particular instrument used. Sodium chloride at 1% Na and undiluted seawater cause only 2 to 29% losses of signal for typical analyte elements. A heavy matrix element (Bi) at 0.1% also induces only approximately 14% loss of analyte signal. However, barium causes a much worse matrix effect, that is, approximately 90% signal loss at 5000 ppm Na. Also, matrix effects during FI are much more severe when a grounded metal shield is inserted between the load coil and the torch, which is the most common mode of operation for the particular ICP-MS device used.

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

EPA Science Inventory

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

Messenger RNA Detection in Leukemia Cell lines by Novel Metal-Tagged in situ Hybridization using Inductively Coupled Plasma Mass Spectrometry.

PubMed

Ornatsky, Olga I; Baranov, Vladimir I; Bandura, Dmitry R; Tanner, Scott D; Dick, John

2006-01-01

Conventional gene expression profiling relies on using fluorescent detection of hybridized probes. Physical characteristics of fluorophores impose limitations on achieving a highly multiplex gene analysis of single cells. Our work demonstrates the feasibility of using metal-tagged in situ hybridization for mRNA detection by inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS as an analytical detector has a number of unique and relevant properties: 1) metals and their stable isotopes generate non-overlapping distinct signals that can be detected simultaneously; 2) these signals can be measured over a wide dynamic range; 3) ICP-MS is quantitative and very sensitive. We used commercial antibodies conjugated to europium (Eu) and gold together with biotinylated oligonucleotide probes reacted with terbium-labeled streptavidin to demonstrate simultaneous mRNA and protein detection by ICP-MS in leukemia cells.

Evaluation of Hydrodynamic Chromatography Coupled with UV-Visible, Fluorescence and Inductively Coupled Plasma Mass Spectrometry Detectors for Sizing and Quantifying Colloids in Environmental Media

PubMed Central

Philippe, Allan; Schaumann, Gabriele E.

2014-01-01

In this study, we evaluated hydrodynamic chromatography (HDC) coupled with inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of nanoparticles in environmental samples. Using two commercially available columns (Polymer Labs-PDSA type 1 and 2), a set of well characterised calibrants and a new external time marking method, we showed that flow rate and eluent composition have few influence on the size resolution and, therefore, can be adapted to the sample particularity. Monitoring the agglomeration of polystyrene nanoparticles over time succeeded without observable disagglomeration suggesting that even weak agglomerates can be measured using HDC. Simultaneous determination of gold colloid concentration and size using ICP-MS detection was validated for elemental concentrations in the ppb range. HDC-ICP-MS was successfully applied to samples containing a high organic and ionic background. Indeed, online combination of UV-visible, fluorescence and ICP-MS detectors allowed distinguishing between organic molecules and inorganic colloids during the analysis of Ag nanoparticles in synthetic surface waters and TiO2 and ZnO nanoparticles in commercial sunscreens. Taken together, our results demonstrate that HDC-ICP-MS is a flexible, sensitive and reliable method to measure the size and the concentration of inorganic colloids in complex media and suggest that there may be a promising future for the application of HDC in environmental science. Nonetheless the rigorous measurements of agglomerates and of matrices containing natural colloids still need to be studied in detail. PMID:24587393

Evaluation of hydrodynamic chromatography coupled with UV-visible, fluorescence and inductively coupled plasma mass spectrometry detectors for sizing and quantifying colloids in environmental media.

PubMed

Philippe, Allan; Schaumann, Gabriele E

2014-01-01

In this study, we evaluated hydrodynamic chromatography (HDC) coupled with inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of nanoparticles in environmental samples. Using two commercially available columns (Polymer Labs-PDSA type 1 and 2), a set of well characterised calibrants and a new external time marking method, we showed that flow rate and eluent composition have few influence on the size resolution and, therefore, can be adapted to the sample particularity. Monitoring the agglomeration of polystyrene nanoparticles over time succeeded without observable disagglomeration suggesting that even weak agglomerates can be measured using HDC. Simultaneous determination of gold colloid concentration and size using ICP-MS detection was validated for elemental concentrations in the ppb range. HDC-ICP-MS was successfully applied to samples containing a high organic and ionic background. Indeed, online combination of UV-visible, fluorescence and ICP-MS detectors allowed distinguishing between organic molecules and inorganic colloids during the analysis of Ag nanoparticles in synthetic surface waters and TiO₂ and ZnO nanoparticles in commercial sunscreens. Taken together, our results demonstrate that HDC-ICP-MS is a flexible, sensitive and reliable method to measure the size and the concentration of inorganic colloids in complex media and suggest that there may be a promising future for the application of HDC in environmental science. Nonetheless the rigorous measurements of agglomerates and of matrices containing natural colloids still need to be studied in detail.

Microwave-assisted wet digestion with H2O2 at high temperature and pressure using single reaction chamber for elemental determination in milk powder by ICP-OES and ICP-MS.

PubMed

Muller, Edson I; Souza, Juliana P; Muller, Cristiano C; Muller, Aline L H; Mello, Paola A; Bizzi, Cezar A

2016-08-15

In this work a green digestion method which only used H2O2 as an oxidant and high temperature and pressure in the single reaction chamber system (SRC-UltraWave™) was applied for subsequent elemental determination by inductively coupled plasma-based techniques. Milk powder was chosen to demonstrate the feasibility and advantages of the proposed method. Samples masses up to 500mg were efficiently digested, and the determination of Ca, Fe, K, Mg and Na was performed by inductively coupled plasma optical emission spectrometry (ICP-OES), while trace elements (B, Ba, Cd, Cu, Mn, Mo, Pb, Sr and Zn) were determined by inductively coupled plasma mass spectrometry (ICP-MS). Residual carbon (RC) lower than 918mgL(-1) of C was obtained for digests which contributed to minimizing interferences in determination by ICP-OES and ICP-MS. Accuracy was evaluated using certified reference materials NIST 1549 (non-fat milk powder certified reference material) and NIST 8435 (whole milk powder reference material). The results obtained by the proposed method were in agreement with the certified reference values (t-test, 95% confidence level). In addition, no significant difference was observed between results obtained by the proposed method and conventional wet digestion using concentrated HNO3. As digestion was performed without using any kind of acid, the characteristics of final digests were in agreement with green chemistry principles when compared to digests obtained using conventional wet digestion method with concentrated HNO3. Additionally, H2O2 digests were more suitable for subsequent analysis by ICP-based techniques due to of water being the main product of organic matrix oxidation. The proposed method was suitable for quality control of major components and trace elements present in milk powder in consonance with green sample preparation. Copyright © 2016 Elsevier B.V. All rights reserved.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

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

1993-03-17

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 ismore » 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[center dot]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.« less

Aerosol detection efficiency in inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

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

Aerosol detection efficiency in inductively coupled plasma mass spectrometry

DOE PAGES

Hubbard, Joshua A.; Zigmond, Joseph A.

2016-03-02

We used an electrostatic size classification technique to segregate particles of known composition prior to being injected into an inductively coupled plasma mass spectrometer (ICP-MS). Moreover, we counted size-segregated particles 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 bymore » 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

Inductively Coupled Plasma-Induced Electrical Damage on HgCdTe Etched Surface at Cryogenic Temperatures

NASA Astrophysics Data System (ADS)

Liu, L. F.; Chen, Y. Y.; Ye, Z. H.; Hu, X. N.; Ding, R. J.; He, L.

2018-03-01

Plasma etching is a powerful technique for transferring high-resolution lithographic patterns into HgCdTe material with low etch-induced damage, and it is important for fabricating small-pixel-size HgCdTe infrared focal plane array (IRFPA) detectors. P- to n-type conversion is known to occur during plasma etching of vacancy-doped HgCdTe; however, it is usually unwanted and its removal requires extra steps. Etching at cryogenic temperatures can reduce the etch-induced type conversion depth in HgCdTe via the electrical damage mechanism. Laser beam-induced current (LBIC) is a nondestructive photoelectric characterization technique which can provide information regarding the vertical and lateral electrical field distribution, such as defects and p-n junctions. In this work, inductively coupled plasma (ICP) etching of HgCdTe was implemented at cryogenic temperatures. For an Ar/CH4 (30:1 in SCCM) plasma with ICP input power of 1000 W and RF-coupled DC bias of ˜ 25 V, a HgCdTe sample was dry-etched at 123 K for 5 min using ICP. The sample was then processed to remove a thin layer of the plasma-etched region while maintaining a ladder-like damaged layer by continuously controlling the wet chemical etching time. Combining the ladder etching method and LBIC measurement, the ICP etching-induced electrical damage depth was measured and estimated to be about 20 nm. The results indicate that ICP etching at cryogenic temperatures can significantly suppress plasma etching-induced electrical damage, which is beneficial for defining HgCdTe mesa arrays.

Analysis of metal-binding proteins separated by non-denaturating gel electrophoresis using matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS).

PubMed

Becker, J Susanne; Mounicou, Sandra; Zoriy, Miroslav V; Becker, J Sabine; Lobinski, Ryszard

2008-09-15

Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF-MS) and laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) have become established as very efficient and sensitive biopolymer and elemental mass spectrometric techniques for studying metal-binding proteins (metalloproteins) in life sciences. Protein complexes present in rat tissues (liver and kidney) were separated in their native state in the first dimension by blue native gel electrophoresis (BN-PAGE). Essential and toxic metals, such as zinc, copper, iron, nickel, chromium, cadmium and lead, were detected by scanning the gel bands using quadrupole LA-ICP-MS with and without collision cell as a microanalytical technique. Several proteins were identified by using MALDI-TOF-MS together with a database search. For example, on one protein band cut from the BN-PAGE gel and digested with the enzyme trypsin, two different proteins - protein FAM44B and cathepsin B precursor - were identified. By combining biomolecular and elemental mass spectrometry, it was possible to characterize and identify selected metal-binding rat liver and kidney tissue proteins.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bank, Tracy L.; Roth, Elliot A.; Tinker, Phillip

2016-04-17

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

Ultra-Shallow Depth Profiling of Arsenic Implants in Silicon by Hydride Generation-Inductively Coupled Plasma Atomic Emission Spectrometry

NASA Astrophysics Data System (ADS)

Matsubara, Atsuko; Kojima, Hisao; Itoga, Toshihiko; Kanehori, Keiichi

1995-08-01

High resolution depth profiling of arsenic (As) implanted into silicon wafers by a chemical technique is described. Silicon wafers are precisely etched through repeated oxidation by hydrogen peroxide solution and dissolution of the oxide by hydrofluoric acid solution. The etched silicon thickness is determined by inductively-coupled plasma atomic emission spectrometry (ICP-AES). Arsenic concentration is determined by hydride generation ICP-AES (HG-ICP-AES) with prereduction using potassium iodide. The detection limit of As in a 4-inch silicon wafer is 2.4×1018 atoms/cm3. The etched silicon thickness is controlled to less than 4±2 atomic layers. Depth profiling of an ultra-shallow As diffusion layer with the proposed method shows good agreement with profiling using the four-probe method or secondary ion mass spectrometry.

[Study on microwave digestion of coal for the determination of multi-element by ICP-OES and ICP-MS].

PubMed

Wang, Hui; Song, Qiang; Yao, Qiang; Chen, Chang-He; Yu, Fei-Lu

2012-06-01

Effects of temperature and four acids (HNO3, HNO3/H2O2, HNO3/HF and HNO3/HF+H3BO3) on the coal decomposition by microwave digestion and the multi-element analysis were studied. SARM20 was used as a coal standard reference material. The contents of 10 mineral elements (Al, Ca, Fe, Mg, K, Na, S, Si, Sr and Ti) in the coal SARM20 were determined by inductively coupled plasma-optical emission spectrometry (ICP-OES). And the contents of 20 heavy metals (Li, Be, Sc, V, Cr, Mn, Co, Ni, Cu, Zn, Ga, As, Se, Zr, Sn, Cs, Ba, Ce, Eu and Pb) were determined by inductively coupled plasma-mass spectrometry (ICP-MS). The results showed that the coal was completely decomposed by microwave digestion with HNO3/HF+ H3BO3 at 210 degrees C. Good recoveries for all elements in the coal SARM20 were obtained by this two-step microwave digestion method. The recoveries of the 10 mineral elements were from 87.5% to 98.8%, and the recoveries of the 20 heavy metals were from 85% to 112.5%. All RSDs of tests were below 3%.

Improved documentation of spectral lines for inductively coupled plasma emission spectrometry

NASA Astrophysics Data System (ADS)

Doidge, Peter S.

2018-05-01

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

Complexation studies with lanthanides and humic acid analyzed by ultrafiltration and capillary electrophoresis-inductively coupled plasma mass spectrometry.

PubMed

Kautenburger, Ralf; Beck, Horst Philipp

2007-08-03

For the long-term storage of radioactive waste, detailed information about geo-chemical behavior of radioactive and toxic metal ions under environmental conditions is necessary. Humic acid (HA) can play an important role in the immobilisation or mobilisation of metal ions due to complexation and colloid formation. Therefore, we investigate the complexation behavior of HA and its influence on the migration or retardation of selected lanthanides (europium and gadolinium as homologues of the actinides americium and curium). Two independent speciation techniques, ultrafiltration and capillary electrophoresis coupled with inductively coupled plasma mass spectrometry (CE-ICP-MS) have been compared for the study of Eu and Gd interaction with (purified Aldrich) HA. The degree of complexation of Eu and Gd in 25 mg l(-1) Aldrich HA solutions was determined with a broad range of metal loading (Eu and Gd total concentration between 10(-6) and 10(-4) mol l(-1)), ionic strength of 10 mM (NaClO4) and different pH-values. From the CE-ICP-MS electropherograms, additional information on the charge of the Eu species was obtained by the use of 1-bromopropane as neutral marker. To detect HA in the ICP-MS and separate between HA complexed and non complexed metal ions in the CE-ICP-MS, we have halogenated the HA with iodine as ICP-MS marker.

Authentication of Kalix (N.E. Sweden) vendace caviar using inductively coupled plasma-based analytical techniques: evaluation of different approaches.

PubMed

Rodushkin, I; Bergman, T; Douglas, G; Engström, E; Sörlin, D; Baxter, D C

2007-02-05

Different analytical approaches for origin differentiation between vendace and whitefish caviars from brackish- and freshwaters were tested using inductively coupled plasma double focusing sector field mass spectrometry (ICP-SFMS) and multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). These approaches involve identifying differences in elemental concentrations or sample-specific isotopic composition (Sr and Os) variations. Concentrations of 72 elements were determined by ICP-SFMS following microwave-assisted digestion in vendace and whitefish caviar samples from Sweden (from both brackish and freshwater), Finland and USA, as well as in unprocessed vendace roe and salt used in caviar production. This data set allows identification of elements whose contents in caviar can be affected by salt addition as well as by contamination during production and packaging. Long-term method reproducibility was assessed for all analytes based on replicate caviar preparations/analyses and variations in element concentrations in caviar from different harvests were evaluated. The greatest utility for differentiation was demonstrated for elements with varying concentrations between brackish and freshwaters (e.g. As, Br, Sr). Elemental ratios, specifically Sr/Ca, Sr/Mg and Sr/Ba, are especially useful for authentication of vendace caviar processed from brackish water roe, due to the significant differences between caviar from different sources, limited between-harvest variations and relatively high concentrations in samples, allowing precise determination by modern analytical instrumentation. Variations in the 87Sr/86Sr ratio for vendace caviar from different harvests (on the order of 0.05-0.1%) is at least 10-fold less than differences between caviar processed from brackish and freshwater roe. Hence, Sr isotope ratio measurements (either by ICP-SFMS or by MC-ICP-MS) have great potential for origin differentiation. On the contrary, it was impossible to

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

NASA Astrophysics Data System (ADS)

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

2018-06-01

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

Selected problems with boron determination in water treatment processes. Part I: comparison of the reference methods for ICP-MS and ICP-OES determinations.

PubMed

Kmiecik, Ewa; Tomaszewska, Barbara; Wątor, Katarzyna; Bodzek, Michał

2016-06-01

The aim of the study was to compare the two reference methods for the determination of boron in water samples and further assess the impact of the method of preparation of samples for analysis on the results obtained. Samples were collected during different desalination processes, ultrafiltration and the double reverse osmosis system, connected in series. From each point, samples were prepared in four different ways: the first was filtered (through a membrane filter of 0.45 μm) and acidified (using 1 mL ultrapure nitric acid for each 100 mL of samples) (FA), the second was unfiltered and not acidified (UFNA), the third was filtered but not acidified (FNA), and finally, the fourth was unfiltered but acidified (UFA). All samples were analysed using two analytical methods: inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma optical emission spectrometry (ICP-OES). The results obtained were compared and correlated, and the differences between them were studied. The results show that there are statistically significant differences between the concentrations obtained using the ICP-MS and ICP-OES techniques regardless of the methods of sampling preparation (sample filtration and preservation). Finally, both the ICP-MS and ICP-OES methods can be used for determination of the boron concentration in water. The differences in the boron concentrations obtained using these two methods can be caused by several high-level concentrations in selected whole-water digestates and some matrix effects. Higher concentrations of iron (from 1 to 20 mg/L) than chromium (0.02-1 mg/L) in the samples analysed can influence boron determination. When iron concentrations are high, we can observe the emission spectrum as a double joined and overlapping peak.

Messenger RNA Detection in Leukemia Cell lines by Novel Metal-Tagged in situ Hybridization using Inductively Coupled Plasma Mass Spectrometry

PubMed Central

Ornatsky, Olga I.; Baranov, Vladimir I.; Bandura, Dmitry R.; Tanner, Scott D.; Dick, John

2006-01-01

Conventional gene expression profiling relies on using fluorescent detection of hybridized probes. Physical characteristics of fluorophores impose limitations on achieving a highly multiplex gene analysis of single cells. Our work demonstrates the feasibility of using metal-tagged in situ hybridization for mRNA detection by inductively coupled plasma mass spectrometry (ICP-MS). ICP-MS as an analytical detector has a number of unique and relevant properties: 1) metals and their stable isotopes generate non-overlapping distinct signals that can be detected simultaneously; 2) these signals can be measured over a wide dynamic range; 3) ICP-MS is quantitative and very sensitive. We used commercial antibodies conjugated to europium (Eu) and gold together with biotinylated oligonucleotide probes reacted with terbium-labeled streptavidin to demonstrate simultaneous mRNA and protein detection by ICP-MS in leukemia cells. PMID:23662035

Numerical and Experimental Investigation on the Attenuation of Electromagnetic Waves in Unmagnetized Plasmas Using Inductively Coupled Plasma Actuator

NASA Astrophysics Data System (ADS)

Lin, Min; Xu, Haojun; Wei, Xiaolong; Liang, Hua; Song, Huimin; Sun, Quan; Zhang, Yanhua

2015-10-01

The attenuation of electromagnetic (EM) waves in unmagnetized plasma generated by an inductively coupled plasma (ICP) actuator has been investigated both theoretically and experimentally. A numerical study is conducted to investigate the propagation of EM waves in multilayer plasma structures which cover a square flat plate. Experimentally, an ICP actuator with dimensions of 20 cm×20 cm×4 cm is designed to produce a steady plasma slab. The attenuation of EM waves in the plasma generated by the ICP actuator is measured by a reflectivity arch test method at incident waves of 2.3 GHz and 10.1 GHz, respectively. A contrastive analysis of calculated and measured results of these incident wave frequencies is presented, which suggests that the experiment accords well with our theory. As expected, the plasma slab generated by the ICP actuator can effectively attenuate the EM waves, which may have great potential application prospects in aircraft stealth. supported by National Natural Science Foundation of China (Nos. 51276197, 11472306 and 11402301)

Laser ablation-inductively coupled plasma mass spectrometry: an emerging technology for detecting rare cells in tissue sections.

PubMed

Managh, Amy J; Hutchinson, Robert W; Riquelme, Paloma; Broichhausen, Christiane; Wege, Anja K; Ritter, Uwe; Ahrens, Norbert; Koehl, Gudrun E; Walter, Lisa; Florian, Christian; Schlitt, Hans J; Reid, Helen J; Geissler, Edward K; Sharp, Barry L; Hutchinson, James A

2014-09-01

Administering immunoregulatory cells to patients as medicinal agents is a potentially revolutionary approach to the treatment of immunologically mediated diseases. Presently, there are no satisfactory, clinically applicable methods of tracking human cells in patients with adequate spatial resolution and target cell specificity over a sufficient period of time. Laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) represents a potential solution to the problem of detecting very rare cells in tissues. In this article, this exquisitely sensitive technique is applied to the tracking of gold-labeled human regulatory macrophages (Mregs) in immunodeficient mice. Optimal conditions for labeling Mregs with 50-nm gold particles were investigated by exposing Mregs in culture to variable concentrations of label: Mregs incubated with 3.5 × 10(9) particles/ml for 1 h incorporated an average of 3.39 × 10(8) Au atoms/cell without loss of cell viability. Analysis of single, gold-labeled Mregs by LA-ICP-MS registered an average of 1.9 × 10(5) counts/cell. Under these conditions, 100% labeling efficiency was achieved, and label was retained by Mregs for ≥36 h. Gold-labeled Mregs adhered to glass surfaces; after 24 h of culture, it was possible to colabel these cells with human-specific (154)Sm-tagged anti-HLA-DR or (174)Yb-tagged anti-CD45 mAbs. Following injection into immunodeficient mice, signals from gold-labeled human Mregs could be detected in mouse lung, liver, and spleen for at least 7 d by solution-based inductively coupled plasma mass spectrometry and LA-ICP-MS. These promising results indicate that LA-ICP-MS tissue imaging has great potential as an analytical technique in immunology. Copyright © 2014 by The American Association of Immunologists, Inc.

Elimination of boron memory effect in inductively coupled plasma-mass spectrometry by ammonia gas injection into the spray chamber during analysis

NASA Astrophysics Data System (ADS)

Al-Ammar, Assad S.; Gupta, Rajesh K.; Barnes, Ramon M.

2000-06-01

Injection of 10-20 ml/min of ammonia gas into an inductively coupled plasma-mass spectrometry (ICP-MS) spray chamber during boron determination eliminates the memory effect of a 1 μg/ml B solution within a 2-min washing time. Ammonia gas injection also reduces the boron blank by a factor of four and enhances the sensitivity by 33-90%. Boron detection limits are improved from 12 and 14 to 3 and 4 ng/ml, respectively, for two ICP-MS instruments. Trace boron concentrations in certified reference materials agree well using ammonia gas injection.

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

USDA-ARS?s Scientific Manuscript database

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...

Deep inductively coupled plasma etching of ELO-GaN grown with high fill factor

NASA Astrophysics Data System (ADS)

Gao, Haiyong; Lee, Jaesoong; Ni, Xianfeng; Leach, Jacob; Özgür, Ümit; Morkoç, Hadis

2011-02-01

The epitaxial lateral overgrowth (ELO) gallium nitride (GaN) was grown with high fill factor using metal organic chemical vapor deposition (MOCVD). The inductively coupled plasma (ICP) etching of ELO-GaN based on Cl2/Ar/SiCl4 gas mixture was performed. Surface properties of ELO-GaN subjected to ICP etching have been investigated and optimized etching condition in ELO-GaN with ICP etching is presented. Radiofrequency (RF) power and the flow rate of Cl2 gas were modified during the experiments. The window region, wing region and the edge region of ELO-GaN pattern present different etching characteristics. Different etching conditions were studied to get the minimized plasma-induced damage, relatively high etching rates, and excellent surface profiles. Etch depths of the etched ELO-GaN with smooth surface up to about 19 μm were achieved. The most suitable three-step etching condition is discussed with the assessment based on the morphology observation of the etched surface of ELO-GaN patterns.

Solution-based calibration strategy for laser ablation-inductively coupled plasma-mass spectrometry using desolvating nebulizer system

NASA Astrophysics Data System (ADS)

Zhang, Guoxia; Li, Qing; Zhu, Yan; Wang, Zheng

2018-07-01

An additional quantification strategy using a desolvating nebulizer system (DNS) for solution-based calibration was developed. For quantitative analysis, laser ablation (LA) and DNS-generated aerosols were coupled using a "Y" connector and introduced into the inductively coupled plasma (ICP). These aerosols were also observed by scanning electron microscopy following collection on a silicon chip. Internal standards (108Ag, 64Cu, 89Y) were used to correct for the different aerosol transport efficiencies between the DNS and LA. The correlation coefficients of the calibration curves for all elements ranged from 0.9986 to 0.9999. Standard reference materials (NIST 610-616 and GBW08407-08411) were used to demonstrate the accuracy and precision of the method. The results were in good agreement with certified values, and the relative standard deviation (RSD) of most elements was <3%. The limits of detection (LODs) for 50Cr, 55Mn, 59Co, 60Ni, 66Zn, 89Y, 110Cd, 139La, 140Ce, 146Nd, 147Sm, 157Gd, 163Dy, 166Er, and 208Pb were 23, 3, 3, 19, 31, 4, 12, 0.4, 0.9, 0.1, 0.2, 2, 0.3, 0.4, and 21 ng/g, respectively, which were significantly better than those obtained by other methods. Further, this approach was applied for the analysis of multiple elements in biological tissues, and the results were in good agreement with those obtained using solution-based inductively coupled plasma-mass spectrometry (ICP-MS).

Elemental bioimaging by means of LA-ICP-OES: investigation of the calcium, sodium and potassium distribution in tobacco plant stems and leaf petioles.

PubMed

Thyssen, G M; Holtkamp, M; Kaulfürst-Soboll, H; Wehe, C A; Sperling, M; von Schaewen, A; Karst, U

2017-06-21

Laser ablation-inductively coupled plasma-optical emission spectroscopy (LA-ICP-OES) is presented as a valuable tool for elemental bioimaging of alkali and earth alkali elements in plants. Whereas LA-ICP-OES is commonly used for micro analysis of solid samples, laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) has advanced to the gold standard for bioimaging. However, especially for easily excitable and ubiquitous elements such as alkali and earth alkali elements, LA-ICP-OES holds some advantages regarding simultaneous detection, costs, contamination, and user-friendliness. This is demonstrated by determining the calcium, sodium and potassium distribution in tobacco plant stem and leaf petiole tissues. A quantification of the calcium contents in a concentration range up to 1000 μg g -1 using matrix-matched standards is presented as well. The method is directly compared to a LA-ICP-MS approach by analyzing parallel slices of the same samples.

Upcycling Waste Lard Oil into Vertical Graphene Sheets by Inductively Coupled Plasma Assisted Chemical Vapor Deposition.

PubMed

Wu, Angjian; Li, Xiaodong; Yang, Jian; Du, Changming; Shen, Wangjun; Yan, Jianhua

2017-10-12

Vertical graphene (VG) sheets were single-step synthesized via inductively coupled plasma (ICP)-enhanced chemical vapor deposition (PECVD) using waste lard oil as a sustainable and economical carbon source. Interweaved few-layer VG sheets, H₂, and other hydrocarbon gases were obtained after the decomposition of waste lard oil. The influence of parameters such as temperature, gas proportion, ICP power was investigated to tune the nanostructures of obtained VG, which indicated that a proper temperature and H₂ concentration was indispensable for the synthesis of VG sheets. Rich defects of VG were formed with a high I D / I G ratio (1.29), consistent with the dense edges structure observed in electron microscopy. Additionally, the morphologies, crystalline degree, and wettability of nanostructure carbon induced by PECVD and ICP separately were comparatively analyzed. The present work demonstrated the potential of our PECVD recipe to synthesize VG from abundant natural waste oil, which paved the way to upgrade the low-value hydrocarbons into advanced carbon material.

Capacitively-coupled inductive sensor

DOEpatents

Ekdahl, Carl A.

1984-01-01

A capacitively coupled inductive shunt current sensor which utilizes capacitive coupling between flanges having an annular inductive channel formed therein. A voltage dividing capacitor is connected between the coupling capacitor and ground to provide immediate capacitive division of the output signal so as to provide a high frequency response of the current pulse to be detected. The present invention can be used in any desired outer conductor such as the outer conductor of a coaxial transmission line, the outer conductor of an electron beam transmission line, etc.

On the possibility of the multiple inductively coupled plasma and helicon plasma sources for large-area processes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, Jin-Won; Lee, Yun-Seong, E-mail: leeeeys@kaist.ac.kr; Chang, Hong-Young

2014-08-15

In this study, we attempted to determine the possibility of multiple inductively coupled plasma (ICP) and helicon plasma sources for large-area processes. Experiments were performed with the one and two coils to measure plasma and electrical parameters, and a circuit simulation was performed to measure the current at each coil in the 2-coil experiment. Based on the result, we could determine the possibility of multiple ICP sources due to a direct change of impedance due to current and saturation of impedance due to the skin-depth effect. However, a helicon plasma source is difficult to adapt to the multiple sources duemore » to the consistent change of real impedance due to mode transition and the low uniformity of the B-field confinement. As a result, it is expected that ICP can be adapted to multiple sources for large-area processes.« less

Spark ablation-inductively coupled plasma spectrometry for analysis of geologic materials

USGS Publications Warehouse

Golightly, D.W.; Montaser, A.; Smith, B.L.; Dorrzapf, A.F.

1989-01-01

Spark ablation-inductively coupled plasma (SA-ICP) spectrometry is applied to the measurement of hafnium-zirconium ratios in zircons and to the determination of cerium, cobalt, iron, lead, nickel and phosphorus in ferromanganese nodules. Six operating parameters used for the high-voltage spark and argon-ICP combination are established by sequential simplex optimization of both signal-to-background ratio and signal-to-noise ratio. The time-dependences of the atomic emission signals of analytes and matrix elements ablated from a finely pulverized sample embedded in a pressed disk of copper demonstrate selective sampling by the spark. Concentration ratios of hafnium to zirconium in zircons are measured with a precision of 4% (relative standard deviation, RSD). For ferromanganese nodules, spectral measurements based on intensity ratios of analyte line to the Mn(II) 257.610 nm line provide precisions of analysis in the range from 7 to 14% RSD. The accuracy of analysis depends on use of standard additions of the reference material USGS Nod P-1, and an independent measurement of the Mn concentration. ?? 1989.

LIBS coupled with ICP/OES for the spectral analysis of betel leaves

NASA Astrophysics Data System (ADS)

Rehan, I.; Rehan, K.; Sultana, S.; Khan, M. Z.; Muhammad, R.

2018-05-01

Laser-induced breakdown spectroscopy (LIBS) system was optimized and was applied for the elemental analysis and exposure of the heavy metals in betel leaves in air. Pulsed Nd:YAG (1064 nm) in conjunction with a suitable detector (LIBS 2000+, Ocean Optics, Inc) having the optical resolution of 0.06 nm was used to record the emission spectra from 200 to 720 nm. Elements like Al, Ba, Ca, Cr, Cu, P, Fe, K, Mg, Mn, Na, P, S, Sr, and Zn were found to be present in the samples. The abundances of observed elements were calculated through normalized calibration curve method, integrated intensity ratio method, and calibration free-LIBS approach. Quantitative analyses were accomplished under the assumption of local thermodynamic equilibrium (LTE) and optically thin plasma. LIBS findings were validated by comparing its results with the results obtained using a typical analytical technique of inductively coupled plasma-optical emission spectroscopy (ICP/OES). Limit of detection (LOD) of the LIBS system was also estimated for heavy metals.

Analysis of 34S in Individual Organic Compounds by Coupled GC-ICP-MS

NASA Astrophysics Data System (ADS)

Sessions, A. L.; Amrani, A.; Adkins, J. F.

2009-12-01

The abundances of 2H, 13C, and 15N in organic compounds have been extremely useful in many aspects of biogeochemistry. While sulfur plays an equally important role in many earth-surface processes, the isotopes of sulfur in organic matter have not been extensively employed in large part because there has been no direct route to the analysis of 34S in individual organic compounds. To remedy this, we have developed a highly sensitive and robust method for the analysis of 34S in individual organic compounds by coupled gas chromatography (GC) and multicollector inductively-coupled plasma mass spectrometry (ICP-MS). Isobaric interference from O2+ is minimized by employing dry plasma conditions, and is cleanly resolved at all masses using medium resolution on the Thermo Neptune ICP-MS. Correction for mass bias is accomplished using standard-sample bracketing with peaks of SF6 reference gas. The precision of measured δ34S values approaches 0.1‰ for analytes containing >40 pmol S, and is better than 0.5‰ for those containing as little as 6 pmol S. External accuracy is better than 0.3‰. Integrating only the center of chromatographic peaks, rather than the entire peak, offers significant gain in precision and chromatographic resolution with minimal effect on accuracy, but requires further study for verification as a routine method. Coelution of organic compounds that do not contain S can cause degraded analytical precision and accuracy. As a demonstration of the potential for this new method, we will present data from 3 sample types: individual organosulfur compounds from crude oil, dimethyl sulfide from seawater, and trace H2S from bacterial culture headspace.

Multivariate classification of edible salts: Simultaneous Laser-Induced Breakdown Spectroscopy and Laser-Ablation Inductively Coupled Plasma Mass Spectrometry Analysis

NASA Astrophysics Data System (ADS)

Lee, Yonghoon; Nam, Sang-Ho; Ham, Kyung-Sik; Gonzalez, Jhanis; Oropeza, Dayana; Quarles, Derrick; Yoo, Jonghyun; Russo, Richard E.

2016-04-01

Laser-Induced Breakdown Spectroscopy (LIBS) and Laser-Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS), both based on laser ablation sampling, can be employed simultaneously to obtain different chemical fingerprints from a sample. We demonstrated that this analysis approach can provide complementary information for improved classification of edible salts. LIBS could detect several of the minor metallic elements along with Na and Cl, while LA-ICP-MS spectra were used to measure non-metallic and trace heavy metal elements. Principal component analysis using LIBS and LA-ICP-MS spectra showed that their major spectral variations classified the sample salts in different ways. Three classification models were developed by using partial least squares-discriminant analysis based on the LIBS, LA-ICP-MS, and their fused data. From the cross-validation performances and confusion matrices of these models, the minor metallic elements (Mg, Ca, and K) detected by LIBS and the non-metallic (I) and trace heavy metal (Ba, W, and Pb) elements detected by LA-ICP-MS provided complementary chemical information to distinguish particular salt samples.

Application of infrared thermography for online monitoring of wall temperatures in inductively coupled plasma torches with conventional and low-flow gas consumption

NASA Astrophysics Data System (ADS)

Engelhard, Carsten; Scheffer, Andy; Maue, Thomas; Hieftje, Gary M.; Buscher, Wolfgang

2007-10-01

Inductively coupled plasma (ICP) sources typically used for trace elemental determination and speciation were investigated with infrared (IR) thermography to obtain spatially resolved torch temperature distributions. Infrared thermographic imaging is an excellent tool for the monitoring of temperatures in a fast and non-destructive way. This paper presents the first application of IR thermography to inductively coupled plasma torches and the possibility to investigate temperatures and thermal patterns while the ICP is operating and despite background emission from the plasma itself. A fast and easy method is presented for the determination of temperature distributions and stress features within ICP torches. Two different ICP operating torches were studied: a commercially available Fassel-type ICP unit with 14 L min - 1 total Ar consumption and a SHIP torch with the unusually low Ar flow of 0.6 L min - 1 . Spatially resolved infrared images of both torches were obtained and laterally resolved temperature profiles were extracted. After temperature-resolved calibration of the emissivity (between 0.5 and 0.35 at 873-1323 K) and transmission (20% between 3.75 and 4.02 μm) of the fused quartz used in the torch construction, an image correction was applied. Inhomogeneous temperature distributions with locally defined stress areas in the conventional Fassel-type torch were revealed. As a general trend, it was found that the SHIP torch exhibited higher temperatures ( Tmax = 1580 K) than the conventional torch ( Tmax = 730 K). In the former case, torch sites with efficient and inefficient cooling were discovered and the external flow of cooling air (24-48 m s - 1 ) was identified as the limiting factor.

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

PubMed

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.

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

PubMed

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.

Determination of glyphosate and phosphate in water by ion chromatography--inductively coupled plasma mass spectrometry detection.

PubMed

Guo, Zhong-Xian; Cai, Qiantao; Yang, Zhaoguang

2005-12-30

Quantitative determination of trace glyphosate and phosphate in waters was achieved by coupling ion chromatography (IC) separation with inductively coupled plasma mass spectrometry (ICP-MS) detection. The separation of glyphosate and phosphate on a polymer anion-exchange column (Dionex IonPac AS16, 4.0 mm x 250 mm) was obtained by eluting them with 20 mM citric acid at 0.50 mL min(-1), and the analytes were detected directly and selectively by ICP-MS at m/z = 31. Parameters affecting their chromatographic behaviors and ICP-MS characteristics were systematically examined. Based on a 500-microL sample injection volume, the detection limits were 0.7 microgL(-1) for both glyphosate and phosphate, and the calibrations were linear up to 400 microgL(-1). Polyphosphates, aminomethylphosphonic acid (the major metabolite of glyphosate), non-polar and other polar phosphorus-containing pesticides showed different chromatographic behaviors from the analytes of interest and therefore did not interference. The determination was also interference free from the matrix anions (nitrate, nitrite, sulphate, chloride, etc.) and metallic ions. The analysis of certified reference material, drinking water, reservoir water and Newater yielded satisfactory results with spiked recoveries of 97.1-107.0% and relative standard deviations of < or = 7.4% (n = 3). Compared to other reported methods for glyphosate and phosphate, the developed IC-ICP-MS method is sensitive and simple, and does not require any chemical derivatization, sample preconcentration and mobile phase conductivity suppression.

Measurement of low radioactivity background in a high voltage cable by high resolution inductively coupled plasma mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vacri, M. L. di; Nisi, S.; Balata, M.

2013-08-08

The measurement of naturally occurring low level radioactivity background in a high voltage (HV) cable by high resolution inductively coupled plasma mass spectrometry (HR ICP MS) is presented in this work. The measurements were performed at the Chemistry Service of the Gran Sasso National Laboratory. The contributions to the radioactive background coming from the different components of the heterogeneous material were separated. Based on the mass fraction of the cable, the whole contamination was calculated. The HR ICP MS results were cross-checked by gamma ray spectroscopy analysis that was performed at the low background facility STELLA (Sub Terranean Low Levelmore » Assay) of the LNGS underground lab using HPGe detectors.« less

Uniformity studies of inductively coupled plasma etching in fabrication of HgCdTe detector arrays

NASA Astrophysics Data System (ADS)

Bommena, R.; Velicu, S.; Boieriu, P.; Lee, T. S.; Grein, C. H.; Tedjojuwono, K. K.

2007-04-01

Inductively coupled plasma (ICP) chemistry based on a mixture of CH 4, Ar, and H II was investigated for the purpose of delineating HgCdTe mesa structures and vias typically used in the fabrication of second and third generation infrared photo detector arrays. We report on ICP etching uniformity results and correlate them with plasma controlling parameters (gas flow rates, total chamber pressure, ICP power and RF power). The etching rate and surface morphology of In-doped MWIR and LWIR HgCdTe showed distinct dependences on the plasma chemistry, total pressure and RF power. Contact stylus profilometry and cross-section scanning electron microscopy (SEM) were used to characterize the anisotropy of the etched profiles obtained after various processes and a standard deviation of 0.06 μm was obtained for etch depth on 128 x 128 format array vias. The surface morphology and the uniformity of the etched surfaces were studied by plan view SEM. Atomic force microscopy was used to make precise assessments of surface roughness.

Isotope ratio analysis of individual sub-micrometer plutonium particles with inductively coupled plasma mass spectrometry.

PubMed

Esaka, Fumitaka; Magara, Masaaki; Suzuki, Daisuke; Miyamoto, Yutaka; Lee, Chi-Gyu; Kimura, Takaumi

2010-12-15

Information on plutonium isotope ratios in individual particles is of great importance for nuclear safeguards, nuclear forensics and so on. Although secondary ion mass spectrometry (SIMS) is successfully utilized for the analysis of individual uranium particles, the isobaric interference of americium-241 to plutonium-241 makes difficult to obtain accurate isotope ratios in individual plutonium particles. In the present work, an analytical technique by a combination of chemical separation and inductively coupled plasma mass spectrometry (ICP-MS) is developed and applied to isotope ratio analysis of individual sub-micrometer plutonium particles. The ICP-MS results for individual plutonium particles prepared from a standard reference material (NBL SRM-947) indicate that the use of a desolvation system for sample introduction improves the precision of isotope ratios. In addition, the accuracy of the (241)Pu/(239)Pu isotope ratio is much improved, owing to the chemical separation of plutonium and americium. In conclusion, the performance of the proposed ICP-MS technique is sufficient for the analysis of individual plutonium particles. Copyright © 2010 Elsevier B.V. All rights reserved.

Tandem Laser Induced Breakdown Spectroscopy (LIBS), Laser Ablation Inductively Coupled Plasma Mass Spectroscopy (LA-ICP-MS) and/or Laser Ablation Inductively Coupled Plasma Optical Emission Spectroscopy (LA-ICP-OES) for the analysis of samples of geological interest

NASA Astrophysics Data System (ADS)

Oropeza, D.

2016-12-01

A highly innovative laser ablation sampling instrument (J200 Tandem LA - LIBS) that combines the capabilities and analytical benefits of LIBS, LA-ICP-MS and LA-ICP-OES was used for micrometer-scale, spatially-resolved, elemental analysis of a wide variety of samples of geological interest. Data collected using ablation systems consisted of nanosecond (Nd:YAG operated 266nm) and femtosecond lasers (1030 and 343nm). An ICCD LIBS detector and Quadrupole based mass spectrometer were selected for LIBS and ICP-MS detection, respectively. This tandem instrument allows simultaneous determination of major and minor elements (for example, Si, Ca, Na, and Al, and trace elements such as Li, Ce, Cr, Sr, Y, Zn, Zr among others). The research also focused on elemental mapping and calibration strategies, specifically the use of emission and mass spectra for multivariate data analysis. Partial Least Square Regression (PLSR) is 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 study provides a benchmark to evaluate analytical results for more complex geological sample matrices.

Comparison of ion chromatographic methods based on conductivity detection, post-column-reaction and on-line-coupling IC-ICP-MS for the determination of bromate.

PubMed

Schminke, G; Seubert, A

2000-02-01

An established method for the determination of the disinfection by-product bromate is ion chromatography (IC). This paper presents a comparison of three IC methods based on either conductivity detection (IC-CD), a post-column-reaction (IC-PCR-VIS) or the on-line-coupling with inductively coupled plasma mass spectrometry (IC-ICP-MS). Main characteristics of the methods such as method detection limits (MDL), time of analysis and sample pretreatment are compared and applicability for routine analysis is critically discussed. The most sensitive and rugged method is IC-ICP-MS, followed by IC-PCR-VIS. The photometric detection is subject to a minor interference in real world samples, presumably caused by carbonate. The lowest sensitivity is shown by the IC-CD method as slowest method compared, which, in addition, requires a sample pretreatment. The highest amount of information is delivered by IC-PCR-VIS, which allows the simultaneous determination of the seven standard anions and bromate.

Uncertainty Measurement for Trace Element Analysis of Uranium and Plutonium Samples by Inductively Coupled Plasma-Atomic Emission Spectrometry (ICP-AES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gallimore, David L.

2012-06-13

The measurement uncertainty estimatino associated with trace element analysis of impurities in U and Pu was evaluated using the Guide to the Expression of Uncertainty Measurement (GUM). I this evalution the uncertainty sources were identified and standard uncertainties for the components were categorized as either Type A or B. The combined standard uncertainty was calculated and a coverage factor k = 2 was applied to obtain the expanded uncertainty, U. The ICP-AES and ICP-MS methods used were deveoped for the multi-element analysis of U and Pu samples. A typical analytical run consists of standards, process blanks, samples, matrix spiked samples,more » post digestion spiked samples and independent calibration verification standards. The uncertainty estimation was performed on U and Pu samples that have been analyzed previously as part of the U and Pu Sample Exchange Programs. Control chart results and data from the U and Pu metal exchange programs were combined with the GUM into a concentration dependent estimate of the expanded uncertainty. Comparison of trace element uncertainties obtained using this model was compared to those obtained for trace element results as part of the Exchange programs. This process was completed for all trace elements that were determined to be above the detection limit for the U and Pu samples.« less

Simulation of a large size inductively coupled plasma generator and comparison with experimental data

NASA Astrophysics Data System (ADS)

Lei, Fan; Li, Xiaoping; Liu, Yanming; Liu, Donglin; Yang, Min; Yu, Yuanyuan

2018-01-01

A two-dimensional axisymmetric inductively coupled plasma (ICP) model with its implementation in the COMSOL (Multi-physics simulation software) platform is described. Specifically, a large size ICP generator filled with argon is simulated in this study. Distributions of the number density and temperature of electrons are obtained for various input power and pressure settings and compared. In addition, the electron trajectory distribution is obtained in simulation. Finally, using experimental data, the results from simulations are compared to assess the veracity of the two-dimensional fluid model. The purpose of this comparison is to validate the veracity of the simulation model. An approximate agreement was found (variation tendency is the same). The main reasons for the numerical magnitude discrepancies are the assumption of a Maxwellian distribution and a Druyvesteyn distribution for the electron energy and the lack of cross sections of collision frequencies and reaction rates for argon plasma.

Assessment of heavy metal contamination in core sediment samples in Gulf of Izmir, Aegean Sea, Turkey (by inductively coupled plasma-optical emission spectrometry (ICP-OES))

NASA Astrophysics Data System (ADS)

Ünal Yumun, Zeki; Kam, Erol; Kurt, Dilek

2017-04-01

Heavy metal and radionuclide analysis studies are crucial in explaining biotic and abiotic interactions in ecosystems. This type of analysis is highly needed in environments such as coastal areas, gulfs or lakes where human activities are generally concentrated. Sediments are one of the best biological indicators for the environment since the pollution accumulates in the sediments by descent to the sea floor. In this study, sediments were collected from the Gulf of Izmir (Eastern Aegean Sea, Turkey) considering the accumulated points of domestic and industrial wastes to make an anthropogenic pollution analysis. The core sediments had different depths of 0.00-30.00 m at four different locations where Karsiyaka, Bayrakli, Incialti and Cesmealti in the Gulf of Izmir. The purpose of the study was determining Cd, Co, Cr, Cu, Mn, Ni, Pb, and Zn concentrations in the drilling samples to assess their levels and spatial distribution in crucial areas of the Aegean Sea by inductively coupled plasma-optical emission spectrometry (ICP-OES) with microwave digestion techniques. The heavy metal concentrations found in sediments varied for Cd: ICP-OES, pollution, sediment.

Inductively coupled plasma atomic emission spectrometric determination of tin in canned food.

PubMed

Sumitani, H; Suekane, S; Nakatani, A; Tatsuka, K

1993-01-01

Various canned foods were digested sequentially with HNO3 and HCl, diluted to 100 mL, and filtered, and then tin was determined by inductively coupled plasma atomic emission spectrometry (ICP/AES). Samples of canned Satsuma mandarin, peach, apricot, pineapple, apple juice, mushroom, asparagus, evaporated milk, short-necked clam, spinach, whole tomato, meat, and salmon were evaluated. Sample preparations did not require time-consuming dilutions, because ICP/AES has wide dynamic range. The standard addition method was used to determine tin concentration. Accuracy of the method was tested by analyzing analytical standards containing tin at 2 levels (50 and 250 micrograms/g). The amounts of tin found for the 50 and 250 micrograms/g levels were 50.5 and 256 micrograms/g, respectively, and the repeatability coefficients of variation were 4.0 and 3.8%, respectively. Recovery of tin from 13 canned foods spiked at 2 levels (50 and 250 micrograms/g) ranged from 93.9 to 109.4%, with a mean of 99.2%. The quantitation limit for tin standard solution was about 0.5 microgram/g.

Potentialities of mass spectrometry (ICP-MS) for actinides determination in urine.

PubMed

Bouvier-Capely, C; Ritt, J; Baglan, N; Cossonnet, C

2004-05-01

The applicability of inductively coupled plasma-mass spectrometry (ICP-MS) for determining actinides in urine was investigated. Performances of ICP-MS including detection limit and analysis time were studied and compared with alpha spectrometry performances. In the field of individual monitoring of workers, the comparison chart obtained in this study can be used as a guide for medical laboratories to select the most adequate procedure to be carried out depending on the case in question (the radioisotope to be measured, the required sensitivity, and the desired response time).

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

NASA Astrophysics Data System (ADS)

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

2012-10-01

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

Comparative study of atomic fluorescence spectroscopy and inductively coupled plasma mass spectrometry for mercury and arsenic multispeciation.

PubMed

Gómez-Ariza, José Luis; Lorenzo, Fernando; García-Barrera, Tamara

2005-05-01

Mercury and arsenic are two elements of undoubted importance owing to their toxic character. Although speciation of these elements has been developed separately, in this work for the first time the speciation of As and Hg using two atomic fluorescence detectors in a sequential ensemble is presented. A coupling based on the combination of high-performance liquid chromatography (where mercury and arsenic species are separated) and two atomic fluorescence detectors in series, with several online treatments, including photooxidation (UV) and hydride generation, has allowed the determination of mercury and arsenic compounds simultaneously. The detection limits for this device were 16, 3, 17, 12 and 8 ng mL(-1) for As(III), monomethylarsinic acid, As(V), Hg2+ and methylmercury, respectively. This coupling was compared with an analogous one based on inductively coupled plasma-mass spectrometry (ICP-MS) detection, with detection limits of 0.7, 0.5, 0.8, 0.9 and 1.1 ng mL(-1), respectively. Multispeciation based on ICP-MS exhibits better sensitivity than the coupling based on tandem atomic fluorescence, but this second device is a very robust system and exhibits obvious advantages related to the low cost of acquisition and maintenance, as well as easy handling, which makes it a suitable system for routine laboratories.

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

ERIC Educational Resources Information Center

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

2016-01-01

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

Characteristics of n-GaN After Cl2/Ar and Cl2/N2 Inductively Coupled Plasma Etching

NASA Astrophysics Data System (ADS)

Han, Yan-Jun; Xue, Song; Guo, Wen-Ping; Sun, Chang-Zheng; Hao, Zhi-Biao; Luo, Yi

2003-10-01

A systematic study on the effect of inductively coupled plasma (ICP) etching on n-type GaN is presented. The optical and electrical properties and surface stoichiometry of n-type GaN are evaluated using room-temperature photoluminescence (PL) and current-voltage (I-V) characteristic measurements, and X-ray photoelectron spectroscopy (XPS), respectively. Investigation of the effect of additive gas (N2 and Ar) and RF power on these characteristics has also been carried out. It is shown that the decrease in the O/Ga ratio after ICP etching can suppress the deterioration of the near-band-edge emission intensity. Furthermore, N vacancy (VN) with a shallow donor nature and Ga vacancy (VGa) with a deep acceptor nature are generated after ICP etching upon the addition of Ar and N2 to Cl2 plasma, respectively. Lower ohmic contact resistance could be obtained when VN or ion-bombardment-induced defect is dominant at the surface. Improved etching conditions have been obtained based on these results.

High-Temperature Isothermal Capacitance Transient Spectroscopy Study on Inductively Coupled Plasma Etching Damage for p-GaN Surfaces

NASA Astrophysics Data System (ADS)

Aoki, Toshichika; Wakayama, Hisashi; Kaneda, Naoki; Mishima, Tomoyoshi; Nomoto, Kazuki; Shiojima, Kenji

2013-11-01

The effects of the inductively coupled plasma (ICP) etching damage on the electrical characteristics of low-Mg-doped p-GaN Schottky contacts were evaluated by high-temperature isothermal capacitance transient spectroscopy. A large single peak for an acceptor-type surface state was dominantly detected for as-grown samples. The energy level and state density were obtained to be 1.18 eV above the valence band, which is close to a Ga vacancy (VGa), and 1.5×1013 cm-2, respectively. It was speculated that a small portion of Ga atoms were missing from the surface, and a high VGa density was observed in a few surface layers. The peak intensity decreased by 60% upon annealing at 800 °C, and further decrease was found by ICP etching. This decrease is consistent with the suppression of the memory effect in current-voltage characteristics. Upon annealing and ICP etching, since the VGa structure might be disordered, the peak intensity decreased.

High Resolution Studies of the Origins of Polyatomic Ions in Inductively Coupled Plasma-Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ferguson, Jill Wisnewski

2006-01-01

The inductively coupled plasma (ICP) is an atmospheric pressure ionization source. Traditionally, the plasma is sampled via a sampler cone. A supersonic jet develops behind the sampler, and this region is pumped down to a pressure of approximately one Torr. A skimmer cone is located inside this zone of silence to transmit ions into the mass spectrometer. The position of the sampler and skimmer cones relative to the initial radiation and normal analytical zones of the plasma is key to optimizing the useful analytical signal [1]. The ICP both atomizes and ionizes the sample. Polyatomic ions form through ion-molecule interactionsmore » either in the ICP or during ion extraction [l]. Common polyatomic ions that inhibit analysis include metal oxides (MO +), adducts with argon, the gas most commonly used to make up the plasma, and hydride species. While high resolution devices can separate many analytes from common interferences, this is done at great cost in ion transmission efficiency--a loss of 99% when using high versus low resolution on the same instrument [2]. Simple quadrupole devices, which make up the bulk of ICP-MS instruments in existence, do not present this option. Therefore, if the source of polyatomic interferences can be determined and then manipulated, this could potentially improve the figures of merit on all ICP-MS devices, not just the high resolution devices often utilized to study polyatomic interferences.« less

Exploration of robust operating conditions in inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

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

2003-11-01

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

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)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Al-Meer, S. H.; Amr, M. A.; Helal, A.I.

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. Themore » 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)« less

Improving Alpha Spectrometry Energy Resolution by Ion Implantation with ICP-MS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dion, Michael P.; Liezers, Martin; Farmer, Orville T.

2015-01-01

We report results of a novel technique using an Inductively Coupled Plasma Mass Spectrometer (ICP-MS) as a method of source preparation for alpha spectrometry. This method produced thin, contaminant free 241Am samples which yielded extraordinary energy resolution which appear to be at the lower limit of the detection technology used in this research.

Absolute measurements and certified reference material for iron isotopes using multiple-collector inductively coupled mass spectrometry.

PubMed

Zhou, Tao; Zhao, Motian; Wang, Jun; Lu, Hai

2008-01-01

Two enriched isotopes, 99.94 at.% 56Fe and 99.90 at.% 54Fe, were blended under gravimetric control to prepare ten synthetic isotope samples whose 56Fe isotope abundances ranged from 95% to 20%. For multiple-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) measurements typical polyatomic interferences were removed by using Ar and H2 as collision gas and operating the MC-ICP-MS system in soft mode. Thus high-precision measurements of the Fe isotope abundance ratios were accomplished. Based on the measurement of the synthetic isotope abundance ratios by MC-ICP-MS, the correction factor for mass discrimination was calculated and the results were in agreement with results from IRMM014. The precision of all ten correction factors was 0.044%, indicating a good linearity of the MC-ICP-MS method for different isotope abundance ratio values. An isotopic reference material was certified under the same conditions as the instrument was calibrated. The uncertainties of ten correction factors K were calculated and the final extended uncertainties of the isotopic certified Fe reference material were 5.8363(37) at.% 54Fe, 91.7621(51) at.% 56Fe, 2.1219(23) at.% 57Fe, and 0.2797(32) at.% 58Fe.

Spectroscopic Characteristic and Analytical Capability of Ar-N₂ Inductively Coupled Plasma in Axially Viewing Optical Emission Spectrometry.

PubMed

Ohata, Masaki

2016-01-01

The spectroscopic characteristics and analytical capability of argon-nitrogen (Ar-N2) inductively coupled plasma (ICP) in axially viewing optical emission spectrometry (OES) were examined and figures of merit were determined in the present study. The spectroscopic characteristics such as the emission intensity profile and the excitation temperature observed from the analytical zone of Ar-N2 ICP in axially viewing ICPOES, in order to elucidate the enhancement of the emission intensity of elements obtained in our previous study, were evaluated and compared to those of the standard ICP. The background and emission intensities of elements as well as their excitation behavior for both atom and ion lines were also examined. As results, a narrower emission intensity profile and an increased excitation temperature as well as enhancements for both background and emission intensities of elements, which could be due to the ICP shrunken as well as the enhancement of the interaction between the central channel of the ICP and samples introduced, were observed for Ar-N2 ICP in axially viewing OES. In addition, the elements with relatively higher excitation and ionization energies such as As, Bi, Cd, Ni, P, and Zn revealed larger enhancements of the emission intensities as well as improved limits of detection (LODs), which were also attributed to the enhanced interaction between Ar-N2 ICP and the samples. Since the Ar-N2 ICP could be obtained easily only by the addition of a small amount of N2 gas to the Ar plasma gas of the standard ICP and no optimization on the alignment between Ar-N2 ICP and the spectrometer in commercially available ICPOES instruments was needed, it could be utilized as simple and optional excitation and ionization sources in axially viewing ICPOES.

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

USGS Publications Warehouse

Garbarino, John R.

2000-01-01

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

Analysis of Inorganic Nanoparticles by Single-particle Inductively Coupled Plasma Time-of-Flight Mass Spectrometry.

PubMed

Hendriks, Lyndsey; Gundlach-Graham, Alexander; Günther, Detlef

2018-04-25

Due to the rapid development of nanotechnologies, engineered nanomaterials (ENMs) and nanoparticles (ENPs) are becoming a part of everyday life: nanotechnologies are quickly migrating from laboratory benches to store shelves and industrial processes. As the use of ENPs continues to expand, their release into the environment is unavoidable; however, understanding the mechanisms and degree of ENP release is only possible through direct detection of these nanospecies in relevant matrices and at realistic concentrations. Key analytical requirements for quantitative detection of ENPs include high sensitivity to detect small particles at low total mass concentrations and the need to separate signals of ENPs from a background of dissolved elemental species and natural nanoparticles (NNPs). To this end, an emerging method called single-particle inductively coupled plasma mass spectrometry (sp-ICPMS) has demonstrated great potential for the characterization of inorganic nanoparticles (NPs) at environmentally relevant concentrations. Here, we comment on the capabilities of modern sp-ICPMS analysis with particular focus on the measurement possibilities offered by ICP-time-of-flight mass spectrometry (ICP-TOFMS). ICP-TOFMS delivers complete elemental mass spectra for individual NPs, which allows for high-throughput, untargeted quantitative analysis of dispersed NPs in natural matrices. Moreover, the multi-element detection capabilities of ICP-TOFMS enable new NP-analysis strategies, including online calibration via microdroplets for accurate NP mass quantification and matrix compensation.

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

USGS Publications Warehouse

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

2009-01-01

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

Self-consistent multidimensional electron kinetic model for inductively coupled plasma sources

NASA Astrophysics Data System (ADS)

Dai, Fa Foster

Inductively coupled plasma (ICP) sources have received increasing interest in microelectronics fabrication and lighting industry. In 2-D configuration space (r, z) and 2-D velocity domain (νθ,νz), a self- consistent electron kinetic analytic model is developed for various ICP sources. The electromagnetic (EM) model is established based on modal analysis, while the kinetic analysis gives the perturbed Maxwellian distribution of electrons by solving Boltzmann-Vlasov equation. The self- consistent algorithm combines the EM model and the kinetic analysis by updating their results consistently until the solution converges. The closed-form solutions in the analytical model provide rigorous and fast computing for the EM fields and the electron kinetic behavior. The kinetic analysis shows that the RF energy in an ICP source is extracted by a collisionless dissipation mechanism, if the electron thermovelocity is close to the RF phase velocities. A criterion for collisionless damping is thus given based on the analytic solutions. To achieve uniformly distributed plasma for plasma processing, we propose a novel discharge structure with both planar and vertical coil excitations. The theoretical results demonstrate improved uniformity for the excited azimuthal E-field in the chamber. Non-monotonic spatial decay in electric field and space current distributions was recently observed in weakly- collisional plasmas. The anomalous skin effect is found to be responsible for this phenomenon. The proposed model successfully models the non-monotonic spatial decay effect and achieves good agreements with the measurements for different applied RF powers. The proposed analytical model is compared with other theoretical models and different experimental measurements. The developed model is also applied to two kinds of ICP discharges used for electrodeless light sources. One structure uses a vertical internal coil antenna to excite plasmas and another has a metal shield to prevent the

Determination of tin isotope ratios in cassiterite by femtosecond laser ablation multicollector inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Schulze, Marie; Ziegerick, Marco; Horn, Ingo; Weyer, Stefan; Vogt, Carla

2017-04-01

In comparison to isotope analysis of dissolved samples femtosecond laser ablation multicollector inductively coupled plasma mass spectrometry (fs-LA-MC-ICP-MS) enables precise isotope ratio analyses consuming much less sample material and with a minimum effort in sample preparation. This is especially important for the investigation of valuable historical objects for which visual traces of sampling are unwanted. The present study provides a basis for tin isotope ratio measurements using LA-MC-ICP-MS technique. For this, in house isotope standards had to be defined. Investigations on interferences and matrix effects illustrate that beside Sb only high Te contents (with values above those to be expected in cassiterite) result in a significant shift of the measured tin isotope ratios. This effect can partly be corrected for using natural isotope abundances. However, a natural isotope fractionation of Te cannot be excluded. Tin beads reduced from cassiterite were analysed by laser ablation and after dissolution. It was shown that tin isotope ratios can be determined accurately by using fs-LA-MC-ICP-MS. Furthermore the homogeneity of tin isotope ratios in cassiterite was proven.

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

PubMed

Lin, Li; Chen, Guang; Chen, Yuhong

2011-07-01

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

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

PubMed

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 <0.0001 to 752.7 μg L(-1). The 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.

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

PubMed Central

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 < 5.8. Linearity value for calibration curve of each metal was 1 > 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 < smoked < sniffing < dipping. However, smoked and sniffing will interchange their position in the case of Mn, Cu, Se and Cd. Multivariate statistical analyses were also performed to evaluate the correlation and variations among tobacco products. Conclusions The present study highlights the quantification of some important metals and metalloids in a wide spectrum of tobacco formulations. The outcome of this study would be beneficial for health authorities and individuals. PMID:22709464

A candidate reference method for serum potassium measurement by inductively coupled plasma mass spectrometry.

PubMed

Yan, Ying; Han, Bingqing; Zeng, Jie; Zhou, Weiyan; Zhang, Tianjiao; Zhang, Jiangtao; Chen, Wenxiang; Zhang, Chuanbao

2017-08-28

Potassium is an important serum ion that is frequently assayed in clinical laboratories. Quality assurance requires reference methods; thus, the establishment of a candidate reference method for serum potassium measurements is important. An inductively coupled plasma mass spectrometry (ICP-MS) method was developed. Serum samples were gravimetrically spiked with an aluminum internal standard, digested with 69% ultrapure nitric acid, and diluted to the required concentration. The 39K/27Al ratios were measured by ICP-MS in hydrogen mode. The method was calibrated using 5% nitric acid matrix calibrators, and the calibration function was established using the bracketing method. The correlation coefficients between the measured 39K/27Al ratios and the analyte concentration ratios were >0.9999. The coefficients of variation were 0.40%, 0.68%, and 0.22% for the three serum samples, and the analytical recovery was 99.8%. The accuracy of the measurement was also verified by measuring certified reference materials, SRM909b and SRM956b. Comparison with the ion selective electrode routine method and international inter-laboratory comparisons gave satisfied results. The new ICP-MS method is specific, precise, simple, and low-cost, and it may be used as a candidate reference method for standardizing serum potassium measurements.

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

NASA Astrophysics Data System (ADS)

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

2015-03-01

The applicability of laser ablation multi-collector inductively coupled plasma-mass spectrometry (LA-MC-ICP-MS) for the determination of the B isotopic composition in Roman glasses was investigated. The δ11B values thus obtained provide information on the natron flux used during the glass-making process. The glass samples used for this purpose were previously characterized using pneumatic nebulization (PN) MC-ICP-MS. Unfortunately, this method is time-consuming and labor-intensive and consumes some 100 mg of sample, which is a rather high amount for ancient materials. Therefore, the use of the less invasive and faster LA-MC-ICP-MS approach was explored. In this work, the results for 29 Roman glasses and 4 home-made glasses obtained using both techniques were compared to assess the suitability of LA-MC-ICP-MS in this context. The results are in excellent agreement within experimental uncertainty. No difference in overall mass discrimination was observed between the Roman glasses, NIST SRM 610 reference glass and B6 obsidian. The expanded uncertainty of the LA-MC-ICP-MS approach was estimated to be < 2‰, which is similar to that obtained upon sample digestion and PN-MC-ICP-MS measurement.

Analysis of trace metals in water by inductively coupled plasma emission spectrometry using sodium dibenzyldithiocarbamate for preconcentration

USGS Publications Warehouse

Smith, C.L.; Motooka, J.M.; Willson, W.R.

1984-01-01

Since concentrations of trace elements in most natural waters seldom exceed the ??g/L level, analysis of trace elements in natural waters by inductively coupled plasma emission spectrometry (ICP) requires a preconcentration procedure. The elements Ag, Bi, Cd, Co, Cu, Fe, Mo, Ni, Pb, Sn, V, W, and Zn were separated and concentrated from 500 mL of water by coprecipitating them with sodium dibenzyldithiocarbamate (NaDBDTC) using nickel or silver as a carrier. The precipitated trace elements were collected on a membrane filter, redissolved from the filter with hot nitric and hydrochloric acids, and analyzed using ICP. Recoveries for all the trace elements except tungsten exceeded 80%. Coprecipitation of trace elements with NaDBDTC eliminated the use of difficult-to-inject organic solvents, and NaDBDTC coprecipitated a wider array of trace elements than ammoniumpyrrolidinedithiocarbamate (APDC), another commonly used coprecipitate.

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

NASA Astrophysics Data System (ADS)

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

2008-11-01

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

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

PubMed

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

2015-07-23

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

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION AND MAINTENANCE OF THE JOBIN-YVON MODEL 70 INDUCTIVELY COUPLED PLASMA ATOMIC ABSORPTION SPECTROMETER (BCO-L-7.1)

EPA Science Inventory

The purpose of this SOP is to detail the operation and maintenance of an Instruments, SA Inc., Jobin-Yvon Model 70 (JY-70) inductively coupled plasma atomic emissions spectrometry (ICP-AES). This procedure was followed to ensure consistent data retrieval during the Arizona NHEXA...

Evaluation of a tunable bandpass reaction cell for an inductively coupled plasma mass spectrometer for the determination of chromium and vanadium in serum and urine

NASA Astrophysics Data System (ADS)

Nixon, David E.; Neubauer, Kenneth R.; Eckdahl, Steven J.; Butz, John A.; Burritt, Mary F.

2002-05-01

A Dynamic Reaction Cell™ inductively coupled argon plasma mass spectrometer (DRC-ICP-MS) was evaluated for the determination of chromium and vanadium in serum and urine. Reaction cell conditions were evaluated for the elimination of ArC + and ClOH + interferences on chromium at mass 52 and OCl + on vanadium at mass 51. A diluent containing only 1% nitric acid and internal standards (Y and Ga) was used to prepare serum and urine for analysis. Instrument response calibration was achieved by using aqueous acidic standards spiked into pooled sera or urine matrices. The slopes of the calibration curves prepared in urine and serum matrices were nearly identical. On average, chromium detection limits are 2.5 times lower using the DRC than Zeeman graphite furnace atomic absorption spectrometry (ZGFAAS). Vanadium detection limits are approximately 50 times lower. Average detection limits achieved with DRC-ICP-MS are 0.075 μg Cr/l and 0.028 μg V/l. Average results for the analysis of National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1598 Bovine Serum (attained over 22 days) are: 0.14 μg Cr/l and 0.068 μg V/l. The reference concentrations for vanadium and chromium in NIST SRM 1598 are (0.06) μg V/l and 0.14±0.08 μg Cr/l, respectively. Results for chromium and vanadium determinations on ICP-MS survey samples from the Toxocologie du Quebec are equivalent to those reported by high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for the same survey samples.

Development of Desolvation System for Single-cell Analysis Using Droplet Injection Inductively Coupled Plasma Atomic Emission Spectroscopy.

PubMed

Ishihara, Yukiko; Aida, Mari; Nomura, Akito; Miyahara, Hidekazu; Hokura, Akiko; Okino, Akitoshi

2015-01-01

With a view to enhance the sensitivity of analytical instruments used in the measurement of trace elements contained in a single cell, we have now equipped the previously reported micro-droplet injection system (M-DIS) with a desolvation system. This modified M-DIS was coupled to inductively coupled plasma atomic emission spectroscopy (ICP-AES) and evaluated for its ability to measure trace elements. A flow rate of 100 mL/min for the additional gas and a measurement point -7.5 mm above the load coil (ALC) have been determined to be the optimal parameters for recording the emission intensity of the Ca(II) spectral lines. To evaluate the influence of the desolvation system, we recorded the emission intensities of the Ca(I), Ca(II), and H-β spectral lines with and without inclusion of the desolvation system. The emission intensity of the H-β spectral line reduces and the magnitude of the Ca(II)/Ca(I) emission intensity ratio increases four-fold with inclusion of the desolvation system. Finally, the elements Ca, Mg, and Fe present in a single cell of Pseudococcomyxa simplex are simultaneously determined by coupling the M-DIS equipped with the desolvation system to ICP-AES.

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

PubMed

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.

Analysis of high-purity germanium dioxide by ETV-ICP-AES with preliminary concentration of trace elements.

PubMed

Medvedev, Nickolay S; Shaverina, Anastasiya V; Tsygankova, Alphiya R; Saprykin, Anatoly I

2016-08-01

The paper presents a combined technique of germanium dioxide analysis by inductively coupled plasma atomic emission spectrometry (ICP-AES) with preconcentration of trace elements by distilling off matrix and electrothermal (ETV) introduction of the trace elements concentrate into the ICP. Evaluation of metrological characteristics of the developed technique of high-purity germanium dioxide analysis was performed. The limits of detection (LODs) for 25 trace elements ranged from 0.05 to 20ng/g. The accuracy of proposed technique is confirmed by "added-found" («or spiking») experiment and comparing the results of ETV-ICP-AES and ICP-AES analysis of high purity germanium dioxide samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

Kaiser, J.; Galiová, M.; Novotný, K.; Červenka, R.; Reale, L.; Novotný, J.; Liška, M.; Samek, O.; Kanický, V.; Hrdlička, A.; Stejskal, K.; Adam, V.; Kizek, R.

2009-01-01

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

Silicon macroporous arrays with high aspect ratio prepared by ICP etching

NASA Astrophysics Data System (ADS)

Wang, Guozheng; Yang, Bingchen; Wang, Ji; Yang, Jikai; Duanmu, Qingduo

2018-02-01

This paper reports on a macroporous silicon arrays with high aspect ratio, the pores of which are of 162, 205, 252, 276μm depths with 6, 10, 15 and 20 μm diameters respectively, prepared by Multiplex Inductively Coupled Plasma (ICP) etching. It was shown that there are very differences in process of high aspect ratio microstructures between the deep pores, a closed structure, and deep trenches, a open structure. The morphology and the aspect ratio dependent etching were analyzed and discussed. The macroporous silicon etched by ICP process yield an uneven, re-entrant, notched and ripples surface within the pores. The main factors effecting on the RIE lag of HARP etching are the passivation cycle time, the pressure of reactive chamber, and the platen power of ICP system.

A concise guide for the determination of less-studied technology-critical elements (Nb, Ta, Ga, In, Ge, Te) by inductively coupled plasma mass spectrometry in environmental samples

NASA Astrophysics Data System (ADS)

Filella, Montserrat; Rodushkin, Ilia

2018-03-01

There is an increasing demand for analytical techniques able to measure so-called 'technology-critical elements', a set of chemical elements increasingly used in technological applications, in environmental matrices. Nowadays, inductively coupled plasma-mass spectrometry (ICP-MS) has become the technique of choice for measuring trace element concentrations. However, its application is often less straightforward than often assumed. The hints and drawbacks of ICP-MS application to the measurement of a set of less-studied technology-critical elements (Nb, Ta, Ga, In, Ge and Te) is discussed here and concise guidelines given.

Inductively coupled wireless RF coil arrays.

PubMed

Bulumulla, S B; Fiveland, E; Park, K J; Foo, T K; Hardy, C J

2015-04-01

As the number of coils increases in multi-channel MRI receiver-coil arrays, RF cables and connectors become increasingly bulky and heavy, degrading patient comfort and slowing workflow. Inductive coupling of signals provides an attractive "wireless" approach, with the potential to reduce coil weight and cost while simplifying patient setup. In this work, multi-channel inductively coupled anterior arrays were developed and characterized for 1.5T imaging. These comprised MR receiver coils inductively (or "wirelessly") linked to secondary or "sniffer" coils whose outputs were transmitted via preamps to the MR system cabinet. The induced currents in the imaging coils were blocked by passive diode circuits during RF transmit. The imaging arrays were totally passive, obviating the need to deliver power to the coils, and providing lightweight, untethered signal reception with easily positioned coils. Single-shot fast spin echo images were acquired from 5 volunteers using a 7-element inductively coupled coil array and a conventionally cabled 7-element coil array of identical geometry, with the inductively-coupled array showing a relative signal-to-noise ratio of 0.86 +/- 0.07. The concept was extended to a larger 9-element coil array to demonstrate the effect of coil element size on signal transfer and RF-transmit blocking. Copyright © 2015 Elsevier Inc. All rights reserved.

Vacuum ultraviolet photon fluxes in argon-containing inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Radovanov, S. B.; Persing, H. M.; Wang, S.; Culver, C. L.; Boffard, J. B.; Lin, C. C.; Wendt, A. E.

2013-09-01

Vacuum ultraviolet (VUV) photons emitted from excited atomic states are ubiquitous in material processing plasmas. Damage of materials is induced by energy transfer from the VUV photons to the surface, causing disorder in the surface region, surface reactions, and affecting bonds in the material bulk. Monitoring of the surface flux of VUV photons from inductively coupled plasmas (ICP) and its dependence on discharge parameters is thus highly desirable. Results of non-invasive, direct windowless VUV detection using a photosensitive diode will be presented. Relative VUV fluxes were also obtained using a sodium salicylate coating on the inside of a vacuum window, converting VUV into visible light detected through the vacuum window. The coating is sensitive to wavelengths in the range 80-300 nm, while the photodiode is only sensitive to wavelengths below 120 nm. In argon the VUV emissions are primarily produced by spontaneous decay from 3p5 4 s resonance levels (1s2,1s4) and may be reabsorbed by ground state atoms. Real-time resonance level concentrations were measured and used to predict the VUV photon flux at the detector for a range of different ICP pressures, powers, and for various admixtures of Ar with N2, and H2. This work was supported in part by NSF grant PHY-1068670.

Inductively and capacitively coupled plasmas at interface: A comparative study towards highly efficient amorphous-crystalline Si solar cells

NASA Astrophysics Data System (ADS)

Guo, Yingnan; Ong, Thiam Min Brian; Levchenko, I.; Xu, Shuyan

2018-01-01

A comparative study on the application of two quite different plasma-based techniques to the preparation of amorphous/crystalline silicon (a-Si:H/c-Si) interfaces for solar cells is presented. The interfaces were fabricated and processed by hydrogen plasma treatment using the conventional plasma-enhanced chemical vacuum deposition (PECVD) and inductively coupled plasma chemical vapour deposition (ICP-CVD) methods The influence of processing temperature, radio-frequency power, treatment duration and other parameters on interface properties and degree of surface passivation were studied. It was found that passivation could be improved by post-deposition treatment using both ICP-CVD and PECVD, but PECVD treatment is more efficient for the improvement on passivation quality, whereas the minority carrier lifetime increased from 1.65 × 10-4 to 2.25 × 10-4 and 3.35 × 10-4 s after the hydrogen plasma treatment by ICP-CVD and PECVD, respectively. In addition to the improvement of carrier lifetimes at low temperatures, low RF powers and short processing times, both techniques are efficient in band gap adjustment at sophisticated interfaces.

Low gas flow inductively coupled plasma optical emission spectrometry for the analysis of food samples after microwave digestion.

PubMed

Nowak, Sascha; Gesell, Monika; Holtkamp, Michael; Scheffer, Andy; Sperling, Michael; Karst, Uwe; Buscher, Wolfgang

2014-11-01

In this work, the recently introduced low flow inductively coupled plasma optical emission spectrometry (ICP-OES) with a total argon consumption below 0.7 L/min is applied for the first time to the field of food analysis. One goal is the investigation of the performance of this low flow plasma compared to a conventional ICP-OES system when non-aqueous samples with a certain matrix are introduced into the system. For this purpose, arsenic is determined in three different kinds of fish samples. In addition several nutrients (K, Na, Mg, Ca) and trace metals (Co, Cu, Mn, Cd, Pb, Zn, Fe, and Ni) are determined in honey samples (acacia) after microwave digestion. The precision of the measurements is characterized by relative standard deviations (RSD) and compared to the corresponding precision values achieved using the conventional Fassel-type torch of the ICP. To prove the accuracy of the low flow ICP-OES method, the obtained data from honey samples are validated by a conventional ICP-OES. For the measurements concerning arsenic in fish, the low flow ICP-OES values are validated by conventional Fassel-type ICP-OES. Furthermore, a certified reference material was investigated with the low gas flow setup. Limits of detection (LOD), according to the 3σ criterion, were determined to be in the low microgram per liter range for all analytes. Recovery rates in the range of 96-106% were observed for the determined trace metal elements. It was proven that the low gas flow ICP-OES leads to results that are comparable with those obtained with the Fassel-type torch for the analysis of food samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Feasibility of Rare Earth Element Determination in Low Concentration in Crude Oil: Direct Sampling Electrothermal Vaporization-Inductively Coupled Plasma Mass Spectrometry.

PubMed

Silva, Jussiane Souza; Schneider Henn, Alessandra; Dressler, Valderi Luiz; Mello, Paola Azevedo; Flores, Erico Marlon Moraes

2018-06-05

A comprehensive study was developed showing the feasibility of determination of rare earth elements (REE) in low concentration in crude oil by using direct sampling electrothermal vaporization system coupled to inductively coupled plasma mass spectrometry (ETV-ICP-MS). The effect of organic modifier on the REE signal was evaluated and the use of 6 mg of citric acid allowed calibration using aqueous reference solutions (selected pyrolysis and vaporization temperatures were 700 and 2200 °C, respectively). Because of the facility of REE in forming refractory compounds inside the graphite furnace during the heating step, the use of a modifier gas (Freon R-12, 3.0 mL min -1 ) was necessary to allow quantitative vaporization of these elements. A flow rate of 0.40 L min -1 was selected for both bypass and carrier gases. Under optimized conditions, the influence of sample mass was evaluated, and even using a relatively high mass of crude oil (up to 18 mg), accurate results were obtained. The accuracy was evaluated by the comparison of results by ETV-ICP-MS with those obtained by ICP-MS with ultrasonic nebulizer (USN) after high-pressure microwave-assisted wet digestion (MAWD) and microwave-induced combustion (MIC) and no statistical difference was observed between the results. The limits of quantification for REE by ETV-ICP-MS were lower (0.02-0.8 ng g -1 ) than those obtained by USN-ICP-MS after MAWD and MIC (0.6-5.1 ng g -1 ). Negligible blank values and relative standard deviations lower than 12% show the feasibility of the proposed ETV-ICP-MS method for routine analysis of crude oil.

Investigation of heavy-metal accumulation in selected plant samples using laser induced breakdown spectroscopy and laser ablation inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Galiová, M.; Kaiser, J.; Novotný, K.; Novotný, J.; Vaculovič, T.; Liška, M.; Malina, R.; Stejskal, K.; Adam, V.; Kizek, R.

2008-12-01

Single-pulse Laser-Induced Breakdown Spectroscopy (LIBS) and Laser-Ablation Inductively Coupled Plasma Mass-Spectrometry (LA-ICP-MS) were applied for mapping the silver and copper distribution in Helianthus Annuus L. samples treated with contaminant in controlled conditions. For Ag and Cu detection the 328.07 nm Ag(I) and 324.75 nm Cu(I) lines were used, respectively. The LIBS experimental conditions (mainly the laser energy and the observation window) were optimized in order to avoid self-absorption effect in the measured spectra. In the LA-ICP-MS analysis the Ag 107 and Cu 63 isotopes were detected. The capability of these two analytical techniques for high-resolution mapping of selected trace chemical elements was demonstrated.

Synthesis of Silicon Nanoparticles in Inductively Coupled Plasmas

NASA Astrophysics Data System (ADS)

Markosyan, Aram H.; Le Picard, Romain; Girshick, Steven L.; Kushner, Mark J.

2016-09-01

The synthesis of silicon nanoparticles (Si-NPs) is being investigated for their use in photo-emitting electronics, photovoltaics, and biotechnology. The ability to control the size and mono-disperse nature of Si-NPs is important to optimizing these applications. In this paper we discuss results from a computational investigation of Si-NP formation and growth in an inductively coupled plasma (ICP) reactor with the goal of achieving this control. We use a two dimensional numerical model where the algorithms for the kinetics of NP formation are self-consistently coupled with a plasma hydrodynamics simulation. The reactor modeled here resembles a GEC reference cell through which, for the base case, a mixture of Ar/SiH4 = 70/30 flows at 150 sccm at a pressure of 100 mTorr. In continuous wave mode, three coils located on top of the reactor deliver 150 W. The electric plasma potential confines negatively charged particles at the center of the discharge, increasing the residence time of negative NPs, which enables the NPs to potentially grow to large and controllable sizes of many to 100s nm. We discuss methods of controlling NP growth rates by varying the mole fraction and flow rate of SiH4, and using a pulsed plasma by varying the pulse period and duty cycle. Work supported by DOE Office of Fusion Energy Science and National Science Foundation.

Resolution of rare earth element interferences in fossil energy by-product samples using sector-field ICP-MS

DOE PAGES

Thompson, Robert L.; Bank, Tracy; Roth, Elliot; ...

2016-07-30

Here, the supply and price of rare earth elements (REEs) have become a concern to many countries in the world, which has led to renewed interest in exploration and recovery of REEs from secondary or waste sources. Potential high REE waste sources that are of particular interest are coal mining, preparation, combustion, and other fossil energy by-products, including those from natural gas production. In this work, we have examined a set of five solid samples from the treatment of produced and flowback water containing elevated concentrations of barium. In order to confirm the correct concentrations of Eu, we studied thesemore » materials using sector field inductively coupled plasma mass spectrometry (SF-ICP-MS), which is capable of resolving species of nearly identical masses, including Eu and BaO. While the use of quadrupole inductively coupled plasma mass spectrometry (Q-ICP-MS) for the REE analysis of most geological sample matrices should pose no problem, the presence of large amounts of Ba, as encountered in water treatment solids from natural gas produced and flowback samples may require SF-ICP-MS for accurate determination of all REEs.« less

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.

PubMed

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

Étude comparative des techniques d'analyse par fluorescence X à dispersion d'énergie (ED-XRF) et à dispersion de longueur d'onde (WD-XRF), et par spectrométrie d'émission atomique à source plasma couplée par induction (ICP-AES)

NASA Astrophysics Data System (ADS)

Rahmani, A.; Benyaïch, F.; Bounakhla, M.; Bilal, E.; Moutte, J.; Gruffat, J. J.; Zahry, F.

2004-11-01

Dans ce travail, nous présentons une étude comparative des techniques d'analyse par fluorescence X à dispersion d'énergie (ED-XRF) et à dispersion de longueur d'onde (WD-XRF), et par spectrométrie d'émission atomique à source plasma couplée par induction (ICP-AES). Les résultats de la calibration des spectromètres à dispersion d'énergie, à excitation par sources radioactives (55Fe, 109Cd et 241Am) et à excitation secondaire (cible secondaire Mo et Cu) du Centre National pour l'Energie, les Sciences et les Techniques Nucléaires (CNESTEN, Rabat, Maroc) sur des échantillons étalons de références de l'Agence International de l'Energie Atomique (AIEA) et du Community Bureau of Référence (BCR) ont été comparés aux résultats d'analyse des mêmes échantillons étalons par la spectrométrie X à dispersion de longueur d'onde (WD-XRF) et par spectrométrie d'émission atomique à source plasma couplé par induction (ICP-AES) au département GENERIC du centre SPIN à l'Ecole des Mines de Saint-Etienne (France). Les trois techniques d'analyse utilisées donnent des résultats comparables pour le dosage des éléments majeurs, alors que pour les traces on note des déviations importantes à cause des effets de matrice qui sont difficiles à corriger dans le cas de la fluorescence X.

U.S.-MEXICO BORDER PROGRAM ARIZONA BORDER STUDY--STANDARD OPERATING PROCEDURE FOR OPERATION, CALIBRATION, AND MAINTENANCE OF THE JOBIN-YVON MODEL 70 INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION SPECTROMETER (BCO-L-7.1)

EPA Science Inventory

The purpose of this SOP is to detail the operation and maintenance of an Instruments, SA Inc., Jobin-Yvon Model 70 (JY-70) inductively coupled plasma atomic emissions spectrometry (ICP-AES). This procedure was followed to ensure consistent data retrieval during the Arizona NHEXA...

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

PubMed

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

2015-11-27

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

Comparison of Analytical Methods for the Determination of Uranium in Seawater Using Inductively Coupled Plasma Mass Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wood, Jordana R.; Gill, Gary A.; Kuo, Li-Jung

2016-04-20

Trace element determinations in seawater by inductively coupled plasma mass spectrometry are analytically challenging due to the typically very low concentrations of the trace elements and the potential interference of the salt matrix. In this study, we did a comparison for uranium analysis using inductively coupled plasma mass spectrometry (ICP-MS) of Sequim Bay seawater samples and three seawater certified reference materials (SLEW-3, CASS-5 and NASS-6) using seven different analytical approaches. The methods evaluated include: direct analysis, Fe/Pd reductive precipitation, standard addition calibration, online automated dilution using an external calibration with and without matrix matching, and online automated pre-concentration. The methodmore » which produced the most accurate results was the method of standard addition calibration, recovering uranium from a Sequim Bay seawater sample at 101 ± 1.2%. The on-line preconcentration method and the automated dilution with matrix-matched calibration method also performed well. The two least effective methods were the direct analysis and the Fe/Pd reductive precipitation using sodium borohydride« less

Preliminary investigation of electrothermal vaporization sample introduction for inductively coupled plasma time-of-flight mass spectrometry.

PubMed

Mahoney, P P; Ray, S J; Li, G; Hieftje, G M

1999-04-01

The coupling of an electrothermal vaporization (ETV) apparatus to an inductively coupled plasma time-of-flight mass spectrometer (ICP-TOFMS) is described. The ability of the ICP-TOFMS to produce complete elemental mass spectra at high repetition rates is experimentally demonstrated. A signal-averaging data acquisition board is employed to rapidly record complete elemental spectra throughout the vaporization stage of the ETV temperature cycle; a solution containing 34 elements is analyzed. The reduction of both molecular and atomic isobaric interferences through the temperature program of the furnace is demonstrated. Isobaric overlaps among the isotopes of cadmium, tin, and indium are resolved by exploiting differences in the vaporization characteristics of the elements. Figures of merit for the system are defined with several different data acquisition schemes capable of operating at the high repetition rate of the TOF instrument. With the use of both ion counting and a boxcar averager, the dynamic range is shown to be linear over a range of at least 6 orders of magnitude. A pair of boxcar averagers are used to measure the isotope ratio for silver with a precision of 1.9% RSD, despite a cycle-to-cycle precision of 19% RSD. Detection limits of 10-80 fg are calculated for seven elements, based upon a 10-microL injection.

Application of ICP-OES for Evaluating Energy Extraction and Production Wastewater Discharge Impacts on Surface Waters in Western Pennsylvania

EPA Science Inventory

Oil and gas extraction and coal-fired electrical power generating stations produce wastewaters that are treated and discharged to rivers in Western Pennsylvania with public drinking water system (PDWS) intakes. Inductively coupled plasma optical emission spectroscopy (ICP-OES) w...

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

PubMed

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.

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

PubMed

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

2016-01-01

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

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

NASA Astrophysics Data System (ADS)

Larsen, Erik H.

1998-02-01

Achievement of optimum selectivity, sensitivity and robustness in speciation analysis using high performance liquid chromatography (HPLC) with inductively coupled mass spectrometry (ICP-MS) detection requires that each instrumental component is selected and optimized with a view to the ideal operating characteristics of the entire hyphenated system. An isocratic HPLC system, which employs an aqueous mobile phase with organic buffer constituents, is well suited for introduction into the ICP-MS because of the stability of the detector response and high degree of analyte sensitivity attained. Anion and cation exchange HPLC systems, which meet these requirements, were used for the seperation of selenium and arsenic species in crude extracts of biological samples. Furthermore, the signal-to-noise ratios obtained for these incompletely ionized elements in the argon ICP were further enhanced by a factor of four by continously introducing carbon as methanol via the mobile phase into the ICP. Sources of error in the HPLC system (column overload), in the sample introduction system (memory by organic solvents) and in the ICP-MS (spectroscopic interferences) and their prevention are also discussed. The optimized anion and cation exchange HPLC-ICP-MS systems were used for arsenic speciation in contaminated ground water and in an in-house shrimp reference sample. For the purpose of verification, HPLC coupled with tandem mass spectrometry with electrospray ionization was additionally used for arsenic speciation in the shrimp sample. With this analytical technique the HPLC retention time in combination with mass analysis of the molecular ions and their collision-induced fragments provide almost conclusive evidence of the identity of the analyte species. The speciation methods are validated by establishing a mass balance of the analytes in each fraction of the extraction procedure, by recovery of spikes and by employing and comparing independent techniques. The urgent need for

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

PubMed

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.

The separation of 99Tc from low and medium-level radioactive wastes and its determination by inductively coupled plasma mass spectrometry.

PubMed

Hepiegne, P; Dall'ava, D; Clement, R; Degros, J P

1995-06-01

A chemical separation method has been developed for the determination of (99)Tc in various types of radioactive wastes. Such a method includes (i) fusion with NaOH, (ii) extraction in a column containing methyltrioctylammonium chloride, (iii) extraction by solvent with N-benzoyl-N-phenylhydroxylamine and, (iv) measurement by inductively-coupled plasma mass spectrometry (ICP-MS). From the performance standpoint, the recovery of (99)Tc, using (99m)Tc as a yield tracer, is higher than 70%. This analytical method, as developed, ensures effective decontamination with respect to the radionuclides, insofar the decontamination factors are greater than 10(+5), whenever the residual activity may be measured. Taking into account a 3sigma counting error, the detection limit obtained with the ICP-MS technique is 1.9 mBq/ml; the method enabling hence to detect activities as low as 0.3 Bq/g, with analysed samples of 0.2 g and a radiochemical yield of 70%. Studies have been dedicated to the (99)Tc measurement, using the electrothermal vaporization ICP-MS technique, which lowers the detection limit by a factor 10, with the standard solution (0.3 pg/ml), compared with the previous ICP-MS technique.

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

NASA Astrophysics Data System (ADS)

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.

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

NASA Astrophysics Data System (ADS)

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

2011-05-01

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

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

USGS Publications Warehouse

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

1987-01-01

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

Determination of mercury compounds in fish by microwave-assisted extraction and liquid chromatography-vapor generation-inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Chiou, Chwei-Sheng; Jiang, Shiuh-Jen; Kumar Danadurai, K. Suresh

2001-07-01

A method employing a vapor generation system and LC combined with inductively coupled plasma mass spectrometry (LC-ICP-MS) is presented for the determination of mercury in biological tissues. An open vessel microwave digestion system was used to extract the mercury compounds from the sample matrix. The efficiency of the mobile phase, a mixture of L-cysteine and 2-mercaptoethanol, was evaluated for LC separation of inorganic mercury [Hg(II)], methylmercury (methyl-Hg) and ethylmercury (ethyl-Hg). The sensitivity, detection limits and repeatability of the liquid chromatography (LC) ICP-MS system with a vapor generator were comparable to, or better than, that of an LC-ICP-MS system with conventional pneumatic nebulization, or other sample introduction techniques. The experimental detection limits for various mercury species were in the range of 0.05-0.09 ng ml -1 Hg, based on peak height. The proposed method was successfully applied to the determination of mercury compounds in a swordfish sample purchased from the local market. The accuracy of the method was evaluated by analyzing a marine biological certified reference material (DORM-2, NRCC).

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

NASA Astrophysics Data System (ADS)

Yoshida, Satoshi

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

[Determination of heavy metals for RoHS compliance by ICP-OES spectrometry coupled with microwave extraction system].

PubMed

Hua, Li; Wu, Yi-Ping; An, Bing; Lai, Xiao-Wei

2008-11-01

The harm of heavy metals contained in electronic and electrical equipment (EEE) on environment is of high concern by human. Aiming to handle the great challenge of RoHS compliance, the determinations of trace or ultratrace chromium (Cr), cadmium (Cd), mercury (Hg) and lead (Pb) by inductively coupled plasma optical emission spectrometry (ICP-OES) was performed in the present paper, wherein, microwave extraction technology was used to prepare the sample solutions. In addition, the precision, recovery, repeatability and interference issues of this method were also discussed. The results exhibited that using the microwave extraction system to prepare samples is more quick, lossless, contamination-free in comparison with the conventional extraction methods such as dry ashing, wet-oven extraction etc. By analyzing the recoveries of these four heavy metals over different working time and wavelengths, the good recovery range between 85% and 115% showed that there was only tiny loss or contamination during the process of microwave extraction, sample introduction and ICP detection. Repeatability experiments proved that ICP plasma had a good stability during the working time and the matrix effect was small. Interference was a problem troublesome for atomic absorption spectrometry (AAS), however, the techniques of standard additions or inter-element correction (IEC) method can effectively eliminated the interferences of Ni, As, Fe etc. with the Cd determination. By employing the multi-wavelengths and two correction point methods, the issues of background curve sloping shift and spectra overlap were successfully overcome. Besides, for the determinations of trace heavy metal elements, the relative standard deviation (RSD) was less than 3% and the detection limits were less than 1 microg x L(-10 (3sigma, n = 5) for samples, standard solutions, and standard additions, which proved that ICP-OES has a good precision and high reliability. This provided a reliable technique support

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

DTIC Science & Technology

2015-04-01

monodisperse particles. ENPs in environmental samples will likely have much broader size distributions and thus FFF-ICP-MS was tested over a greater...Figure 6). Resolution is based on ICP-MS sensitivity, and will likely decrease as the difference in particle diameter decreases. Second, this...Alvarez. 2006. Antibacterial activity of fullerene water suspensions: Effects of preparation method and particle size. Environmental Science

Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

LaFreniere, K.E.

A direct injection nebulizer (DIN) was designed, developed and evaluated to determine its potential utilization as an effective interface for flow injection analysis (FIA) and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma-atomic emission spectroscopic detection. The analytical figures of merit for the DIN when used as an interface for FIA-ICP-AES were found to be comparable to or better than those obtained with conventional pneumatic nebulization in terms of limits of detection (LODs), reproducibility, linearity, and interelement effects. In the HPLC mode, the LODDs were found to be comparable to those obtained by continuous-flow sample introduction into themore » ICP, or inferior by up to only a factor of four. Stable plasma operation was maintained for the DIN sample introduction of a variety of pure organic solvents, including acetonitrile, methanol, methyl-isobutylketone, and pyridine. The HPLC-DIN-ICP-AES facility was specifically applied for the speciation of inorganic and organo-metallic species contained in synthetic mixtures, vanilla extracts and a variety of energy-related materials, such as shale oil process water, coal extracts, shale oil, crude oil, and an SRC II. Suggestions for future research are also considered.« less

Characteristics of n-GaN after ICP etching

NASA Astrophysics Data System (ADS)

Han, Yanjun; Xue, Song; Guo, Wenping; Hao, Zhi-Biao; Sun, Changzheng; Luo, Yi

2002-09-01

In this work, a systematic study on the plasma-induced damage on n-type GaN by inductively coupled plasma (ICP) etching is presented. After n-contact metal formation and annealing, electrical property is evaluated by the I-V characteristics. Room temperature photoluminescence (PL) measurement of etched GaN surfaces is performed to investigate the etching damage on the optical properties of n-type GaN. Investigation of the effect of additive gas RF chuck power on these characteristics has also been carried out. The better etching conditions have been obtained based on these results.

Inductive Electron Heating Revisited

NASA Astrophysics Data System (ADS)

Tuszewski, M.

1996-11-01

Inductively Coupled Plasmas (ICPs) have been studied for over a century. Recently, ICPs have been rediscovered by the multi-billion dollar semiconductor industry as an important class of high-density, low-pressure plasma sources suitable for the manufacture of next-generation integrated circuits. Present low-pressure ICP development is among the most active areas of plasma research. However, this development remains largely empirical, a prohibitively expensive approach for upcoming 300-mm diameter wafers. Hence, there is an urgent need for basic ICP plasma physics research, including experimental characterization and predictive numerical modeling. Inductive radio frequency (rf) power absorption is fundamental to the ICP electron heating and the resulting plasma transport but remains poorly understood. For example, recent experimental measurements and supporting fluid calculationsfootnote M. Tuszewski, Phys. Rev. Lett. 77 in press (1996) on a commercial deposition tool prototype show that the induced rf magnetic fields in the source can cause an order of magnitude reduction in plasma conductivity and in electron heating power density. In some cases, the rf fields penetrate through the entire volume of the ICP discharges while existing models that neglect the induced rf magnetic fields predict rf absorption in a thin skin layer near the plasma surface. The rf magnetic fields also cause more subtle changes in the plasma density and in the electron temperature spatial distributions. These data will be presented and the role of basic research in the applied world of semiconductor manufacturing will be discussed. ^*This research was conducted under the auspices of the U.S. DOE, supported by funds provided by the University of California for discretionary research by Los Alamos National Laboratory.

Determination of depleted uranium in urine via isotope ratio measurements using large-bore direct injection high efficiency nebulizer-inductively coupled plasma mass spectrometry.

PubMed

Westphal, Craig S; McLean, John A; Hakspiel, Shelly J; Jackson, William E; McClain, David E; Montaser, Akbar

2004-09-01

Inductively coupled plasma mass spectrometry (ICP-MS), coupled with a large-bore direct injection high efficiency nebulizer (LB-DIHEN), was utilized to determine the concentration and isotopic ratio of uranium in 11 samples of synthetic urine spiked with varying concentrations and ratios of uranium isotopes. Total U concentrations and (235)U/(238)U isotopic ratios ranged from 0.1 to 10 microg/L and 0.0011 and 0.00725, respectively. The results are compared with data from other laboratories that used either alpha-spectrometry or quadrupole-based ICP-MS with a conventional nebulizer-spray chamber arrangement. Severe matrix effects due to the high total dissolved solid content of the samples resulted in a 60 to 80% loss of signal intensity, but were compensated for by using (233)U as an internal standard. Accurate results were obtained with LB-DIHEN-ICP-MS, allowing for the positive identification of depleted uranium based on the (235)U/(238)U ratio. Precision for the (235)U/(238)U ratio is typically better than 5% and 15% for ICP-MS and alpha-spectrometry, respectively, determined over the concentrations and ratios investigated in this study, with the LB-DIHEN-ICP-MS system providing the most accurate results. Short-term precision (6 min) for the individual (235)U and (238)U isotopes in synthetic urine is better than 2% (N = 7), compared to approximately 5% for conventional nebulizer-spray chamber arrangements and >10% for alpha-spectrometry. The significance of these measurements is discussed for uranium exposure assessment of Persian Gulf War veterans affected by depleted uranium ammunitions.

Precise and accurate isotope ratio measurements by ICP-MS.

PubMed

Becker, J S; Dietze, H J

2000-09-01

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

Three-phase inductive-coupled structures for contactless PHEV charging system

NASA Astrophysics Data System (ADS)

Lee, Jia-You; Shen, Hung-Yu; Li, Cheng-Bin

2016-07-01

In this article, a new-type three-phase inductive-coupled structure is proposed for the contactless plug-in hybrid electric vehicle (PHEV) charging system regarding with SAE J-1773. Four possible three-phase core structures are presented and subsequently investigated by the finite element analysis. To study the correlation between the core geometric parameter and the coupling coefficient, the magnetic equivalent circuit model of each structure is also established. In accordance with the simulation results, the low reluctance and the sharing of flux path in the core material are achieved by the proposed inductive-coupled structure with an arc-shape and three-phase symmetrical core material. It results in a compensation of the magnetic flux between each phase and a continuous flow of the output power in the inductive-coupled structure. Higher coupling coefficient between inductive-coupled structures is achieved. A comparison of coupling coefficient, mutual inductance, and self-inductance between theoretical and measured results is also performed to verify the proposed model. A 1 kW laboratory scale prototype of the contactless PHEV charging system with the proposed arc-shape three-phase inductive-coupled structure is implemented and tested. An overall system efficiency of 88% is measured when two series lithium iron phosphate battery packs of 25.6 V/8.4 Ah are charged.

Precise and traceable carbon isotope ratio measurements by multicollector ICP-MS: what next?

PubMed

Santamaria-Fernandez, Rebeca

2010-06-01

This article reviews recent developments in the use of multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) to provide high-precision carbon isotope ratio measurements. MC-ICP-MS could become an alternative method to isotope ratio mass spectrometry (IRMS) for rapid carbon isotope ratio determinations in organic compounds and characterisation and certification of isotopic reference materials. In this overview, the advantages, drawbacks and potential of the method for future applications are critically discussed. Furthermore, suggestions for future improvements in terms of precision and sensitivity are made. No doubt, this is an exciting analytical challenge and, as such, hurdles will need to be cleared.

Exploration geochemical technique for the determination of preconcentrated organometallic halides by ICP-AES

USGS Publications Warehouse

Motooka, J.M.

1988-01-01

An atomic absorption extraction technique which is widely used in geochemical exploration for the determination of Ag, As, Au, Bi, Cd, Cu, Mo, Pb, Sb, and Zn has been modified and adapted to a simultaneous inductively coupled plasma-atomic emission instrument. the experimental and operating parameters are described for the preconcentration of the metals into their organometallic halides and for the determination of the metals. Lower limits of determination are equal to or improved over those for flame atomic absorption (except Au) and ICP results are very similar to the accepted AA values, with precision for the ICP data in excess of that necessary for exploration purposes.

Rapid determination of 237Np in soil samples by multi-collector inductively-coupled plasma mass spectrometry and gamma spectrometry.

PubMed

Yi, Xiaowei; Shi, Yanmei; Xu, Jiang; He, Xiaobing; Zhang, Haitao; Lin, Jianfeng

A radiochemical procedure is developed for the determination of 237 Np in soil with multi-collector inductively-coupled plasma mass spectrometry (MC-ICP-MS) and gamma-spectrometry. 239 Np (milked from 243 Am) was used as an isotopic tracer for chemical yield determination. The neptunium in the soil is separated by thenoyl-trifluoracetone extraction from 1 M HNO 3 solution after reducing Np to Np(IV) with ferrous sulfamate, and then purified with Dowex 1 × 2 anion exchange resin. 239 Np in the resulting solution is measured with gamma-spectrometry for chemical yield determination while the 237 Np is measured with MC-ICP-MS. Measurement results for soil samples are presented together with those for two reference samples. By comparing the determined value with the reference value of the 237 Np activity concentration, the feasibility of the procedure was validated.

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

DOE Office of Scientific and Technical Information (OSTI.GOV)

Havrilla, George Joseph; McIntosh, Kathryn Gallagher; Judge, Elizabeth

2016-10-20

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

Geographical traceability of wild Boletus edulis based on data fusion of FT-MIR and ICP-AES coupled with data mining methods (SVM)

NASA Astrophysics Data System (ADS)

Li, Yun; Zhang, Ji; Li, Tao; Liu, Honggao; Li, Jieqing; Wang, Yuanzhong

2017-04-01

In this work, the data fusion strategy of Fourier transform mid infrared (FT-MIR) spectroscopy and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was used in combination with Support Vector Machine (SVM) to determine the geographic origin of Boletus edulis collected from nine regions of Yunnan Province in China. Firstly, competitive adaptive reweighted sampling (CARS) was used for selecting an optimal combination of key wavenumbers of second derivative FT-MIR spectra, and thirteen elements were sorted with variable importance in projection (VIP) scores. Secondly, thirteen subsets of multi-elements with the best VIP score were generated and each subset was used to fuse with FT-MIR. Finally, the classification models were established by SVM, and the combination of parameter C and γ (gamma) of SVM models was calculated by the approaches of grid search (GS) and genetic algorithm (GA). The results showed that both GS-SVM and GA-SVM models achieved good performances based on the #9 subset and the prediction accuracy in calibration and validation sets of the two models were 81.40% and 90.91%, correspondingly. In conclusion, it indicated that the data fusion strategy of FT-MIR and ICP-AES coupled with the algorithm of SVM can be used as a reliable tool for accurate identification of B. edulis, and it can provide a useful way of thinking for the quality control of edible mushrooms.

A matrix effect and accuracy evaluation for the determination of elements in milk powder LIBS and laser ablation/ICP-OES spectrometry.

PubMed

Gilon, N; El-Haddad, J; Stankova, A; Lei, W; Ma, Q; Motto-Ros, V; Yu, J

2011-11-01

Laser ablation coupled to inductively coupled plasma optical emission spectrometry (LA-ICP-OES) and laser-induced breakdown spectroscopy (LIBS) were investigated for the determination of Ca, Mg, Zn and Na in milk samples. The accuracy of both methods was evaluated by comparison of the concentration found using LA-ICP-OES and LIBS with classical wet digestion associated with ICP-OES determination. The results were not fully acceptable, with biases from less than 1% to more than 60%. Matrix effects were also investigated. The sample matrix can influence the temperature, electron number density (n (e)) and other excitation characteristics in the ICP. These ICP characteristics were studied and evaluated during ablation of eight milk samples. Differences in n (e) (from 8.9 to 13.8 × 10(14) cm(-3)) and rotational temperature (ranging from 3,400 to 4,400 K) occurred with no correlation with trueness. LIBS results obtained after classical external calibration procedure gave degraded accuracy, indicating a strong matrix effect. The LIBS measurements clearly showed that the major problem in LA-ICP was related to the ablation process and that LIBS spectroscopy is an excellent diagnostic tool for LA-ICP techniques.

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

PubMed

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.

Interface COMSOL-PHREEQC (iCP), an efficient numerical framework for the solution of coupled multiphysics and geochemistry

NASA Astrophysics Data System (ADS)

Nardi, Albert; Idiart, Andrés; Trinchero, Paolo; de Vries, Luis Manuel; Molinero, Jorge

2014-08-01

This paper presents the development, verification and application of an efficient interface, denoted as iCP, which couples two standalone simulation programs: the general purpose Finite Element framework COMSOL Multiphysics® and the geochemical simulator PHREEQC. The main goal of the interface is to maximize the synergies between the aforementioned codes, providing a numerical platform that can efficiently simulate a wide number of multiphysics problems coupled with geochemistry. iCP is written in Java and uses the IPhreeqc C++ dynamic library and the COMSOL Java-API. Given the large computational requirements of the aforementioned coupled models, special emphasis has been placed on numerical robustness and efficiency. To this end, the geochemical reactions are solved in parallel by balancing the computational load over multiple threads. First, a benchmark exercise is used to test the reliability of iCP regarding flow and reactive transport. Then, a large scale thermo-hydro-chemical (THC) problem is solved to show the code capabilities. The results of the verification exercise are successfully compared with those obtained using PHREEQC and the application case demonstrates the scalability of a large scale model, at least up to 32 threads.

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

PubMed

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

2016-09-01

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

Slurry sampling electrothermal vaporization inductively coupled plasma mass spectrometry for the determination of Cr, Cd and Pb in plastics.

PubMed

Li, Po-Chien; Jiang, Shiuh-Jen

2006-07-01

Ultrasonic slurry sampling electrothermal vaporization dynamic reaction cell inductively coupled plasma mass spectrometry (USS-ETV-DRC-ICP-MS) for the determination of Cr, Cd and Pb in several plastic samples, using NH4NO3 as the modifier, is described. The influences of the instrumental operating conditions and the slurry preparation technique on the ion signals are investigated. A reduction in the intensity of the background at signals corresponding to chromium masses (arising from matrix elements) was achieved by using NH3 as the reaction cell gas in the DRC. The method was applied to determine Cr, Cd and Pb in two polystyrene (PS) samples and a polyvinyl chloride (PVC) sample using two different calibration methods, namely standard addition and isotope dilution. The results were in good agreement with those for digested samples analyzed by ultrasonic nebulization DRC-ICP-MS. The precision between sample replicates was better than 17% with the USS-ETV-DRC-ICP-MS method. The method detection limits, estimated from standard addition curves, were about 6-9, 1-2 and 8-11 ng g(-1) for Cr, Cd and Pb, respectively, in the original plastic samples.

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

NASA Astrophysics Data System (ADS)

Xiao, Zhili; Tan, Chao; Dong, Feng

2017-08-01

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

Quantitative characterization of gold nanoparticles by size-exclusion and hydrodynamic chromatography, coupled to inductively coupled plasma mass spectrometry and quasi-elastic light scattering.

PubMed

Pitkänen, Leena; Montoro Bustos, Antonio R; Murphy, Karen E; Winchester, Michael R; Striegel, André M

2017-08-18

The physicochemical characterization of nanoparticles (NPs) is of paramount importance for tailoring and optimizing the properties of these materials as well as for evaluating the environmental fate and impact of the NPs. Characterizing the size and chemical identity of disperse NP sample populations can be accomplished by coupling size-based separation methods to physical and chemical detection methods. Informed decisions regarding the NPs can only be made, however, if the separations themselves are quantitative, i.e., if all or most of the analyte elutes from the column within the course of the experiment. We undertake here the size-exclusion chromatographic characterization of Au NPs spanning a six-fold range in mean size. The main problem which has plagued the size-exclusion chromatography (SEC) analysis of Au NPs, namely lack of quantitation accountability due to generally poor NP recovery from the columns, is overcome by carefully matching eluent formulation with the appropriate stationary phase chemistry, and by the use of on-line inductively coupled plasma mass spectrometry (ICP-MS) detection. Here, for the first time, we demonstrate the quantitative analysis of Au NPs by SEC/ICP-MS, including the analysis of a ternary NP blend. The SEC separations are contrasted to HDC/ICP-MS (HDC: hydrodynamic chromatography) separations employing the same stationary phase chemistry. Additionally, analysis of Au NPs by HDC with on-line quasi-elastic light scattering (QELS) allowed for continuous determination of NP size across the chromatographic profiles, circumventing issues related to the shedding of fines from the SEC columns. The use of chemically homogeneous reference materials with well-defined size range allowed for better assessment of the accuracy and precision of the analyses, and for a more direct interpretation of results, than would be possible employing less rigorously characterized analytes. Published by Elsevier B.V.

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

PubMed

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

2017-11-27

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

Acquisition of a High-resolution Inductively Coupled Plasma Mass Spectrometer for Cosmochemical and Geochemical Research

NASA Technical Reports Server (NTRS)

Lauretta, D. S.

2004-01-01

The primary goal of our research in this program is to develop new techniques for the analysis of volatile trace elements in very small samples using inductively coupled plasma mass spectrometry (ICP-MS) in preparation for samples returned by the Stardust mission. The instrument that will serve as the basis of our experiments is the ELEMENT2 high-resolution ICP-MS. We have spent the past year designing the laboratory to house this instrument as well as space to store and prepare samples returned by the Stardust mission. Unfortunately, the location that we had initially selected for the instrument turned out to be insufficient for our needs. This was determined almost eight months into the first year of our funding cycle, after extensive work including the production of engineering drawings. However, during this time the Lunar and Planetary Laboratory was selected to lead Phoenix, the first Mars Scout mission. As a result of this award LPL purchased a new, 50,000 square foot building. We have acquired 1400 square feet of laboratory space in this new facility. Four-hundred square feet will be used for a class-100 clean room. This area is designated for storage and preparation of extraterrestrial materials. The additional 1000 square feet will house the ELEMENT2 ICP-MS and peripheral devices. This is an enormous amount of space for this instrument, but it provides plenty of room for expansion in the future. The ICP-MS and the clean room facilities have been purchased. The instrument has been delivered. The startup time for this instrument is relatively short and we expect to be collecting our first data by mid-summer.

Determination of essential and toxic elements in Cordyceps kyushuensis Kawam by inductively coupled plasma mass spectrometry.

PubMed

Zhang, Guoying; Zhao, Yanxin; Liu, Fengjun; Ling, Jianya; Lin, Jianqiang; Zhang, Changkai

2013-01-01

In this study, a total of 20 elements (essential, non-essential and toxic): lithium (Li), sodium (Na), potassium (K), gallium (Ga), magnesium (Mg), zinc (Zn), iron (Fe), copper (Cu), manganese (Mn), vanadium (V), chromium (Cr), nickel (Ni), cobalt (Co), molybdenum (Mo), selenium (Se), barium (Ba), tin (Sn), arsenic (As), lead (Pb) cadmium (Cd) and mercury (Hg) in natural and cultured Cordyceps kyushuensis have been determined by means of inductively coupled plasma mass spectrometry (ICP-MS). Cultured stroma, natural stroma and natural worm were digested by microwave-assisted method before analysis. The proposed ICP-MS method was validated by analyzing a certified reference material (CRM) GBW10015 (spinach). The results of one-way analysis of variance (ANOVA) revealed that the element concentrations in the three kinds of samples were significantly different (p<0.05). Except for Mg, Zn, Cu, the values of other elemental contents were the highest in the stroma of natural C. kyushuensis. In comparison with the worm, the concentrations of determined elements in wild stroma were higher. The remarkable difference of elemental contents between cultured and natural stroma may be caused by distinct growing environment. This finding highlighted the usefulness of ICP-MS elemental analysis and enhanced the value of C. kyushuensis as a candidate for nourishing food based on its composition. Copyright © 2012 Elsevier B.V. All rights reserved.

Measurements of natural uranium concentration and isotopic composition with permil-level precision by inductively coupled plasma-quadrupole mass spectrometry

NASA Astrophysics Data System (ADS)

Shen, Chuan-Chou; Lin, Huei-Ting; Chu, Mei-Fei; Yu, Ein-Fen; Wang, Xianfeng; Dorale, Jeffrey A.

2006-09-01

A new analytical technique using inductively coupled plasma-quadrupole mass spectrometry (ICP-QMS) has been developed that produces permil-level precision in the measurement of uranium concentration ([U]) and isotopic composition (δ234U) in natural materials. A 233U-236U double spike method was used to correct for mass fractionation during analysis. To correct for ratio drifting, samples were bracketed by uranium standard measurements. A sensitivity of 6-7 × 108 cps/ppm was generated with a sample solution uptake rate of 30 μL/min. With a measurement time of 15-20 min, standards of 30-ng uranium produced a within-run precision better than 3‰ (±2 R.S.D.) for δ234U and better than 2‰ for [U]. Replicate measurements made on standards show that a between-run reproducibility of 3.5‰ for δ234U and 2‰ for [U] can be achieved. ICP-QMS data of δ234U and [U] in seawater, coral, and speleothem materials are consistent with the data measured by other ICP-MS and TIMS techniques. Advantages of the ICP-QMS method include low cost, easy maintenance, simple instrumental operation, and few sample preparation steps. Sample size requirements are small, such as 10-14 mg of coral material. The results demonstrate that this technique can be applied to natural samples with various matrices.

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

DTIC Science & Technology

2016-02-29

development a tightly coupled magneto-hydrodynamic model for Inductively Coupled Radio- Frequency (RF) Plasmas. Non Local Thermodynamic Equilibrium (NLTE...for Inductively Coupled Radio-Frequency (RF) Plasmas. Non Local Thermodynamic Equilibrium (NLTE) effects are described based on a hybrid State-to-State... thermodynamic variable. This choice allows one to hide the non-linearity of the gas (total) thermal conductivity κ and can partially alle- 2 viate numerical

Analysis of iodinated X-ray contrast agents in water samples by ion chromatography and inductively-coupled plasma mass spectrometry.

PubMed

Sacher, Frank; Raue, Brigitte; Brauch, Heinz-Jürgen

2005-08-26

In this paper, an analytical method for the determination of six iodinated X-ray contrast agents (amidotrizoic acid, iohexol, iomeprol, iopamidol, iopromide, and ioxitalamic acid), iodide, and iodate in water samples is presented. The method is based on a separation of the analytes by ion chromatography (IC) and a subsequent detection by inductively-coupled plasma mass spectrometry (ICP-MS). The method was optimised with respect to separation conditions (column type and eluent composition) and extensively validated. Without pre-concentration of the samples, limits of detection below 0.2 microg/l could be achieved whereby reproducibility was below 6% for all compounds under investigation.

Simulation of SiO2 etching in an inductively coupled CF4 plasma

NASA Astrophysics Data System (ADS)

Xu, Qing; Li, Yu-Xing; Li, Xiao-Ning; Wang, Jia-Bin; Yang, Fan; Yang, Yi; Ren, Tian-Ling

2017-02-01

Plasma etching technology is an indispensable processing method in the manufacturing process of semiconductor devices. Because of the high fluorine/carbon ratio of CF4, the CF4 gas is often used for etching SiO2. A commercial software ESI-CFD is used to simulate the process of plasma etching with an inductively coupled plasma model. For the simulation part, CFD-ACE is used to simulate the chamber, and CFD-TOPO is used to simulate the surface of the sample. The effects of chamber pressure, bias voltage and ICP power on the reactant particles were investigated, and the etching profiles of SiO2 were obtained. Simulation can be used to predict the effects of reaction conditions on the density, energy and angular distributions of reactant particles, which can play a good role in guiding the etching process.

Measurements of collisionless heating effects in the H-mode of an inductively coupled plasma system

NASA Astrophysics Data System (ADS)

Zaka-Ul-Islam, Mujahid; Graham, Bill; Gans, Timo; Niemi, Kari; O'Connell, Deborah

2013-09-01

Inductively coupled plasma systems (ICPs) for processing applications are often operated at low pressures, in the near-collisionless regime. In this regime, the electron mean free path is comparable or larger than the plasma dimensions. The electron dynamics in such ICPs has been investigated here, using phase and space resolved optical emission spectroscopy (PROES) and Langmuir probe measurements. The PROES measurements are also used to calculate the Fourier harmonics components of the 2D excitation (in the radial axial plane). The experimental system is a standard GEC cell with the axial gap of ~4 cm, powered by 13.56 MHz RF power supply. The gas pressure was varied between 0.5 - 2 Pa. The PROES measurements and Fourier harmonics components confirm many of the previous simulation results in comparable operational regimes. The results show that in the 2D (radial-axial) plane, the plasma power is deposited in a spatially non-uniform and non-linear manner, with axial layers of positive and negative power absorption. The contribution of these nonlinear effects decreases with an increase in the pressure, as observed in previous experimental and simulation results.

A field survey of metal binding to metallothionein and other cytosolic ligands in liver of eels using an on-line isotope dilution method in combination with size exclusion (SE) high pressure liquid chromatography (HPLC) coupled to Inductively Coupled Plasma time-of-flight Mass Spectrometry (ICP-TOFMS).

PubMed

Van Campenhout, Karen; Goenaga Infante, Heidi; Goemans, Geert; Belpaire, Claude; Adams, Freddy; Blust, Ronny; Bervoets, Lieven

2008-05-15

The effect of metal exposure on the accumulation and cytosolic speciation of metals in livers of wild populations of European eel with special emphasis on metallothioneins (MT) was studied. Four sampling sites in Flanders showing different degrees of heavy metal contamination were selected for this purpose. An on-line isotope dilution method in combination with size exclusion (SE) high pressure liquid chromatography (HPLC) coupled to Inductively Coupled Plasma time-of-flight Mass Spectrometry (ICP-TOFMS) was used to study the cytosolic speciation of the metals. The distribution of the metals Cd, Cu, Ni, Pb and Zn among cytosolic fractions displayed strong differences. The cytosolic concentration of Cd, Ni and Pb increased proportionally with the total liver levels. However, the cytosolic concentrations of Cu and Zn only increased above a certain liver tissue threshold level. Cd, Cu and Zn, but not Pb and Ni, were largely associated with the MT pool in correspondence with the environmental exposure and liver tissue concentrations. Most of the Pb and Ni and a considerable fraction of Cu and Zn, but not Cd, were associated to High Molecular Weight (HMW) fractions. The relative importance of the Cu and Zn in the HMW fraction decreased with increasing contamination levels while the MT pool became progressively more important. The close relationship between the cytosolic metal load and the total MT levels or the metals bound on the MT pool indicates that the metals, rather than other stress factors, are the major factor determining MT induction.

Multielemental analysis of prehistoric animal teeth by laser-induced breakdown spectroscopy and laser ablation inductively coupled plasma mass spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Galiova, Michaela; Kaiser, Jozef; Fortes, Francisco J.

2010-05-01

Laser-induced breakdown spectroscopy (LIBS) and laser ablation (LA) inductively coupled plasma (ICP) mass spectrometry (MS) were utilized for microspatial analyses of a prehistoric bear (Ursus arctos) tooth dentine. The distribution of selected trace elements (Sr, Ba, Fe) was measured on a 26 mmx15 mm large and 3 mm thick transverse cross section of a canine tooth. The Na and Mg content together with the distribution of matrix elements (Ca, P) was also monitored within this area. The depth of the LIBS craters was measured with an optical profilometer. As shown, both LIBS and LA-ICP-MS can be successfully used for themore » fast, spatially resolved analysis of prehistoric teeth samples. In addition to microchemical analysis, the sample hardness was calculated using LIBS plasma ionic-to-atomic line intensity ratios of Mg (or Ca). To validate the sample hardness calculations, the hardness was also measured with a Vickers microhardness tester.« less

Gel electrophoresis coupled to inductively coupled plasma-mass spectrometry using species-specific isotope dilution for iodide and iodate determination in aerosols.

PubMed

Brüchert, Wolfram; Helfrich, Andreas; Zinn, Nico; Klimach, Thomas; Breckheimer, Markus; Chen, Hongwei; Lai, Senchao; Hoffmann, Thorsten; Bettmer, Jörg

2007-02-15

In this paper, we present an online coupling of gel electrophoresis (GE) and inductively coupled plasma-mass spectrometry (ICP-MS) for the determination of iodine species (iodide and iodate) in liquid (seawater) and aerosol samples. For the first time, this approach is applied to the analysis of small molecules, and initial systematic investigations revealed that the migration behavior as well as the detection sensitivity strongly depends on the matrix (e.g., high concentrations of chloride). These effects could consequently affect the accuracy of analytical results, so that they need to be considered for the analysis of real samples. The technique used for quantification is species-specific isotope dilution analysis (ssIDA), which is a matrix-independent calibration method under certain conditions. We demonstrate that the use of 129I-enriched iodide and iodate allows the correction of the impact of the matrix on both, the electrophoretic migration and the detection sensitivity of the ICP-MS. After optimization, this coupling offers a novel and alternative method in the analysis of iodine compounds in various matrices. Here, we demonstrate the analytical capability of the technique for the chemical characterization of marine aerosols. The results show the presence of iodide and iodate at the ng m(-3) and sub-ng m(-3) level in the investigated aerosol samples, which were taken at the coastal research station in Mace Head, Ireland. These results are in good agreement with other recent studies, which demonstrated that the iodine chemistry in the marine atmosphere is only poorly understood. In addition to iodide and iodate, another iodine compound could be separated and detected in certain samples with high total iodine concentrations and was identified as elemental iodine, probably in form of triiodide, by peak matching. However, it may arise from an artifact during sample preparation.

Elemental Analysis in Biological Matrices Using ICP-MS.

PubMed

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.

Application of laser ablation multicollector inductively coupled plasma mass spectrometry for the measurement of calcium and lead isotope ratios in packaging for discriminatory purposes.

PubMed

Santamaria-Fernandez, Rebeca; Wolff, Jean-Claude

2010-07-30

The potential of high-precision calcium and lead isotope ratio measurements using laser ablation coupled to multicollector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) to aid distinction between four genuine and five counterfeit pharmaceutical packaging samples and further classification of counterfeit packaging samples has been evaluated. We highlight the lack of reference materials for LA-MC-ICP-MS isotope ratio measurements in solids. In this case the problem is minimised by using National Institute of Standards and Technology Standard Reference Material (NIST SRM) 915a calcium carbonate (as solid pellets) and NIST SRM610 glass disc for sample bracketing external standardisation. In addition, a new reference material, NIST SRM915b calcium carbonate, has been characterised in-house for Ca isotope ratios and is used as a reference sample. Significant differences have been found between genuine and counterfeit samples; the method allows detection of counterfeits and aids further classification of packaging samples. Typical expanded uncertainties for measured-corrected Ca isotope ratio values ((43)Ca/(44)Ca and (42)Ca/(44)Ca) were found to be below 0.06% (k = 2, 95% confidence) and below 0.2% for measured-corrected Pb isotope ratios ((207)Pb/(206)Pb and (208)Pb/(206)Pb). This is the first time that Ca isotope ratios have been measured in packaging materials using LA coupled to a multicollector (MC)-ICP-MS instrument. The use of LA-MC-ICP-MS for direct measurement of Ca and Pb isotopic variations in cardboard/ink in packaging has definitive potential to aid counterfeit detection and classification. Copyright 2010 John Wiley & Sons, Ltd.

Reduction of polyatomic interferences in ICP-MS by collision/reaction cell (CRC-ICP-MS) techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Eiden, Greg C; Barinaga, Charles J; Koppenaal, David W

2012-05-01

Polyatomic and other spectral interferences in plasma source mass spectrometry (PSMS) can be dramatically reduced using collision and reaction cells (CRC). These devices have been used for decades in fundamental studies of ion-molecule chemistry, but have only recently been applied to PSMS. Benefits of this approach as applied in inductively coupled plasma MS (ICP-MS) include interference reduction, isobar separation, and thermalization/focusing of ions. Novel ion-molecule chemistry schemes are now routinely designed and empirically evaluated with relative ease. These “chemical resolution” techniques can avert interferences requiring mass spectral resolutions of >600,000 (m/m). Purely physical ion beam processes, including collisional dampening andmore » collisional dissociation, are also employed to provide improved sensitivity, resolution, and spectral simplicity. CRC techniques are now firmly entrenched in current-day ICP-MS technology, enabling unprecedented flexibility and freedom from many spectral interferences. A significant body of applications has now been reported in the literature. CRC techniques are found to be most useful for specialized or difficult analytical needs and situations, and are employed in both single- and multi-element determination modes.« less

Sulfur-based absolute quantification of proteins using isotope dilution inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Lee, Hyun-Seok; Heun Kim, Sook; Jeong, Ji-Seon; Lee, Yong-Moon; Yim, Yong-Hyeon

2015-10-01

An element-based reductive approach provides an effective means of realizing International System of Units (SI) traceability for high-purity biological standards. Here, we develop an absolute protein quantification method using double isotope dilution (ID) inductively coupled plasma mass spectrometry (ICP-MS) combined with microwave-assisted acid digestion for the first time. We validated the method and applied it to certify the candidate protein certified reference material (CRM) of human growth hormone (hGH). The concentration of hGH was determined by analysing the total amount of sulfur in hGH. Next, the size-exclusion chromatography method was used with ICP-MS to characterize and quantify sulfur-containing impurities. By subtracting the contribution of sulfur-containing impurities from the total sulfur content in the hGH CRM, we obtained a SI-traceable certification value. The quantification result obtained with the present method based on sulfur analysis was in excellent agreement with the result determined via a well-established protein quantification method based on amino acid analysis using conventional acid hydrolysis combined with an ID liquid chromatography-tandem mass spectrometry. The element-based protein quantification method developed here can be generally used for SI-traceable absolute quantification of proteins, especially pure-protein standards.

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.

PubMed

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.

Efficient interface for online coupling of capillary electrophoresis with inductively coupled plasma-mass spectrometry and its application in simultaneous speciation analysis of arsenic and selenium.

PubMed

Liu, Lihong; Yun, Zhaojun; He, Bin; Jiang, Guibin

2014-08-19

A simple and highly efficient online system coupling of capillary electrophoresis to inductively coupled plasma-mass spectrometry (CE-ICP-MS) for simultaneous separation and determination of arsenic and selenium compounds was developed. CE was coupled to an ICP-MS system by a sprayer with a novel direct-injection high-efficiency nebulizer (DIHEN) chamber as the interface. By using this interface, six arsenic species, including arsenite (As(III), arsenate (As(V)), monomethylarsonic acid (MMA), dimethylarsinic acid (DMA), arsenobetaine (AsB), and arsenocholine (AsC) and five selenium species (such as sodium selenite (Se(IV)), sodium selenate (Se(VI)), selenocysteine (SeCys), selenomethionine (SeMet), and Se-methylselenocysteine (MeSeCys)) were baseline-separated and determined in a single run within 9 min under the optimized conditions. Minimum dead volume, low and steady sheath flow liquid, high nebulization efficiency, and high sample transport efficiency were obtained by using this interface. Detection limits were in the range of 0.11-0.37 μg L(-1) for the six arsenic compounds (determined as (75)As at m/z 75) and 1.33-2.31 μg L(-1) for the five selenium species (determined as (82)Se at m/z 82). Repeatability expressed as the relative standard deviations (RSD, n = 6) of both migration time and peak area were better than 2.68% for arsenic compounds and 3.28% for selenium compounds, respectively. The proposed method had been successfully applied for the determination of arsenic and selenium species in the certified reference materials DORM-3, water, urine, and fish samples.

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

PubMed

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.

Studies on transport phenomena in electrothermal vaporization sample introduction applied to inductively coupled plasma for optical emission and mass spectrometry

NASA Astrophysics Data System (ADS)

Kántor, T.; Maestre, S.; de Loos-Vollebregt, M. T. C.

2005-10-01

In the present work electrothermal vaporization (ETV) was used in both inductively coupled plasma mass spectrometry (ICP-MS) and optical emission spectrometry (OES) for sample introduction of solution samples. The effect of (Pd + Mg)-nitrate modifier and CaCl 2 matrix/modifier of variable amounts were studied on ETV-ICP-MS signals of Cr, Cu, Fe, Mn and Pb and on ETV-ICP-OES signals of Ag, Cd, Co, Cu, Fe, Ga, Mn and Zn. With the use of matrix-free standard solutions the analytical curves were bent to the signal axes (as expected from earlier studies), which was observed in the 20-800 pg mass range by ICP-MS and in the 1-50 ng mass range by ICP-OES detection. The degree of curvature was, however, different with the use of single element and multi-element standards. When applying the noted chemical modifiers (aerosol carriers) in microgram amounts, linear analytical curves were found in the nearly two orders of magnitude mass ranges. Changes of the CaCl 2 matrix concentration (loaded amount of 2-10 μg Ca) resulted in less than 5% changes in MS signals of 5 elements (each below 1 ng) and OES signals of 22 analytes (each below 15 ng). Exceptions were Pb (ICP-MS) and Cd (ICP-OES), where the sensitivity increase by Pd + Mg modifier was much larger compared to other elements studied. The general conclusions suggest that quantitative analysis with the use of ETV sample introduction requires matrix matching or matrix replacement by appropriate chemical modifier to the specific concentration ranges of analytes. This is a similar requirement to that claimed also by the most commonly used pneumatic nebulization of solutions, if samples with high matrix concentration are concerned.

Geographical traceability of wild Boletus edulis based on data fusion of FT-MIR and ICP-AES coupled with data mining methods (SVM).

PubMed

Li, Yun; Zhang, Ji; Li, Tao; Liu, Honggao; Li, Jieqing; Wang, Yuanzhong

2017-04-15

In this work, the data fusion strategy of Fourier transform mid infrared (FT-MIR) spectroscopy and inductively coupled plasma-atomic emission spectrometry (ICP-AES) was used in combination with Support Vector Machine (SVM) to determine the geographic origin of Boletus edulis collected from nine regions of Yunnan Province in China. Firstly, competitive adaptive reweighted sampling (CARS) was used for selecting an optimal combination of key wavenumbers of second derivative FT-MIR spectra, and thirteen elements were sorted with variable importance in projection (VIP) scores. Secondly, thirteen subsets of multi-elements with the best VIP score were generated and each subset was used to fuse with FT-MIR. Finally, the classification models were established by SVM, and the combination of parameter C and γ (gamma) of SVM models was calculated by the approaches of grid search (GS) and genetic algorithm (GA). The results showed that both GS-SVM and GA-SVM models achieved good performances based on the #9 subset and the prediction accuracy in calibration and validation sets of the two models were 81.40% and 90.91%, correspondingly. In conclusion, it indicated that the data fusion strategy of FT-MIR and ICP-AES coupled with the algorithm of SVM can be used as a reliable tool for accurate identification of B. edulis, and it can provide a useful way of thinking for the quality control of edible mushrooms. Copyright © 2017. Published by Elsevier B.V.

Comparison of laser ablation and dried solution aerosol as sampling systems in inductively coupled plasma mass spectrometry.

PubMed

Coedo, A G; Padilla, I; Dorado, M T

2004-12-01

This paper describes a study designed to determine the possibility of using a dried aerosol solution for calibration in laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The relative sensitivities of tested materials mobilized by laser ablation and by aqueous nebulization were established, and the experimentally determined relative sensitivity factors (RSFs) were used in conjunction with aqueous calibration for the analysis of solid steel samples. To such a purpose a set of CRM carbon steel samples (SS-451/1 to SS-460/1) were sampled into an ICP-MS instrument by solution nebulization using a microconcentric nebulizer with membrane desolvating (D-MCN) and by laser ablation (LA). Both systems were applied with the same ICP-MS operating parameters and the analyte signals were compared. The RSF (desolvated aerosol response/ablated solid response) values were close to 1 for the analytes Cr, Ni, Co, V, and W, about 1.3 for Mo, and 1.7 for As, P, and Mn. Complementary tests were carried out using CRM SS-455/1 as a solid standard for one-point calibration, applying LAMTRACE software for data reduction and quantification. The analytical results are in good agreement with the certified values in all cases, showing that the applicability of dried aerosol solutions is a good alternative calibration system for laser ablation sampling.

Numerical analysis of effects of ion-neutral collision processes on RF ICP discharge

NASA Astrophysics Data System (ADS)

Nishida, K.; Mattei, S.; Lettry, J.; Hatayama, A.

2018-01-01

The discharge process of a radiofrequency (RF) inductively coupled plasma (ICP) has been modeled by an ElectroMagnetic Particle-in-Cell Monte Carlo Collision method (EM PIC-MCC). Although the simulation had been performed by our previous model to investigate the discharge mode transition of the RF ICP from a kinetic point of view, the model neglected the collision processes of ions (H+ and H2+) with neutral particles. In this study, the RF ICP discharge process has been investigated by the latest version of the model which takes the ion-neutral collision processes into account. The basic characteristics of the discharge mode transition provided by the previous model have been verified by the comparison between the previous and present results. As for the H-mode discharge regime, on the other hand, the ion-neutral collisions play an important role in evaluating the growth of the plasma. Also, the effect of the ion-neutral collisions on the kinetic feature of the plasma has been investigated, which has highlighted the importance of kinetic perspective for modeling the RF ICP discharge.

Comparative sulfur analysis using thermal combustion or inductively coupled plasma methodology and mineral composition of common livestock feedstuffs.

PubMed

Kerr, B J; Ziemer, C J; Weber, T E; Trabue, S L; Bearson, B L; Shurson, G C; Whitney, M H

2008-09-01

The objective of this study was to compare the use of thermal combustion (CNS) and inductively coupled plasma (ICP) to measure the total S content in plant-, animal-, and mineral-based feedstuffs, and to provide concentrations of other macro- and micro-minerals contained in these feedstuffs. Forty-five feedstuffs (464 total samples) were obtained from suppliers as well as swine feed and pet food manufacturers throughout the United States. Mineral data from IPC analysis were summarized on a DM basis using sample mean and SD, whereas the comparison of total S content between CNS and ICP was examined by bivariate plot and correspondence correlation. Analyses of a wide range of feedstuffs by CNS and ICP for total S were comparable for all but a few feedstuffs. For potassium iodide and tribasic copper chloride, ICP estimated total S to be lower than when analyzed by CNS (bias = 2.51 +/- 0.15 SE, P < 0.01). In contrast, for defluorinated phosphate and limestone, ICP estimated total S to be greater than when analyzed by CNS (bias = -1.46 +/- 0.51 SE, P < 0.01). All other samples had similar estimates of total S, whether analyzed by CNS or ICP. As expected, S composition varied greatly among feedstuffs. For total S, plant-based feedstuffs generally had lower total S compared with animal-based feedstuffs, whereas minerals supplied in sulfate form had the greatest concentration of total S. In addition to total S, mineral composition data are provided for all feedstuffs as obtained by ICP analysis. Within specific feedstuffs, mineral composition was quite variable, potentially due to low concentrations in the feed-stuff causing high mathematical variation or due to the source of feedstock obtained. In general, analyzed values of P were similar to previous tabular values. These data provide feed formulators a database from which modifications in dietary minerals can be accomplished and from which mineral requirements can be met more precisely to reduce losses of minerals into

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

NASA Astrophysics Data System (ADS)

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

2009-06-01

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

Comparative study of laminar and turbulent flow model with different operating parameters for radio frequency-inductively coupled plasma torch working at 3  MHz frequency at atmospheric pressure

DOE Office of Scientific and Technical Information (OSTI.GOV)

Punjabi, Sangeeta B., E-mail: p.sangeeta@gmail.com; Department of Physics, University of Mumbai, Kalina, Santacruz; Sahasrabudhe, S. N.

2014-01-15

This paper provides 2D comparative study of results obtained using laminar and turbulent flow model for RF (radio frequency) Inductively Coupled Plasma (ICP) torch. The study was done for the RF-ICP torch operating at 50 kW DC power and 3 MHz frequency located at BARC. The numerical modeling for this RF-ICP torch is done using ANSYS software with the developed User Defined Function. A comparative study is done between laminar and turbulent flow model to investigate how temperature and flow fields change when using different operating conditions such as (a) swirl and no swirl velocity for sheath gas flow rate, (b) variationmore » in sheath gas flow rate, and (c) variation in plasma gas flow rate. These studies will be useful for different material processing applications.« less

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.

PubMed

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

2007-01-16

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 <1.1% and <0.3%, respectively, on both (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 <14.3% while external precisions were <2.9%. The level of external precision acquired in this study is high enough to distinguish between most modern Pb sources. LA-MC-ICP-MS measurements differed from thermal ionisation mass spectrometry (TIMS) values by 1% or less while the accuracy obtained using LA-Q-ICP-MS compared to solution MC-ICP-MS was 3.1% or better using a run bracketing (RB) mass bias correction method. Sample heterogeneity and detector switching when measuring (208)Pb by Q-ICP-MS are identified as sources of reduced analytical performance.

Novel method for metalloproteins determination in human breast milk by size exclusion chromatography coupled to inductively coupled plasma mass spectrometry.

PubMed

Acosta, Mariano; Torres, Sabier; Mariño-Repizo, Leonardo; Martinez, Luis D; Gil, Raúl A

2018-06-02

Levels of essential metals in human breast milk (HBM) have been determined by different analytical techniques, but there is few woks about human whey milk fractions. However, the current trend lies in metalloproteomic and identification of different metalloproteins. In this sense, native separative techniques (N-PAGE and SEC) coupled to ICP-MS provide us with valuable information. Besides it is necessary the development of new methodologies in order to determine with accuracy and precision the profile of such metals and metalloproteins in the different whey protein fractions of HBM. Thus, the aim of this work was to develop a new method for metals and metalloproteins determination by SEC-ICP-MS in whey protein fractions of HBM. Human whey fractions were obtained of HBM samples by ultracentrifugation. Then, protein fractions of whey milk were separated by SEC coupled to ICP-MS for metalloproteins and Mn, Co, Cu and Se quantification. Besides, protein profile of whey milk was determined by N-PAGE and computer assisted image analysis. SEC-ICP-MS results indicated that first and second protein fractions showed detectable levels of the Mn, Co, Cu, and Se. Protein profile determined by N-PAGE and image analysis showed that molecular weight of protein fractions ranged between 68,878-1,228.277 Da. In this work, metalloproteins were analyzed by SEC coupled to ICP-MS, with adequate sensitivity and accuracy. Our study has shown the presence of Mn, Co, Cu and Se bound to two protein fractions in whey milk of HBM. Metals levels analyzed were within the ranges reported in the literature. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

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

2013-03-22

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

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

PubMed

Horner, Nolan S; Beauchemin, Diane

2012-03-02

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

Evaluation of a direct injection nebulizer interface for flow injection analysis and high performance liquid chromatography with inductively coupled plasma-atomic emission spectroscopic detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

LaFreniere, K.E.

A direct injection nebulizer (DIN) was designed, developed, and evaluated to determine its potential utilization as an effective interface for flow injection analysis (FIA) and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma-atomic emission spectroscopic detection. The analytical figures of merit for the DIN when used as an interface for FIA-ICP-AES were found to be comparable to or better than those obtained with conventional pneumatic nebulization in terms of limits of detection (LODs), reproducibility, linearity, and interelement effects. Stable plasma operation was maintained for the DIN sample introduction of a variety of pure organic solvents, including acetonitrile, methanol,more » methylisobutylketone, and pyridine. The HPLC-DIN-ICP-AES facility was specifically applied for the speciation of inorganic and organometallic species contained in synthetic mixtures, vanilla extracts, and a variety of energy-related materials, such as shale oil process water, coal extracts, shale oil, crude oil, and an SRC II. Suggestions for future research are also considered. 227 refs., 44 figs., 15 tabs.« less

Determination of arsenic species in fish, crustacean and sediment samples from Thailand using high performance liquid chromatography (HPLC) coupled with inductively coupled plasma mass spectrometry (ICP-MS).

PubMed

Rattanachongkiat, S; Millward, G E; Foulkes, M E

2004-04-01

Suitable techniques have been developed for the extraction of arsenic species in a variety of biological and environmental samples from the Pak Pa-Nang Estuary and catchment, located in Southern Thailand, and for their determination using HPLC directly coupled with ICP-MS. The estuary catchment comprises a tin mining area and inhabitants of the region can suffer from various stages of arsenic poisoning. The important arsenic species, AsB, DMA, MMA, and inorganic arsenic (As III and V) have been determined in fish and crustacean samples to provide toxicological information on those fauna which contribute to the local diet. A Hamilton PRP-X100 anion-exchange HPLC system employing a step elution has been used successfully to achieve separation of the arsenic species. A nitric acid microwave digestion procedure, followed by carrier gas nitrogen addition- (N2)-ICP-MS analysis was used to measure total arsenic in sample digests and extracts. The arsenic speciation of the biological samples was preserved using a Trypsin enzymatic extraction procedure. Extraction efficiencies were high, with values of 82-102%(As) for fish and crustacean samples. Validation for these procedures was carried out using certified reference materials. Fish and crustacean samples from the Pak Pa-Nang Estuary showed a range for total arsenic concentration, up to 17 microg g(-1) dry mass. The major species of arsenic in all fauna samples taken was AsB, together with smaller quantities of DMA and, more importantly, inorganic As. For sediment samples, arsenic species were determined following phosphoric acid (1 M H3PO4) extraction in an open focused microwave system. A phosphate-based eluant, pH 6-7.5, with anion exchange HPLC coupled with ICP-MS was used for separation and detection of AsIII, AsV, MMA and DMA. The optimum conditions, identified using an estuarine sediment reference material (LGC), were achieved using 45 W power and a 20 minute heating period for extraction of 0.5 g sediment. The

Advances in HPLC-ICP-MS interface techniques for metal speciation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hill, S.J.

The relentless demand for lower detection limits is increasingly coupled to the requirement for elemental speciation. This is particularly true in environmental and clinical fields where total levels are often insufficient for mobility and toxicity studies. This demand for both qualitative and quantitative data on the individual species present in complex samples has led to the development of various interfaces to couple some form of chromatography, usually gas chromatography (GC) or high performance liquid chromatography (HPLC) to an element specific detector. Today inductively coupled plasma-mass spectrometry is often employed since it offers excellent detection limits, element specific information (including isotopicmore » data) and the potential for multi-element studies. Ms presentation will concentrate on HPLC couplings although the advantages and disadvantages of both GC and HPLC couplings to ICP-MS will be discussed. Particular attention will be given to the optimization of both the chromatography and detection systems. Details will be presented of several successful HPLC interface designs and ways of facilitating high levels of a range of organic solvents (e.g. methanol and THF) in the HPLC mobile phase will be highlighted. The advantages of using a sheath gas and practical ways of achieving this will also be discussed. Finally the use of isotope dilution analysis in conjunction with HPLC-ICP-MS will be outlined. In all cases the impact of using the most appropriate approach will be demonstrated using both environmental and clinical samples.« less

Gunshot residue testing in suicides: Part II: Analysis by inductive coupled plasma-atomic emission spectrometry.

PubMed

Molina, D Kimberley; Castorena, Joe L; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

2007-09-01

Several different methods can be employed to test for gunshot residue (GSR) on a decedent's hands, including scanning electron microscopy with energy dispersive x-ray (SEM/EDX) and inductive coupled plasma-atomic emission spectrometry (ICP-AES). In part I of this 2-part series, GSR results performed by SEM/EDX in undisputed cases of suicidal handgun wounds were studied. In part II, the same population was studied, deceased persons with undisputed suicidal handgun wounds, but GSR testing was performed using ICP-AES. A total of 102 cases were studied and analyzed for caliber of weapon, proximity of wound, and the results of the GSR testing. This study found that 50% of cases where the deceased was known to have fired a handgun immediately prior to death had positive GSR results by ICP/AES, which did not differ from the results of GSR testing by SEM/EDX. Since only 50% of cases where the person is known to have fired a weapon were positive for GSR by either method, this test should not be relied upon to determine whether someone has discharged a firearm and is not useful as a determining factor of whether or not a wound is self-inflicted or non-self-inflicted. While a positive GSR result may be of use, a negative result is not helpful in the medical examiner setting as a negative result indicates that either a person fired a weapon prior to death or a person did not fire a weapon prior to death.

Characteristics of pulsed dual frequency inductively coupled plasma

NASA Astrophysics Data System (ADS)

Seo, Jin Seok; Kim, Kyoung Nam; Kim, Ki Seok; Kim, Tae Hyung; Yeom, Geun Young

2015-01-01

To control the plasma characteristics more efficiently, a dual antenna inductively coupled plasma (DF-ICP) source composed of a 12-turn inner antenna operated at 2 MHz and a 3-turn outer antenna at 13.56 MHz was pulsed. The effects of pulsing to each antenna on the change of plasma characteristics and SiO2 etch characteristics using Ar/C4F8 gas mixtures were investigated. When the duty percentage was decreased from continuous wave (CW) mode to 30% for the inner or outer ICP antenna, decrease of the average electron temperature was observed for the pulsing of each antenna. Increase of the CF2/F ratio was also observed with decreasing duty percentage of each antenna, indicating decreased dissociation of the C4F8 gas due to the decreased average electron temperature. When SiO2 etching was investigated as a function of pulse duty percentage, increase of the etch selectivity of SiO2 over amorphous carbon layer (ACL) was observed while decreasing the SiO2 etch rate. The increase of etch selectivity was related to the change of gas dissociation characteristics, as observed by the decrease of average electron temperature and consequent increase of the CF2/F ratio. The decrease of the SiO2 etch rate could be compensated for by using the rf power compensated mode, that is, by maintaining the same time-average rf power during pulsing, instead of using the conventional pulsing mode. Through use of the power compensated mode, increased etch selectivity of SiO2/ACL similar to the conventional pulsing mode could be observed without significant decrease of the SiO2 etch rate. Finally, by using the rf power compensated mode while pulsing rf powers to both antennas, the plasma uniformity over the 300 mm diameter substrate could be improved from 7% for the CW conditions to about around 3.3% with the duty percentage of 30%.

Separation of silver ions and starch modified silver nanoparticles using high performance liquid chromatography with ultraviolet and inductively coupled mass spectrometric detection

NASA Astrophysics Data System (ADS)

Hanley, Traci A.; Saadawi, Ryan; Zhang, Peng; Caruso, Joseph A.; Landero-Figueroa, Julio

2014-10-01

The production of commercially available products marketed to contain silver nanoparticles is rapidly increasing. Species-specific toxicity is a phenomenon associated with many elements, including silver, making it imperative to develop a method to identify and quantify the various forms of silver (namely, silver ions vs. silver nanoparticles) possibly present in these products. In this study a method was developed using high performance liquid chromatography (HPLC) with ultraviolet (UV-VIS) and inductively coupled mass spectrometric (ICP-MS) detection to separate starch stabilized silver nanoparticles (AgNPs) and silver ions (Ag+) by cation exchange chromatography with 0.5 M nitric acid mobile phase. The silver nanoparticles and ions were baseline resolved with an ICP-MS response linear over four orders of magnitude, 0.04 mg kg- 1 detection limit, and 90% chromatographic recovery for silver solutions containing ions and starch stabilized silver nanoparticles smaller than 100 nm.

Evaluation of a tunable bandpass reaction cell inductively coupled plasma mass spectrometer for the determination of selenium in serum and urine

NASA Astrophysics Data System (ADS)

Nixon, David E.; Neubauer, Kenneth R.; Eckdahl, Steven J.; Butz, John A.; Burritt, Mary F.

2003-01-01

A Dynamic Reaction Cell™ inductively coupled plasma mass spectrometer (DRC-ICP-MS) was evaluated for the determination of selenium in serum and urine. Reaction cell conditions were evaluated for the suppression of Ar 2+ dimer at m/ z 78 and 80 using methane as the reaction gas. A diluent containing 10% ethanol, 1% nitric acid, 0.5% Triton X-100 with gallium and yttrium internal standards was used to dilute urine and serum samples. Instrument response calibration was achieved by using aqueous acidic standards spiked into a urine matrix. Slopes for aqueous inorganic selenium, seleno- DL-cystine, seleno- DL-methionine and trimethylselenonium iodide spiked into urine and serum matrices were nearly identical. In general, reagent blank readings and detection limits were significantly lower in the DRC mode (reaction cell pressurized) than the standard mode (cell vented). Average results for the analysis of National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1598 bovine serum (attained over 13 days) are: 43.8±3.6 μg Se/l. Reference concentration is 43.6±3.6 μg Se/l. For NIST SRM 2670 Normal Urine the DRC-ICP-MS results are 30.7±4.6 μg Se/l with a certified concentration of 30±8 μg Se/l. For NIST SRM 2670 Elevated Urine the DRC-ICP-MS results are 463±35 μg Se/l with a certified concentration of 460±30 μg Se/l. The DRC-ICP-MS results for selenium determinations in urine and serum survey samples from the Institut National de Sante Publique du Quebec were compared with the reference concentrations and results produced by conventional ICP-MS. While conventional ICP-MS gave acceptable results for survey samples, DRC-ICP-MS gave excellent results for both urine and sera. Closer correlation was observed for DRC-ICP-MS results with target concentrations than with conventional ICP-MS.

Trace element analysis of synthetic mono- and poly-crystalline CaF 2 by ultraviolet laser ablation inductively coupled plasma mass spectrometry at 266 and 193 nm

NASA Astrophysics Data System (ADS)

Koch, J.; Feldmann, I.; Hattendorf, B.; Günther, D.; Engel, U.; Jakubowski, N.; Bolshov, M.; Niemax, K.; Hergenröder, R.

2002-06-01

The analytical figures of merit for ultraviolet laser ablation-inductively coupled plasma mass spectrometry (UV-LA-ICP-MS) at 266 nm with respect to the trace element analysis of high-purity, UV-transmitting alkaline earth halides are investigated and discussed. Ablation threshold energy density values and ablation rates for mono- and poly-crystalline CaF 2 samples were determined. Furthermore, Pb-, Rb-, Sr-, Ba- and Yb-specific analysis was performed. For these purposes, a pulsed Nd:YAG laser operated at the fourth harmonic of the fundamental wavelength (λ=266 nm) and a double-focusing sector field ICP-MS detector were employed. Depending on the background noise and isotope-specific sensitivity, the detection limits typically varied from 0.7 ng/g for Sr to 7 ng/g in the case of Pb. The concentrations were determined using a glass standard reference material (SRM NIST612). In order to demonstrate the sensitivity of the arrangement described, comparative measurements by means of a commercial ablation system consisting of an ArF excimer laser (λ=193 nm) and a quadrupole-type ICP-MS (ICP-QMS) instrument were carried out. The accuracy of both analyses was in good agreement, whereas ablation at 266 nm and detection using sector-field ICP-MS led to a sensitivity that was one order of magnitude above that obtained at 193 nm with ICP-QMS.

Highly sensitive measurement of whole blood chromium by inductively coupled plasma mass spectrometry.

PubMed

Cieslak, Wendy; Pap, Kathleen; Bunch, Dustin R; Reineks, Edmunds; Jackson, Raymond; Steinle, Roxanne; Wang, Sihe

2013-02-01

Chromium (Cr), a trace metal element, is implicated in diabetes and cardiovascular disease. A hypochromic state has been associated with poor blood glucose control and unfavorable lipid metabolism. Sensitive and accurate measurement of blood chromium is very important to assess the chromium nutritional status. However, interferents in biological matrices and contamination make the sensitive analysis challenging. The primary goal of this study was to develop a highly sensitive method for quantification of total Cr in whole blood by inductively coupled plasma mass spectrometry (ICP-MS) and to validate the reference interval in a local healthy population. This method was developed on an ICP-MS with a collision/reaction cell. Interference was minimized using both kinetic energy discrimination between the quadrupole and hexapole and a selective collision gas (helium). Reference interval was validated in whole blood samples (n=51) collected in trace element free EDTA tubes from healthy adults (12 males, 39 females), aged 19-64 years (38.8±12.6), after a minimum of 8 h fasting. Blood samples were aliquoted into cryogenic vials and stored at -70 °C until analysis. The assay linearity was 3.42 to 1446.59 nmol/L with an accuracy of 87.7 to 99.8%. The high sensitivity was achieved by minimization of interference through selective kinetic energy discrimination and selective collision using helium. The reference interval for total Cr using a non-parametric method was verified to be 3.92 to 7.48 nmol/L. This validated ICP-MS methodology is highly sensitive and selective for measuring total Cr in whole blood. Copyright © 2012 The Canadian Society of Clinical Chemists. Published by Elsevier Inc. All rights reserved. Published by Elsevier Inc. All rights reserved.

Closed inductively coupled plasma cell

DOEpatents

Manning, Thomas J.; Palmer, Byron A.; Hof, Douglas E.

1990-01-01

A closed inductively coupled plasma cell generates a relatively high power, low noise plasma for use in spectroscopic studies. A variety of gases can be selected to form the plasma to minimize spectroscopic interference and to provide a electron density and temperature range for the sample to be analyzed. Grounded conductors are placed at the tube ends and axially displaced from the inductive coil, whereby the resulting electromagnetic field acts to elongate the plasma in the tube. Sample materials can be injected in the plasma to be excited for spectroscopy.

Closed inductively coupled plasma cell

DOEpatents

Manning, T.J.; Palmer, B.A.; Hof, D.E.

1990-11-06

A closed inductively coupled plasma cell generates a relatively high power, low noise plasma for use in spectroscopic studies is disclosed. A variety of gases can be selected to form the plasma to minimize spectroscopic interference and to provide a electron density and temperature range for the sample to be analyzed. Grounded conductors are placed at the tube ends and axially displaced from the inductive coil, whereby the resulting electromagnetic field acts to elongate the plasma in the tube. Sample materials can be injected in the plasma to be excited for spectroscopy. 1 fig.

Sequential photocatalyst-assisted digestion and vapor generation device coupled with anion exchange chromatography and inductively coupled plasma mass spectrometry for speciation analysis of selenium species in biological samples.

PubMed

Tsai, Yun-ni; Lin, Cheng-hsing; Hsu, I-hsiang; Sun, Yuh-chang

2014-01-02

We have developed an on-line sequential photocatalyst-assisted digestion and vaporization device (SPADVD), which operates through the nano-TiO2-catalyzed photo-oxidation and reduction of selenium (Se) species, for coupling between anion exchange chromatography (LC) and inductively coupled plasma mass spectrometry (ICP-MS) systems to provide a simple and sensitive hyphenated method for the speciation analysis of Se species without the need for conventional chemical digestion and vaporization techniques. Because our proposed on-line SPADVD allows both organic and inorganic Se species in the column effluent to be converted on-line into volatile Se products, which are then measured directly through ICP-MS, the complexity of the procedure and the probability of contamination arising from the use of additional chemicals are both low. Under the optimized conditions for SPADVD - using 1g of nano-TiO2 per liter, at pH 3, and illuminating for 80 s - we found that Se(IV), Se(VI), and selenomethionine (SeMet) were all converted quantitatively into volatile Se products. In addition, because the digestion and vaporization efficiencies of all the tested selenicals were improved when using our proposed on-line LC/SPADVD/ICP-MS system, the detection limits for Se(IV), Se(VI), and SeMet were all in the nanogram-per-liter range (based on 3σ). A series of validation experiments - analysis of neat and spiked extracted samples - indicated that our proposed methods could be applied satisfactorily to the speciation analysis of organic and inorganic Se species in the extracts of Se-enriched supplements. Copyright © 2013. Published by Elsevier B.V.

Ionic liquids improved reversed-phase HPLC on-line coupled with ICP-MS for selenium speciation.

PubMed

Chen, Beibei; He, Man; Mao, Xiangju; Cui, Ran; Pang, Daiwen; Hu, Bin

2011-01-15

Room-temperature ionic liquids (RTILs) improved reversed-phase high performance liquid chromatography (RP-HPLC) on-line combined with inductively coupled plasma mass spectrometry (ICP-MS) was developed for selenium speciation. The different parameters affecting the retention behaviors of six target selenium species especially the effect of RTILs as mobile phase additives have been studied, it was found that the mobile phase consisting of 0.4% (v/v) 1-butyl-3-methylimidazolium chloride ([BMIM]Cl), 0.4% (v/v) 1-butyl-2,3-dimethylimidazolium tetrafluroborate ([BMMIM]BF(4)) and 99.2% (v/v) water has effectively improved the peak profile and six target selenium species including Na(2)SeO(3) (Se(IV)), Na(2)SeO(4) (Se(VI)), L-selenocystine (SeCys(2)), D,L-selenomethionine (SeMet), Se-methylseleno-l-cysteine (MeSeCys), seleno-D,L-ethionine (SeEt) were separated in 8 min. In order to validate the accuracy of the method, a Certified Reference Material of SELM-1 yeast sample was analyzed and the results obtained were in good agreement with the certified values. The developed method was also successfully applied to the speciation of selenium in Se-enriched yeasts and clover. For fresh Se-enriched yeast cells, it was found that the spiked SeCys(2) in living yeast cells could be transformed into SeMet. Compared with other ion-pair RP-HPLC-ICP-MS approaches for selenium speciation, the proposed method possessed the advantages including ability to regulate the retention time of the target selenium species by selecting the suitable RTILs and their concentration, simplicity, rapidness and low injection volume, thus providing wide potential applications for elemental speciation in biological systems. Copyright © 2010 Elsevier B.V. All rights reserved.

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

PubMed

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.

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

NASA Astrophysics Data System (ADS)

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

2015-04-01

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

Rare earth elements profile in a cultivated and non-cultivated soil determined by laser ablation-inductively coupled plasma mass spectrometry.

PubMed

Neves, Vinicius M; Heidrich, Graciela M; Hanzel, Flavia B; Muller, Edson I; Dressler, Valderi L

2018-05-01

Rare earth elements (REEs) have several applications but the effects on environment are not well known. Therefore, the aim of this work is to establish a method for direct solid sample analysis by laser ablation-inductively coupled plasma mass spectrometry (LA-ICP-MS) to evaluate the concentration and distribution of REEs in cultivated and non-cultivated soil. Samples were collected in two areas to 40 cm of depth. The LA-ICP-MS method is easy to be implemented and the sample treatment is very fast comprising only its drying, grounding and pressing as a pellet. The accuracy of the method was evaluated by using a certified reference material (BCR 667 - Estuarine Sediment, Institute for Reference Materials and Measurements (IRMM)) where good agreement with the certified values was obtained. Analyte recovery at two levels of concentration (2.5 and 15.0 μg g -1 ) was also performed and recoveries in the range of 85%-120% were achieved, values that are acceptable for LA-ICP-MS analysis. In general, the concentration of the REEs is higher in the cultivated soil and increased from the surface to deeper layers, which can be a consequence of fertilizer application. Copyright © 2018 Elsevier Ltd. All rights reserved.

Urinary iodine: comparison of a simple method for its determination in microplates with measurement by inductively-coupled plasma mass spectrometry

PubMed Central

Haap, Michael; Roth, Heinz Jürgen; Huber, Thomas; Dittmann, Helmut; Wahl, Richard

2017-01-01

The aim of our study was to develop and validate an inexpensive, rapid, easy to use quantitative method to determine urinary iodine without major procurement costs for equipment. The rationale behind introducing this method is the increasing demand for urinary iodine assessments. Our study included 103 patients (76 female, 27 male), age (arithmetic mean) 52 ± 17.3 years. Urinary iodine was determined in microplates by a modification of the Sandell-Kolthoff reaction. The results were compared with inductively-coupled plasma mass spectrometry (ICP-MS) for iodine, considered as reference method. Geometric mean of urinary iodine determined by the Sandell-Kolthoff reaction method was 62.69 μg/l (95% confidence interval 53.16–73.92) whereas by the ICP-MS method it was 65.53 μg/l (95% confidence interval 54.77–78.41). Passing-Bablok regression equations for both methods gave y = 3.374 + 0.873x (y: Sandell-Kolthoff method, x: ICP-MS). Spearman´s correlation coefficient was 0.981, indicating a very high degree of agreement between the two methods. Bland-Altman plots showed no significant systematic difference between the two methods. The modified Sandell-Kolthoff method using microtiter plate technique presented here is a simple, inexpensive semi-automated method to determine urinary iodine with very little toxic waste. Comparison with the ICP-MS-technique yielded a good agreement between the two methods. PMID:28045077

The determination of mercury in mushrooms by CV-AAS and ICP-AES techniques.

PubMed

Jarzynska, Grazyna; Falandysz, Jerzy

2011-01-01

This research presents an example of an excellent applied study on analytical problems due to hazardous mercury determination in environmental materials and validity of published results on content of this element in wild growing mushrooms. The total mercury content has been analyzed in a several species of wild-grown mushrooms and some herbal origin certified reference materials, using two analytical methods. One method was commonly known and well validated the cold-vapour atomic absorption spectroscopy (CV-AAS) after a direct sample pyrolysis coupled to the gold wool trap, which was a reference method. A second method was a procedure that involved a final mercury measurement using the inductively-coupled plasma atomic emission spectroscopy (ICP-AES) at λ 194.163 nm, which was used by some authors to report on a high mercury content of a large sets of wild-grown mushrooms. We found that the method using the ICP-AES at λ 194.163 nm gave inaccurate and imprecise results. The results of this study imply that because of unsuitability of total mercury determination using the ICP-AES at λ 194.163 nm, the reports on great concentrations of this metal in a large sets of wild-grown mushrooms, when examined using this method, have to be studied with caution, since data are highly biased.

Establishing human heart chromium, cobalt and vanadium concentrations by inductively coupled plasma mass spectrometry.

PubMed

Day, Patrick L; Eckdahl, Steven J; Maleszewski, Joseph J; Wright, Thomas C; Murray, David L

2017-05-01

Chromium, cobalt, and vanadium are used in metallic joint prosthesis. Case studies have associated elevated heart tissue cobalt concentrations with myocardial injury. To document the long term heart metal ion concentrations, a validated inductively coupled plasma mass spectroscopy (ICP-MS) method was needed. The method utilized a closed-vessel microwave digestion system to digest the samples. An ICP-MS method utilizing Universal Cell Technology was used to determine our target analyte concentrations. Accuracy was verified using reference materials. Precision, sensitivity, recovery and linearity studies were performed. This method was used to establish a reference range for a non-implant containing cohort of 80 autopsy human heart tissues RESULTS: This method demonstrated an analytic measurement range of 0.5-100ng/mL for each element. Accuracy was within ±10% of target value for each element. Within-run precision for each element was below 20% CV. The chromium, vanadium and cobalt concentrations (mean±SD) were 0.1523±0.2157μg/g, 0.0094±0.0211μg/g and 0.1039±0.1305μg/g respectively in 80 non-implant containing human heart tissue samples. This method provides acceptable recovery of the chromium, cobalt and vanadium in heart tissue; allowing assessment of the effects of metallic joint prosthesis on myocardial health. Copyright © 2017 Elsevier GmbH. All rights reserved.

Axially and radially viewed inductively coupled plasmas — a critical review

NASA Astrophysics Data System (ADS)

Brenner, I. B.; Zander, A. T.

2000-08-01

The present status of axially viewed inductively coupled plasmas (ICP) is reviewed with special emphasis placed on the analytical performance of currently available systems. Descriptions are given of the various designs of the plasma-spectrometer configuration. Conventional figures of merit such as limits of detection, background behavior, interferences due to easily ionized elements (EIE), Ca and acids, and the Mg II 280.270 nm/Mg I 285.213 nm intensity ratio, are used to compare the performance of axially viewed and radially viewed ICPs. Various modes of sample introduction, including conventional pneumatic and ultrasonic nebulization (USN), thermospray and a direct injection probe will be described. For axially viewed ICPs, limits of detection (LOD) are improved by factors varying from approximately 2 to 30. Additional improvements by factors of 2-20 can be obtained using USN. The improvement factors generally depend on energy potentials of the spectral lines and the element. Although limits of detection in the presence of Ca and Na are degraded relative to an aqueous solution 10-30-fold, USN LODs using an axially viewed ICP are improved relative to those obtained using a pneumatic nebulizer for solutions containing Ca and Na. With normal aerosol load and under robust plasma conditions (as evidenced by Mg II/Mg I intensity ratios >8), EIE, Ca and mineral acid induced interferences are relatively small and are similar in axial and conventional radial configurations. However, interferences due to Ca are larger than those caused by Na due to the larger amount of energy required to dissociate the matrix. Matrix effects increase considerably when an USN is employed. For robust plasmas, ICP operating conditions and performance for multi-element quantitative analysis do not differ significantly from those of conventional radial configurations. In cases where robustness decreases, matrix interferences should be taken into account when establishing optimum conditions for

Cl 2-based dry etching of the AlGaInN system in inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Cho, Hyun; Vartuli, C. B.; Abernathy, C. R.; Donovan, S. M.; Pearton, S. J.; Shul, R. J.; Han, J.

1998-12-01

Cl 2-Based inductively coupled plasmas with low additional d.c. self-biases (-100 V) produce convenient etch rates (500-1500 Å·min -1) for GaN, AlN, InN, InAlN and InGaN. A systematic study of the effects of additive gas (Ar, N 2, H 2), discharge composition and ICP source power and chuck power on etch rate and surface morphology has been performed. The general trends are to go through a maximum in etch rate with percent Cl 2 in the discharge for all three mixtures and to have an increase (decrease) in etch rate with source power (pressure). Since the etching is strongly ion-assisted, anisotropic pattern transfer is readily achieved. Maximum etch selectivities of approximately 6 for InN over the other nitrides were obtained.

[Determination of tungsten and cobalt in the air of workplace by ICP-OES].

PubMed

Zhang, J; Ding, C G; Li, H B; Song, S; Yan, H F

2017-08-20

Objective: To establish the inductively coupled plasma optical emission spectrometry (ICP-OES) method for determination of cobalt and tungsten in the air of workplace. Methods: The cobalt and tungsten were collected by filter membrane and then digested by nitric acid, inductively coupled plasma optical emission spectrometry (ICP-OES) was used for the detection of cobalt and tungsten. Results: The linearity of tungsten was good at the range of 0.01-1 000 μg/ml with a correlation coefficient of 0.999 9, the LOD and LOQ were 0.006 7 μg/ml and 0.022 μg/ml, respectively. The recovery was ranged from 98%-101%, the RSD of intra-and inter-batch precision were 1.1%-3.0% and 2.1%-3.8%, respectively. The linearity of cobalt was good at the range of 0.01-100 μg/ml with a correlation coefficient of 0.999 9, the LOD and LOQ were 0.001 2 μg/ml and 0.044 μg/ml, respectively. The recovery was ranged from 95%-97%, the RSD of intra-and inter-batch precision were 1.1%-2.4% and 1.1%-2.9%, respectively. The sampling efficiency of tungsten and cobalt were higher than 94%. Conclusion: The linear range, sensitivity and precision of the method was suitable for the detection of tungsten and cobalt in the air of workplace.

Low level detection of Cs-135 and Cs-137 in environmental samples by ICP-MS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liezers, Martin; Farmer, Orville T.; Thomas, Linda MP

2009-10-01

The measurement of the fission product cesium isotopes 135Cs and 137Cs at low femtogram (fg) 10-15 levels in ground water by Inductively Coupled Plasma-Mass Spectrometry ICP-MS is reported. To eliminate the potential natural barium isobaric interference on the cesium isotopes, in-line chromatographic separation of the cesium from barium was performed followed by high sensitivity ICP-MS analysis. A high efficiency desolvating nebulizer system was employed to maximize ICP-MS sensitivity ~10cps/femtogram. The three sigma detection limit measured for 135Cs was 2fg/ml (0.1uBq/ml) and for 137Cs 0.9fg/ml (0.0027Bq/ml) with analysis time of less than 30 minutes/sample. Cesium detection and 135/137 isotope ratio measurementmore » at very low femtogram levels using this method in a ground water matrix is also demonstrated.« less

Sedimentation Time Measurements of Soil Particles by Light Scattering and Determination of Chromium, Lead, and Iron in Soil Samples via ICP

ERIC Educational Resources Information Center

Todebush, Patricia Metthe; Geiger, Franz M.

2005-01-01

The study of soil samples, using light scattering and Inductively Coupled Plasma spectrometry (ICP) to determine colloid sedimentation rates and the quantity of chromium, lead, and iron in the sample is described. It shows the physical and chemical behavior of solid components in soil, and how such pollutant binding colloid surfaces directly…

Screening of TiO2 and Au nanoparticles in cosmetics and determination of elemental impurities by multiple techniques (DLS, SP-ICP-MS, ICP-MS and ICP-OES).

PubMed

de la Calle, Inmaculada; Menta, Mathieu; Klein, Marlène; Séby, Fabienne

2017-08-15

Cosmetics are part of the daily life of most of the people. Thus, a complete characterization of the products we applied in our skin is necessary. In this work, an analytical investigation of a wide variety of cosmetics from the point of view of total element content and metallic nanoparticles (NPs) has been performed. Firstly, we analyzed the total element content by ICP-MS and ICP-OES after acid digestion as an assessment of the presence of metal impurities. Prohibited elements in cosmetics, according to the European Commission regulation No 1223/2009, were not detected, and only elements mentioned in the label were found (e.g. Al, Fe, Ti and Si). Secondly, a screening of the presence of NPs has been performed by Dynamic Light Scattering (DLS) and Single Particle Inductively-Coupled Plasma Mass Spectrometry (SP-ICP-MS). Two sample preparation procedures were applied. The first protocol consisted in the preparation of suspensions in 0.1% w/v SDS and the second based on defatting with hexane followed by resuspension in water. DLS was employed as a routine method for a fast analysis of NPs, but this technique showed limitations due to the lack of specificity. SP-ICP-MS analyses were then performed, first as a screening technique to evaluate the presence of TiO 2 and Au NPs in cosmetics suspensions prepared in SDS; and second, when a positive answer was obtained about the presence of NPs from the screening, SP-ICP-MS was used for particle size determination. Results showed that only TiO 2 NPs were present in two sunscreens, one anti-wrinkle day cream, one lip balm protector labeled as 'nano' and in one brand of toothpaste not labeled as 'nano'. Sizes obtained for both sample preparations were compared and ranged from 30 to 120nm in most of the samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Method of low tantalum amounts determination in niobium and its compounds by ICP-OES technique.

PubMed

Smolik, Marek; Turkowska, Magdalena

2013-10-15

A method of determination of low amounts of tantalum in niobium and niobium compounds without its prior separation by means of inductively coupled plasma optical emission spectrometry (ICP-OES) has been worked out. The method involves dissolution of the analyzed samples of niobium as well as its various compounds (oxides, fluorides, chlorides, niobates(V)) in fluoride environments, precipitation of sparingly soluble niobic(tantalic) acid (Nb2O5(Ta2O5) · xH2O), converting them into soluble complex compounds by means of oxalic acid with addition of hydrogen peroxide and finally analyzing directly obtained solutions by ICP-OES. This method permits determination of Ta in niobium at the level of 10(-3)% with relatively good precision (≤ 8% RSD) and accuracy (recovery factor: 0.9-1.1). Relative differences in the results obtained by two independent methods (ICP-OES and ICP-MS) do not exceed 14%, and other elements present in niobium compounds (Ti, W, Zr, Hf, V, Mo, Fe, Cr) at the level of 10(-2)% do not affect determination. © 2013 Elsevier B.V. All rights reserved.

In-house validation of a method for determination of silver nanoparticles in chicken meat based on asymmetric flow field-flow fractionation and inductively coupled plasma mass spectrometric detection.

PubMed

Loeschner, Katrin; Navratilova, Jana; Grombe, Ringo; Linsinger, Thomas P J; Købler, Carsten; Mølhave, Kristian; Larsen, Erik H

2015-08-15

Nanomaterials are increasingly used in food production and packaging, and validated methods for detection of nanoparticles (NPs) in foodstuffs need to be developed both for regulatory purposes and product development. Asymmetric flow field-flow fractionation with inductively coupled plasma mass spectrometric detection (AF(4)-ICP-MS) was applied for quantitative analysis of silver nanoparticles (AgNPs) in a chicken meat matrix following enzymatic sample preparation. For the first time an analytical validation of nanoparticle detection in a food matrix by AF(4)-ICP-MS has been carried out and the results showed repeatable and intermediately reproducible determination of AgNP mass fraction and size. The findings demonstrated the potential of AF(4)-ICP-MS for quantitative analysis of NPs in complex food matrices for use in food monitoring and control. The accurate determination of AgNP size distribution remained challenging due to the lack of certified size standards. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

PubMed

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.

Experimental evaluation of analyte excitation mechanisms in the inductively coupled plasma

NASA Astrophysics Data System (ADS)

Lehn, Scott A.; Hieftje, Gary M.

2003-10-01

The inductively coupled plasma (ICP) is a justifiably popular source for atomic emission spectrometry. However, despite its popularity, the ICP is still only partially understood. Even the mechanisms of analyte excitation remain unclear; some energy levels are quite clearly populated by charge transfer while others might be populated by electron-ion recombination, by electron impact, or by Penning processes. Distinguishing among these alternatives is possible by means of a steady-state kinetics approach that examines correlations between the emission of a selected atom, ion, or level and the local number densities of species assumed to produce the excitation. In an earlier investigation, strong correlations were found between either calcium atom or ion emission and selected combinations of calcium atom or ion number densities and electron number densities in the plasma. However, all radially resolved data employed in the earlier study were produced from Abel inversion and from measurements that were crude by today's standards. Now, by means of tomographic imaging, laser-saturated atomic fluorescence, and Thomson and Rayleigh scattering, it is possible to measure the required radially resolved data without Abel inversion and with far greater fidelity. The correlations previously studied for calcium have been investigated with these more reliable data. Ion-electron recombination, either radiative or with argon as a third body, was determined to be the most likely excitation mechanism for calcium atom, while electron impact appeared to be the most important process to produce excite-state calcium ions. These results were consistent with the previous study. However, the present study suggests that collisional deactivation, rather than radiative decay, is the most likely mode of returning both calcium atoms and ions to the ground state.

Inductively coupled plasma etching of GaAs low loss waveguides for a traveling waveguide polarization converter, using chlorine chemistry

NASA Astrophysics Data System (ADS)

Lu, J.; Meng, X.; Springthorpe, A. J.; Shepherd, F. R.; Poirier, M.

2004-05-01

A traveling waveguide polarization converter [M. Poirier et al.] has been developed, which involves long, low loss, weakly confined waveguides etched in GaAs (epitaxially grown by molecular beam epitaxy), with electroplated ``T electrodes'' distributed along the etched floor adjacent to the ridge walls, and airbridge interconnect metallization. This article describes the development of the waveguide fabrication, based on inductively coupled plasma (ICP) etching of GaAs using Cl2 chemistry; the special processes required to fabricate the electrodes and metallization [X. Meng et al.], and the device characteristics [M. Poirier et al.], are described elsewhere. The required waveguide has dimensions nominally 4 μm wide and 2.1 μm deep, with dimensional tolerances ~0.1 μm across the wafer and wafer to wafer. A vertical etch profile with very smooth sidewalls and floors is required to enable the plated metal electrodes to be fabricated within 0.1 μm of the ridge. The ridges were fabricated using Cl2 ICP etching and a photoresist mask patterned with an I-line stepper; He backside cooling, combined with an electrostatic chuck, was employed to ensure good heat transfer to prevent resist reticulation. The experimental results showed that the ridge profile is very sensitive to ICP power and platen rf power. High ICP power and low platen power tend to result in more isotropic etching, whereas increasing platen power increases the photoresist etch rate, which causes rougher ridge sidewalls. No strong dependence of GaAs etch rate and ridge profile were observed with small changes in process temperature (chuck temperature). However, when the chuck temperature was decreased from 25 to 0 °C, etch uniformity across a 3 in. wafer improved from 6% to 3%. Photoresist and polymer residues present after the ICP etch were removed using a combination of wet and dry processes. .

Monitoring of platinum surface contamination in seven Dutch hospital pharmacies using inductively coupled plasma mass spectrometry

PubMed Central

Huitema, A. D. R.; Bakker, E. N.; Douma, J. W.; Schimmel, K. J. M.; van Weringh, G.; de Wolf, P. J.; Schellens, J. H. M.; Beijnen, J. H.

2007-01-01

Objective: To develop, validate, and apply a method for the determination of platinum contamination, originating from cisplatinum, oxaliplatinum, and carboplatinum. Methods: Inductively coupled plasma mass spectrometry (ICP-MS) was used to determine platinum in wipe samples. The sampling procedure and the analytical conditions were optimised and the assay was validated. The method was applied to measure surface contamination in seven Dutch hospital pharmacies. Results: The developed method allowed reproducible quantification of 0.50 ng l−1 platinum (5 pg/wipe sample). Recoveries for stainless steel and linoleum surfaces ranged between 50.4 and 81.4% for the different platinum compounds tested. Platinum contamination was reported in 88% of the wipe samples. Although a substantial variation in surface contamination of the pharmacies was noticed, in most pharmacies, the laminar-airflow (LAF) hoods, the floor in front of the LAF hoods, door handles, and handles of service hatches showed positive results. This demonstrates that contamination is spread throughout the preparation rooms. Conclusion: We developed and validated an ultra sensitive and reliable ICP-MS method for the determination of platinum in surface samples. Surface contamination with platinum was observed in all hospital pharmacies sampled. The interpretation of these results is, however, complicated. PMID:17377802

One-milliliter wet-digestion for inductively coupled plasma mass spectrometry (ICP-MS): determination of platinum-DNA adducts in cells treated with platinum(II) complexes.

PubMed

Yamada, Kanae; Kato, Naoyuki; Takagi, Akimitsu; Koi, Minoru; Hemmi, Hiromichi

2005-08-01

Platinum (Pt)-DNA adducts formed by the anti-tumor agent cisplatin are recognized by the DNA mismatch repair (MMR) system. To investigate the involvement of MMR proteins including hMLH1 in the removal of these adducts, we developed a mL-scale wet-digestion method for inductively coupled plasma mass spectrometry (ICP-MS). The detection limit was 0.01 ng mL(-1) Pt, which corresponded to 2 pg Pt/microg DNA when 10 microg of DNA was used. The mean relative errors were 5.4% or better for a dynamic range of 0.01-10 ng mL(-1) Pt. DNA (approximately 500 microg) had no matrix effect. To improve the accuracy, DNA preparations were treated with ribonuclease and the apparent reduction in the concentration of Pt was corrected using cellular DNA levels, which were determined with Hoechst 33258. No significant differences were observed, in terms of the formation of Pt-DNA adducts or their removal over 6 h, between hMLH1-deficient HCT116 cells, a human colorectal cancer cell line, and hMLH1-complemented HCT116+ch3 cells (n=5; P>0.05), indicating that the hMLH1-dependent DNA repair systems contribute to neither the formation nor the removal of the adducts at detectable levels. In addition, approximately 19% of the adducts were removed within 6 h in both cell lines. A time course analysis (~24 h) suggested that the removal of cisplatin-generated Pt-DNA adducts follows first-order kinetics (t(1/2)=32 h). The amount of Pt-DNA adduct formed by oxaliplatin in 1 h was 56% (ratio of means) of that generated by an equimolar concentration of cisplatin in HCT116. The proposed procedure could be useful for determining Pt-DNA adducts formed by Pt(II) complexes.

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

PubMed

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

2017-01-28

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

Deposition and element fractionation processes during atmospheric pressure laser sampling for analysis by ICP-MS

NASA Astrophysics Data System (ADS)

Eggins, S. M.; Kinsley, L. P. J.; Shelley, J. M. G.

1998-05-01

We have used an ArF excimer laser coupled to a quadrupole inductively coupled plasma mass spectrometry (ICP-MS) for the measurement of a range of elements during excavation of a deepening ablation pit in a synthetic glass (NIST 612). Analyte behaviour shows progressive volatile element enrichment at shallow hole depths, with a change to refractory element enrichment as the ablation pit deepens further. Examination of ablation pit morphology and the surface condensate deposited around the ablation site reveals the importance of sequential condensation of refractory, then volatile phases from the cooling plasma plume after the end of the laser pulse. We interpret the observed element fractionation behaviour to reflect a change in ablation processes from photothermal dominated to plasma dominated mechanisms. The development of the surface deposit is greatly reduced by ablating in an ambient atmosphere of He instead of Ar and is accompanied by a two- to four-fold increase in ICP-MS sensitivity.

Size determination and quantification of engineered cerium oxide nanoparticles by flow field-flow fractionation coupled to inductively coupled plasma mass spectrometry.

PubMed

Sánchez-García, L; Bolea, E; Laborda, F; Cubel, C; Ferrer, P; Gianolio, D; da Silva, I; Castillo, J R

2016-03-18

Facing the lack of studies on characterization and quantification of cerium oxide nanoparticles (CeO2 NPs), whose consumption and release is greatly increasing, this work proposes a method for their sizing and quantification by Flow Field-flow Fractionation (FFFF) coupled to Inductively Coupled Plasma-Mass Spectrometry (ICP-MS). Two modalities of FFFF (Asymmetric Flow- and Hollow Fiber-Flow Field Flow Fractionation, AF4 and HF5, respectively) are compared, and their advantages and limitations discussed. Experimental conditions (carrier composition, pH, ionic strength, crossflow and carrier flow rates) are studied in detail in terms of NP separation, recovery, and repeatability. Size characterization of CeO2 NPs was addressed by different approaches. In the absence of feasible size standards of CeO2 NPs, suspensions of Ag, Au, and SiO2 NPs of known size were investigated. Ag and Au NPs failed to show a comparable behavior to that of the CeO2 NPs, whereas the use of SiO2 NPs provided size estimations in agreement to those predicted by the theory. The latter approach was thus used for characterizing the size of CeO2 NPs in a commercial suspension. Results were in adequate concordance with those achieved by transmission electron microscopy, X-ray diffraction and dynamic light scattering. The quantification of CeO2 NPs in the commercial suspension by AF4-ICP-MS required the use of a CeO2 NPs standards, since the use of ionic cerium resulted in low recoveries (99 ± 9% vs. 73 ± 7%, respectively). A limit of detection of 0.9 μg L(-1) CeO2 corresponding to a number concentration of 1.8 × 1012 L(-1) for NPs of 5 nm was achieved for an injection volume of 100 μL. Copyright © 2016 Elsevier B.V. All rights reserved.

The effect of ultrafast laser wavelength on ablation properties and implications on sample introduction in inductively coupled plasma mass spectrometry

PubMed Central

LaHaye, N. L.; Harilal, S. S.; Diwakar, P. K.; Hassanein, A.; Kulkarni, P.

2015-01-01

We investigated the role of femtosecond (fs) laser wavelength on laser ablation (LA) and its relation to laser generated aerosol counts and particle distribution, inductively coupled plasma-mass spectrometry (ICP-MS) signal intensity, detection limits, and elemental fractionation. Four different NIST standard reference materials (610, 613, 615, and 616) were ablated using 400 nm and 800 nm fs laser pulses to study the effect of wavelength on laser ablation rate, accuracy, precision, and fractionation. Our results show that the detection limits are lower for 400 nm laser excitation than 800 nm laser excitation at lower laser energies but approximately equal at higher energies. Ablation threshold was also found to be lower for 400 nm than 800 nm laser excitation. Particle size distributions are very similar for 400 nm and 800 nm wavelengths; however, they differ significantly in counts at similar laser fluence levels. This study concludes that 400 nm LA is more beneficial for sample introduction in ICP-MS, particularly when lower laser energies are to be used for ablation. PMID:26640294

Single-Run Single-Mask Inductively-Coupled-Plasma Reactive-Ion-Etching Process for Fabricating Suspended High-Aspect-Ratio Microstructures

NASA Astrophysics Data System (ADS)

Yang, Yao-Joe; Kuo, Wen-Cheng; Fan, Kuang-Chao

2006-01-01

In this work, we present a single-run single-mask (SRM) process for fabricating suspended high-aspect-ratio structures on standard silicon wafers using an inductively coupled plasma-reactive ion etching (ICP-RIE) etcher. This process eliminates extra fabrication steps which are required for structure release after trench etching. Released microstructures with 120 μm thickness are obtained by this process. The corresponding maximum aspect ratio of the trench is 28. The SRM process is an extended version of the standard process proposed by BOSCH GmbH (BOSCH process). The first step of the SRM process is a standard BOSCH process for trench etching, then a polymer layer is deposited on trench sidewalls as a protective layer for the subsequent structure-releasing step. The structure is released by dry isotropic etching after the polymer layer on the trench floor is removed. All the steps can be integrated into a single-run ICP process. Also, only one mask is required. Therefore, the process complexity and fabrication cost can be effectively reduced. Discussions on each SRM step and considerations for avoiding undesired etching of the silicon structures during the release process are also presented.

Evaluation of calcium alginate beads for Ce, La and Nd preconcentration from groundwater prior to ICP OES analysis.

PubMed

Arantes de Carvalho, Gabriel G; Kondaveeti, Stalin; Petri, Denise F S; Fioroto, Alexandre M; Albuquerque, Luiza G R; Oliveira, Pedro V

2016-12-01

Analytical methods for the determination of rare earth elements (REE) in natural waters by plasma spectrochemical techniques often require sample preparation procedures for analytes preconcentration as well as for removing matrix constituents, that may interfere on the analytical measurements. In the present work, calcium alginate (CA) beads were used for the first time aiming at Ce, La and Nd preconcentration from groundwater samples for further determination by inductively coupled plasma optical emission spectrometry (ICP OES). Test samples were analyzed in batch mode by transferring a 40mL test portion (pH=5±0.2) into a 50mL polyethylene flask containing 125mg CA beads. After 15min contact, the analytes were quantitatively extracted from the loaded CA beads with 2.0mL of 1.0molL -1 HCl solution for further determination by ICP OES, using Ce (II) 456.236, La (II) 379.478 and Nd (II) 430.358nm emission lines. The proposed approach is a reliable alternative for REE single-stage preconcentration from aqueous samples, as it provided accurate results based on the addition and recovery analysis of groundwater. The results obtained by the proposed method were also compared with those from reference method based on inductively coupled plasma mass spectrometry (ICP-MS) and no significant differences were observed after applying the Student's t-test at 95% confidence level. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of 238u/235u, 236u/238u and uranium concentration in urine using sf-icp-ms and mc-icp-ms: an interlaboratory comparison.

PubMed

Parrish, Randall R; Thirlwall, Matthew F; Pickford, Chris; Horstwood, Matthew; Gerdes, Axel; Anderson, James; Coggon, David

2006-02-01

Accidental exposure to depleted or enriched uranium may occur in a variety of circumstances. There is a need to quantify such exposure, with the possibility that the testing may post-date exposure by months or years. Therefore, it is important to develop a very sensitive test to measure precisely the isotopic composition of uranium in urine at low levels of concentration. The results of an interlaboratory comparison using sector field (SF)-inductively coupled plasma-mass spectrometry (ICP-MS) and multiple collector (MC)-ICP-MS for the measurement of uranium concentration and U/U and U/U isotopic ratios of human urine samples are presented. Three urine samples were verified to contain uranium at 1-5 ng L and shown to have natural uranium isotopic composition. Portions of these urine batches were doped with depleted uranium (DU) containing small quantities of U, and the solutions were split into 100 mL and 400 mL aliquots that were subsequently measured blind by three laboratories. All methods investigated were able to measure accurately U/U with precisions of approximately 0.5% to approximately 4%, but only selected MC-ICP-MS methods were capable of consistently analyzing U/U to reasonable precision at the approximately 20 fg L level of U abundance. Isotope dilution using a U tracer demonstrates the ability to measure concentrations to better than +/-4% with the MC-ICP-MS method, though sample heterogeneity in urine samples was shown to be problematic in some cases. MC-ICP-MS outperformed SF-ICP-MS methods, as was expected. The MC-ICP-MS methodology described is capable of measuring to approximately 1% precision the U/U of any sample of human urine over the entire range of uranium abundance down to <1 ng L, and detecting very small amounts of DU contained therein.

Characterization Of Nuclear Materials Using Time-Of-Flight ICP-MS

DOE Office of Scientific and Technical Information (OSTI.GOV)

Buerger, Stefan; Riciputi, Lee R; Bostick, Debra A

2006-01-01

The investigation of illicit trafficking of nuclear materials, nuclear safeguards analysis, and non-proliferation control requires sensitive and isotope-selective detection methods to gain crucial nuclear forensic information like isotope 'fingerprints' and multi-element signatures. The advantage of time-of-flight (TOF) mass spectrometry - quasi-simultaneous multi-mass analysis - combined with an inductively coupled plasma (ICP) ion source provides an analytical instrument with multi-element and multi-isotope capability and good detection limits. A TOF-ICP-MS system thus appears to be an advantageous choice for the investigation and characterization of nuclear materials. We present here results using a GBC OptiMass 8000 time-of-flight ICP-MS for the isotope screening ofmore » solid samples by laser ablation and the multi-element determination of impurities in uranium ore concentrates using matrix matched standards. A laser ablation system (New Wave Research, UP 213) coupled to the TOF-ICP-MS instrument has been used to optimize the system for analysis of non-radioactive metal samples of natural isotopic composition for a variety of elements including Cu, Sr, Zr, Mo, Cd, In, Ba, Ta, W, Re, Pt, and Pb in pure metals, alloys, and glasses to explore precision, accuracy, and detection limits. Similar methods were then applied to measure uranium. When the laser system is optimized, no mass bias correction is required. Precision and accuracy for the determination of the isotopic composition is typically 1 - 3% for elemental concentrations of as little as 50 ppm in the matrix, with no requirement for sample preparation. The laser ablation precision and accuracy are within ~10x of the instrumental limits for liquid analysis (0.1%). We have investigated the capabilities of the TOF-ICP-MS for the analysis of impurities in uranium matrices. Matrix matching has been used to develop calibration curves for a range of impurities (alkaline, earth-alkaline, transition metals, and

Growth Mechanisms of Inductively-Coupled Plasma Torch Synthesized Silicon Nanowires and their associated photoluminescence properties

PubMed Central

Agati, M.; Amiard, G.; Le Borgne, V.; Castrucci, P.; Dolbec, R.; De Crescenzi, M.; El Khakani, M. A.; Boninelli, S.

2016-01-01

Ultra-thin Silicon Nanowires (SiNWs) were produced by means of an industrial inductively-coupled plasma (ICP) based process. Two families of SiNWs have been identified, namely long SiNWs (up to 2–3 micron in length) and shorter ones (~100 nm). SiNWs were found to consist of a Si core (with diameter as thin as 2 nm) and a silica shell, of which the thickness varies from 5 to 20 nm. By combining advanced transmission electron microscopy (TEM) techniques, we demonstrate that the growth of the long SiNWs occurred via the Oxide Assisted Growth (OAG) mechanism, while the Vapor Liquid Solid (VLS) mechanism is responsible for the growth of shorter ones. Energy filtered TEM analyses revealed, in some cases, the existence of chapelet-like Si nanocrystals embedded in an otherwise silica nanowire. Such nanostructures are believed to result from the exposure of some OAG SiNWs to high temperatures prevailing inside the reactor. Finally, the intense photoluminescence (PL) of these ICP-grown SiNWs in the 620–950 nm spectral range is a clear indication of the occurrence of quantum confinement. Such a PL emission is in accordance with the TEM results which revealed that the size of nanostructures are indeed below the exciton Bohr radius of silicon. PMID:27874057

Growth Mechanisms of Inductively-Coupled Plasma Torch Synthesized Silicon Nanowires and their associated photoluminescence properties

NASA Astrophysics Data System (ADS)

Agati, M.; Amiard, G.; Le Borgne, V.; Castrucci, P.; Dolbec, R.; de Crescenzi, M.; El Khakani, M. A.; Boninelli, S.

2016-11-01

Ultra-thin Silicon Nanowires (SiNWs) were produced by means of an industrial inductively-coupled plasma (ICP) based process. Two families of SiNWs have been identified, namely long SiNWs (up to 2-3 micron in length) and shorter ones (~100 nm). SiNWs were found to consist of a Si core (with diameter as thin as 2 nm) and a silica shell, of which the thickness varies from 5 to 20 nm. By combining advanced transmission electron microscopy (TEM) techniques, we demonstrate that the growth of the long SiNWs occurred via the Oxide Assisted Growth (OAG) mechanism, while the Vapor Liquid Solid (VLS) mechanism is responsible for the growth of shorter ones. Energy filtered TEM analyses revealed, in some cases, the existence of chapelet-like Si nanocrystals embedded in an otherwise silica nanowire. Such nanostructures are believed to result from the exposure of some OAG SiNWs to high temperatures prevailing inside the reactor. Finally, the intense photoluminescence (PL) of these ICP-grown SiNWs in the 620-950 nm spectral range is a clear indication of the occurrence of quantum confinement. Such a PL emission is in accordance with the TEM results which revealed that the size of nanostructures are indeed below the exciton Bohr radius of silicon.

[Determination of 24 metal elements and their compounds in air of workplace by ICP-AES].

PubMed

Wang, Xiang; Qiu, Jianguo; Zhao, Zhonglin; Guo, Ying

2014-06-01

To establish a method for determination of the levels of 24 metal elements and their compounds in the air of workplace by inductively coupled plasma-atomic emission spectroscopy (ICP- AES). Sampling filters were digested by microwave, and diluted to 25 ml. Twenty-four elements (Mg, Ni, K, Mo, Zn, Ca, Ba, Pb, Mn, Cd, Cr, Co, Cu, Sr, Bi, Tl, Sn, Li, Sb, Zr, In, V, Y, and Be) were simultaneously measured by ICP-AES. The detection limits for 24 elements were 0.001∼0.029 mg/L; liner correlation coefficient r values were all equal to or above 0.9994; the relative standard derivations were less than 5%; the recovery rates were 91.2%∼103.9%; the degradation rates in 7 days were less than 9.7%. ICP-AES technique is a simple, rapid, accurate, and reliable method, which can be used to measure 24 metal elements and their compounds in the air of workplace.

Trace element analysis of rough diamond by LA-ICP-MS: a case of source discrimination?

PubMed

Dalpé, Claude; Hudon, Pierre; Ballantyne, David J; Williams, Darrell; Marcotte, Denis

2010-11-01

Current profiling of rough diamond source is performed using different physical and/or morphological techniques that require strong knowledge and experience in the field. More recently, chemical impurities have been used to discriminate diamond source and with the advance of laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) empirical profiling of rough diamonds is possible to some extent. In this study, we present a LA-ICP-MS methodology that we developed for analyzing ultra-trace element impurities in rough diamond for origin determination ("profiling"). Diamonds from two sources were analyzed by LA-ICP-MS and were statistically classified by accepted methods. For the two diamond populations analyzed in this study, binomial logistic regression produced a better overall correct classification than linear discriminant analysis. The results suggest that an anticipated matrix match reference material would improve the robustness of our methodology for forensic applications. © 2010 American Academy of Forensic Sciences.

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

PubMed

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.

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

PubMed

Nie, Xi-Du; Fu, Liang

2013-07-01

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

Laser ablation inductively coupled plasma mass spectrometry measurement of isotope ratios in depleted uranium contaminated soils.

PubMed

Seltzer, Michael D

2003-09-01

Laser ablation of pressed soil pellets was examined as a means of direct sample introduction to enable inductively coupled plasma mass spectrometry (ICP-MS) screening of soils for residual depleted uranium (DU) contamination. Differentiation between depleted uranium, an anthropogenic contaminant, and naturally occurring uranium was accomplished on the basis of measured 235U/238U isotope ratios. The amount of sample preparation required for laser ablation is considerably less than that typically required for aqueous sample introduction. The amount of hazardous laboratory waste generated is diminished accordingly. During the present investigation, 235U/238U isotope ratios measured for field samples were in good agreement with those derived from gamma spectrometry measurements. However, substantial compensation was required to mitigate the effects of impaired pulse counting attributed to sample inhomogeneity and sporadic introduction of uranium analyte into the plasma.

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

PubMed

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.

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

PubMed

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

2016-12-19

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

Confirmation of sentinel lymph node identity by analysis of fine-needle biopsy samples using inductively coupled plasma-mass spectrometry.

PubMed

Beavis, Alison; Dawson, Michael; Doble, Philip; Scolyer, Richard A; Bourne, Roger; Li, Ling-Xi L; Murali, Rajmohan; Stretch, Jonathan R; Lean, Cynthia L; Uren, Roger F; Thompson, John F

2008-03-01

The sentinel lymph node (SLN) biopsy technique is a reliable means of determining the tumor-harboring status of regional lymph nodes in melanoma patients. When technetium 99 m-labeled antimony trisulfide colloid (99 mTc-Sb2S3) particles are used to perform preoperative lymphoscintigraphy for SLN identification, they are retained in the SLN but are absent or present in only tiny amounts in non-SLNs. The present study investigated the potential for a novel means of assessing the accuracy of surgical identification of SLNs. This involved the use of inductively coupled plasma-mass spectrometry (ICP-MS) to analyze antimony concentrations in fine-needle biopsy (FNB) samples from surgically procured lymph nodes. A total of 47 FNB samples from surgically excised lymph nodes (32 SLNs and 15 non-SLNs) were collected. The SLNs were localized by preoperative lymphoscintigraphy that used 99 mTc-Sb2S3, blue dye, and gamma probe techniques. The concentrations of antimony were measured in the FNB samples by ICP-MS. The mean and median antimony concentrations (in parts per billion) were .898 and .451 in the SLNs, and .015 and .068 in the non-SLNs, the differences being highly statistically significant (P < .00005). Our results show that ICP-MS analysis of antimony concentrations in FNB specimens from lymph nodes can accurately confirm the identity of SLNs. Used in conjunction with techniques such as proton magnetic resonance spectroscopy for the nonsurgical evaluation of SLNs, ICP-MS analysis of antimony concentrations in FNB samples could potentially serve as a minimally invasive alternative to surgery and histopathologic evaluation to objectively classify a given node as sentinel or nonsentinel and determine its tumor-harboring status.

Determination of uranium in tap water by ICP-MS.

PubMed

El Himri, M; Pastor, A; de la Guardia, M

2000-05-01

A fast and accurate procedure has been developed for the determination of uranium at microg L(-1) level in tap and mineral water. The method is based on the direct introduction of samples, without any chemical pre-treatment, into an inductively coupled plasma mass spectrometer (ICP-MS). Uranium was determined at the mass number 238 using Rh as internal standard. The method provides a limit of detection of 2 ng L(-1) and a good repeatability with relative standard deviation values (RSD) about 3% for five independent analyses of samples containing 73 microg L(-1) of uranium. Recovery percentage values found for the determination of uranium in spiked natural samples varied between 91% and 106%. Results obtained are comparable with those found by radiochemical methods for natural samples and of the same order for the certified content of a reference material, thus indicating the accuracy of the ICP-MS procedure without the need of using isotope dilution. A series of mineral and tap waters from different parts of Spain and Morocco were analysed.

Strontium isotope ratios (87Sr/86Sr) of tooth enamel: a comparison of solution and laser ablation multicollector inductively coupled plasma mass spectrometry methods.

PubMed

Copeland, Sandi R; Sponheimer, Matt; le Roux, Petrus J; Grimes, Vaughan; Lee-Thorp, Julia A; de Ruiter, Darryl J; Richards, Michael P

2008-10-01

Strontium isotope ratios (87Sr/86Sr) in tooth enamel provide a means to investigate migration and landscape use in humans and other animals. Established methods for measuring (87)Sr/(86)Sr in teeth use bulk sampling (5-20 mg) and labor-intensive elemental purification procedures before analysis by either thermal ionization mass spectrometry (TIMS) or multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS). Another method for measuring 87Sr/86Sr is laser ablation MC-ICP-MS, but concerns have been expressed about its accuracy for measuring tooth enamel. In this study we test the precision and accuracy of the technique by analyzing 30 modern rodent teeth from the Sterkfontein Valley, South Africa by laser ablation MC-ICP-MS and solution MC-ICP-MS. The results show a mean difference in 87Sr/86Sr measured by laser ablation and by solution of 0.0003 +/- 0.0002. This degree of precision is well within the margin necessary for investigating the potential geographic origins of humans or animals in many areas of the world. Because laser ablation is faster, less expensive, and less destructive than bulk sampling solution methods, it opens the possibility for conducting 87Sr/86Sr analyses of intra-tooth samples and small and/or rare specimens such as micromammal and fossil teeth.

Determination of As, Hg and Pb in herbs using slurry sampling flow injection chemical vapor generation inductively coupled plasma mass spectrometry.

PubMed

Tai, Chia-Yi; Jiang, Shiuh-Jen; Sahayam, A C

2016-02-01

Analysis of herbs for As, Hg and Pb has been carried out using slurry sampling inductively coupled plasma mass spectrometry (ICP-MS) with flow injection vapor generation. Slurry containing 0.5% m/v herbal powder, 0.1% m/v citric acid and 2% v/v HCl was injected into the VG-ICP-MS system for the determination of As, Hg and Pb that obviate dissolution and mineralization. Standard addition and isotope dilution methods were used for quantifications in selected herbal powders. This method has been validated by the determination of As, Hg and Pb in NIST standard reference materials SRM 1547 Peach Leaves and SRM 1573a Tomato Leaves. The As, Hg and Pb analysis results of the reference materials agreed with the certified values. The precision obtained by the reported procedure was better than 7% for all determinations. The detection limit estimated from standard addition curve was 0.008, 0.003, and 0.007 ng mL(-1) for As, Hg and Pb, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

Micro-scale flow system for on-line multielement preconcentration from saliva digests and determination by inductively coupled plasma optical emission spectrometry

NASA Astrophysics Data System (ADS)

Menegário, Amauri A.; Fernanda Giné, Maria

2001-10-01

A micro-scale flow system is proposed for on-line preconcentration of Cd, Cu, Mn, Ni and Pb in saliva samples and their determination by inductively coupled plasma optical emission spectrometry (ICP-OES). A small column containing 8 μl of AG50W-X8 resin was inserted into the flow system, assembled with capillary tubes and connected to a micro-concentric nebulizer. The elution of the analytes was performed with 3 mol l -1 HCl at a flow rate of 82 μl min -1. The ICP-OES signal acquisition program permits measurements for 5 s in the concentrated portion of the transient elution peaks. A sample volume of 1 ml was required to obtain enrichment factors of 46, 23, 17, 18 and 44 for Cd, Cu, Mn, Ni and Pb, respectively. The relative standard deviations for a 50-μg l -1 multi-analyte solution were ≤6.5%. The recoveries for Cd, Cu, Mn, Ni and Pb in digested human saliva samples were between 86 and 111%. The sample throughput was 24 h -1.

Trace analysis of high-purity graphite by LA-ICP-MS.

PubMed

Pickhardt, C; Becker, J S

2001-07-01

Laser-ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) has been established as a very efficient and sensitive technique for the direct analysis of solids. In this work the capability of LA-ICP-MS was investigated for determination of trace elements in high-purity graphite. Synthetic laboratory standards with a graphite matrix were prepared for the purpose of quantifying the analytical results. Doped trace elements, concentration 0.5 microg g(-1), in a laboratory standard were determined with an accuracy of 1% to +/- 7% and a relative standard deviation (RSD) of 2-13%. Solution-based calibration was also used for quantitative analysis of high-purity graphite. It was found that such calibration led to analytical results for trace-element determination in graphite with accuracy similar to that obtained by use of synthetic laboratory standards for quantification of analytical results. Results from quantitative determination of trace impurities in a real reactor-graphite sample, using both quantification approaches, were in good agreement. Detection limits for all elements of interest were determined in the low ng g(-1) concentration range. Improvement of detection limits by a factor of 10 was achieved for analyses of high-purity graphite with LA-ICP-MS under wet plasma conditions, because the lower background signal and increased element sensitivity.

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

PubMed

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

2005-08-15

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

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

PubMed

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).

Inductively coupled helium plasma torch

DOEpatents

Montaser, Akbar; Chan, Shi-Kit; Van Hoven, Raymond L.

1989-01-01

An inductively coupled plasma torch including a base member, a plasma tube and a threaded insert member within the plasma tube for directing the plasma gas in a tangential flow pattern. The design of the torch eliminates the need for a separate coolant gas tube. The torch can be readily assembled and disassembled with a high degree of alignment accuracy.

Accurate quantitation standards of glutathione via traceable sulfur measurement by inductively coupled plasma optical emission spectrometry and ion chromatography

PubMed Central

Rastogi, L.; Dash, K.; Arunachalam, J.

2013-01-01

The quantitative analysis of glutathione (GSH) is important in different fields like medicine, biology, and biotechnology. Accurate quantitative measurements of this analyte have been hampered by the lack of well characterized reference standards. The proposed procedure is intended to provide an accurate and definitive method for the quantitation of GSH for reference measurements. Measurement of the stoichiometrically existing sulfur content in purified GSH offers an approach for its quantitation and calibration through an appropriate characterized reference material (CRM) for sulfur would provide a methodology for the certification of GSH quantity, that is traceable to SI (International system of units). The inductively coupled plasma optical emission spectrometry (ICP-OES) approach negates the need for any sample digestion. The sulfur content of the purified GSH is quantitatively converted into sulfate ions by microwave-assisted UV digestion in the presence of hydrogen peroxide prior to ion chromatography (IC) measurements. The measurement of sulfur by ICP-OES and IC (as sulfate) using the “high performance” methodology could be useful for characterizing primary calibration standards and certified reference materials with low uncertainties. The relative expanded uncertainties (% U) expressed at 95% confidence interval for ICP-OES analyses varied from 0.1% to 0.3%, while in the case of IC, they were between 0.2% and 1.2%. The described methods are more suitable for characterizing primary calibration standards and certifying reference materials of GSH, than for routine measurements. PMID:29403814

Trace element analysis of extraterrestrial metal samples by inductively coupled plasma mass spectrometry: the standard solutions and digesting acids.

PubMed

Wang, Guiqin; Wu, Yangsiqian; Lin, Yangting

2016-02-28

Nearly 99% of the total content of extraterrestrial metals is composed of Fe and Ni, but with greatly variable trace element contents. The accuracy obtained in the inductively coupled plasma mass spectrometry (ICP-MS) analysis of solutions of these samples can be significantly influenced by matrix contents, polyatomic ion interference, and the concentrations of external standard solutions. An ICP-MS instrument (X Series 2) was used to determine 30 standard solutions with different concentrations of trace elements, and different matrix contents. Based on these measurements, the matrix effects were determined. Three iron meteorites were dissolved separately in aqua regia and HNO3. Deviations due to variation of matrix contents in the external standard solutions were evaluated and the analysis results of the two digestion methods for iron meteorites were assessed. Our results show obvious deviations due to unmatched matrix contents in the external standard solutions. Furthermore, discrepancy in the measurement of some elements was found between the sample solutions prepared with aqua regia and HNO3, due to loss of chloride during sample preparation and/or incomplete digestion of highly siderophile elements in iron meteorites. An accurate ICP-MS analysis method for extraterrestrial metal samples has been established using external standard solutions with matched matrix contents and digesting the samples with HNO3 and aqua regia. Using the data from this work, the Mundrabilla iron meteorite previously classified as IAB-ung is reclassified as IAB-MG. Copyright © 2016 John Wiley & Sons, Ltd.

Uncertainty estimation in the determination of metals in superficial water by ICP-OES

NASA Astrophysics Data System (ADS)

Faustino, Mainara G.; Marques, Joyce R.; Monteiro, Lucilena R.; Stellato, Thamiris B.; Soares, Sabrina M. V.; Silva, Tatiane B. S. C.; da Silva, Douglas B.; Pires, Maria Aparecida F.; Cotrim, Marycel E. B.

2016-07-01

From validation studies, it was possible to estimate a measurement uncertainty of several elements such as Al, Ba, Ca, Cu, Cr, Cd, Fe, Mg, Mn, Ni and K in water samples from Guarapiranga Dam. These elements were analyzed by optical emission spectrometry with inductively coupled plasma (ICP-OES). The value of relative estimated uncertainties were between 3% and 15%. The greatest uncertainty contributions were analytical curve, and the recovery method, which were related with elements concentrations and the equipment response. Water samples analyzed were compared with CONAMA Resolution #357/2005.

Polymer monolithic capillary microextraction on-line coupled with inductively coupled plasma-mass spectrometry for the determination of trace Au and Pd in biological samples

NASA Astrophysics Data System (ADS)

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

2014-11-01

A novel method based on on-line polymer monolithic capillary microextraction (CME)-inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of trace Au and Pd in biological samples. For this purpose, poly(glycidyl methacrylate-ethylene dimethacrylate) monolith was prepared and functionalized with mercapto groups. The prepared monolith exhibited good selectivity to Au and Pd, and good resistance to strong acid with a long life span. Factors affecting the extraction efficiency of CME, such as sample acidity, sample flow rate, eluent conditions and coexisting ion interference were investigated in detail. Under the optimal conditions, the limits of detection (LODs, 3σ) were 5.9 ng L- 1 for Au and 8.3 ng L- 1 for Pd, and the relative standard deviations (RSDs, c = 50 ng L-1, n = 7) were 6.5% for Au and 1.1% for Pd, respectively. The developed method was successfully applied to the determination of Au and Pd in human urine and serum samples with the recovery in the range of 84-118% for spiked samples. The developed on-line polymer monolithic CME-ICP-MS method has the advantages of rapidity, simplicity, low sample/reagent consumption, high sensitivity and is suitable for the determination of trace Au and Pd in biological samples with limited amount available and complex matrix.

Recruitment of activated IRF-3 and CBP/p300 to herpes simplex virus ICP0 nuclear foci: Potential role in blocking IFN-{beta} induction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Melroe, Gregory T.; Silva, Lindsey; Schaffer, Priscilla A.

2007-04-10

The host innate response to viral infection includes the production of interferons, which is dependent on the coordinated activity of multiple transcription factors. Herpes simplex virus 1 (HSV-1) has been shown to block efficient interferon expression by multiple mechanisms. We and others have demonstrated that HSV-1 can inhibit the transcription of genes promoted by interferon regulatory factor-3 (IRF-3), including interferon beta (IFN-{beta}), and that the immediate-early ICP0 protein is sufficient for this function. However, the exact mechanism by which ICP0 blocks IRF-3 activity has yet to be determined. Unlike some other viral proteins that inhibit IRF-3 activity, ICP0 does notmore » appear to affect phosphorylation and dimerization of IRF-3. Here, we show that a portion of activated IRF-3 co-localizes with nuclear foci containing ICP0 at early times after virus infection. Co-localization to ICP0-containing foci is also seen with the IRF-3-binding partners and transcriptional co-activators, CBP and p300. In addition, using immunoprecipitation of infected cell lysates, we can immunoprecipitate a complex containing ICP0, IRF-3, and CBP. Thus we hypothesize that ICP0 recruits activated IRF-3 and CBP/p300 to nuclear structures, away from the host chromatin. This leads to the inactivation and accelerated degradation of IRF-3, resulting in reduced transcription of IFN-{beta} and an inhibition of the host response. Therefore, ICP0 provides an example of how viruses can block IFN-{beta} induction by sequestration of important transcription factors essential for the host response.« less

Characterization of silver nanoparticles using flow-field flow fractionation interfaced to inductively coupled plasma mass spectrometry.

PubMed

Poda, A R; Bednar, A J; Kennedy, A J; Harmon, A; Hull, M; Mitrano, D M; Ranville, J F; Steevens, J

2011-07-08

The ability to detect and identify the physiochemical form of contaminants in the environment is important for degradation, fate and transport, and toxicity studies. This is particularly true of nanomaterials that exist as discrete particles rather than dissolved or sorbed contaminant molecules in the environment. Nanoparticles will tend to agglomerate or dissolve, based on solution chemistry, which will drastically affect their environmental properties. The current study investigates the use of field flow fractionation (FFF) interfaced to inductively coupled plasma-mass spectrometry (ICP-MS) as a sensitive and selective method for detection and characterization of silver nanoparticles. Transmission electron microscopy (TEM) is used to verify the morphology and primary particle size and size distribution of precisely engineered silver nanoparticles. Subsequently, the hydrodynamic size measurements by FFF are compared to dynamic light scattering (DLS) to verify the accuracy of the size determination. Additionally, the sensitivity of the ICP-MS detector is demonstrated by fractionation of μg/L concentrations of mixed silver nanoparticle standards. The technique has been applied to nanoparticle suspensions prior to use in toxicity studies, and post-exposure biological tissue analysis. Silver nanoparticles extracted from tissues of the sediment-dwelling, freshwater oligochaete Lumbriculus variegatus increased in size from approximately 31-46nm, indicating a significant change in the nanoparticle characteristics during exposure. Published by Elsevier B.V.

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

PubMed

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

2014-06-01

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

The effect of hydrogen on B4C coatings fabrication in inductively coupled plasma torch

NASA Astrophysics Data System (ADS)

Guo, Q. J.; Zhao, P.; Li, L.; Zhou, Q. J.; Ni, G. H.; Meng, Y. D.

2018-02-01

Boron carbide (B4C) coatings are prepared by an RF inductively coupled plasma (ICP) torch with different amounts of hydrogen introduced into the sheath gas. The effects of the added hydrogen on the characteristics of the plasma are diagnosed by optical emission spectroscopy and high speed photography. The effects on the melting of B4C particles in the plasma are studied by scanning electron microscopy (SEM). The microstructure of the B4C coatings was determined with SEM imaging and x-ray diffraction analysis. The results show that adding hydrogen to the sheath gas leads to plasma contraction, which results in higher gas temperature of plasma. It also enhances B4C particles spheroidizing and improves the compactness of B4C coatings. Plasma processing does not change the main phase of boron carbide. The obtained results on B4C coatings on Cu substrates allows for improving the B4C coatings fabrication process.

Accurate and precise determination of isotopic ratios by MC-ICP-MS: a review.

PubMed

Yang, Lu

2009-01-01

For many decades the accurate and precise determination of isotope ratios has remained a very strong interest to many researchers due to its important applications in earth, environmental, biological, archeological, and medical sciences. Traditionally, thermal ionization mass spectrometry (TIMS) has been the technique of choice for achieving the highest accuracy and precision. However, recent developments in multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) have brought a new dimension to this field. In addition to its simple and robust sample introduction, high sample throughput, and high mass resolution, the flat-topped peaks generated by this technique provide for accurate and precise determination of isotope ratios with precision reaching 0.001%, comparable to that achieved with TIMS. These features, in combination with the ability of the ICP source to ionize nearly all elements in the periodic table, have resulted in an increased use of MC-ICP-MS for such measurements in various sample matrices. To determine accurate and precise isotope ratios with MC-ICP-MS, utmost care must be exercised during sample preparation, optimization of the instrument, and mass bias corrections. Unfortunately, there are inconsistencies and errors evident in many MC-ICP-MS publications, including errors in mass bias correction models. This review examines "state-of-the-art" methodologies presented in the literature for achievement of precise and accurate determinations of isotope ratios by MC-ICP-MS. Some general rules for such accurate and precise measurements are suggested, and calculations of combined uncertainty of the data using a few common mass bias correction models are outlined.

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

NASA Astrophysics Data System (ADS)

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

2017-02-01

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

Metabolomics and Trace Element Analysis of Camel Tear by GC-MS and ICP-MS.

PubMed

Ahamad, Syed Rizwan; Raish, Mohammad; Yaqoob, Syed Hilal; Khan, Altaf; Shakeel, Faiyaz

2017-06-01

Camel tear metabolomics and elemental analysis are useful in getting the information regarding the components responsible for maintaining the protective system that allows living in the desert and dry regions. The aim of this study was to correlate that the camel tears can be used as artificial tears for the evaluation of dryness in the eye. Eye biomarkers of camel tears were analyzed by gas chromatography-mass spectroscopy (GC-MS) and inductively coupled plasma mass spectroscopy (ICP-MS). The major compounds detected in camel tears by GC-MS were alanine, valine, leucine, norvaline, glycine, cadaverine, urea, ribitol, sugars, and higher fatty acids like octadecanoic acid and hexadecanoic acid. GC-MS analysis of camel tears also finds several products of metabolites and its associated metabolic participants. ICP-MS analysis showed the presence of different concentration of elemental composition in the camel tears.

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

PubMed

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

2011-05-01

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

Use of laser ablation-inductively coupled plasma-time of flight-mass spectrometry to identify the elemental composition of vanilla and determine the geographic origin by discriminant function analysis.

PubMed

Hondrogiannis, Ellen M; Ehrlinger, Erin; Poplaski, Alyssa; Lisle, Meredith

2013-11-27

A total of 11 elements found in 25 vanilla samples from Uganda, Madagascar, Indonesia, and Papua New Guinea were measured by laser ablation-inductively coupled plasma-time-of-flight-mass spectrometry (LA-ICP-TOF-MS) for the purpose of collecting data that could be used to discriminate among the origins. Pellets were prepared of the samples, and elemental concentrations were obtained on the basis of external calibration curves created using five National Institute of Standards and Technology (NIST) standards and one Chinese standard with (13)C internal standardization. These curves were validated using NIST 1573a (tomato leaves) as a check standard. Discriminant analysis was used to successfully classify the vanilla samples by their origin. Our method illustrates the feasibility of using LA-ICP-TOF-MS with an external calibration curve for high-throughput screening of spice screening analysis.

Effects of liquid chromatography mobile phases and buffer salts on phosphorus inductively coupled plasma atomic emission and mass spectrometries utilizing ultrasonic nebulization and membrane desolvation.

PubMed

Carr, John E; Kwok, Kaho; Webster, Gregory K; Carnahan, Jon W

2006-01-23

Atomic spectrometry, specifically inductively coupled plasma atomic emission spectrometry (ICP-AES) and mass spectrometry (ICP-MS) show promise for heteroatom-based detection of pharmaceutical compounds. The combination of ultrasonic nebulization (USN) with membrane desolvation (MD) greatly enhances detection limits with these approaches. Because pharmaceutical analyses often incorporate liquid chromatography, the study herein was performed to examine the effects of solvent composition on the analytical behaviors of these approaches. The target analyte was phosphorus, introduced as phosphomycin. AES response was examined at the 253.7 nm atom line and mass 31 ions were monitored for the MS experiments. With pure aqueous solutions, detection limits of 5 ppb (0.5 ng in 0.1 mL injection volumes) were obtained with ICP-MS. The ICP-AES detection limit was 150 ppb. Solvent compositions were varied from 0 to 80% organic (acetonitrile and methanol) with nine buffers at concentrations typically used in liquid chromatography. In general, solvents and buffers had statistically significant, albeit small, effects on ICP-AES sensitivities. A few exceptions occurred in cases where typical liquid chromatography buffer concentrations produced higher mass loadings on the plasma. Indications are that isocratic separations can be reliably performed. Within reasonable accuracy tolerances, it appears that gradient chromatography can be performed without the need for signal response normalization. Organic solvent and buffer effects were more significant with ICP-MS. Sensitivities varied significantly with different buffers and organic solvent content. In these cases, gradient chromatography will require careful analytical calibration as solvent and buffer content is varied. However, for most buffer and solvent combinations, signal and detection limits are only moderately affected. Isocratic separations and detection are feasible.

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

PubMed

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

2017-05-12

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

Measurement of isotope ratios on transient signals by MC-ICP-MS.

PubMed

Günther-Leopold, Ines; Wernli, Beat; Kopajtic, Zlatko; Günther, Detlef

2004-01-01

Precise and accurate isotope ratio measurements are an important task in many applications such as isotope-dilution mass spectrometry, bioavailability studies, or the determination of isotope variations in geological or nuclear samples. The technique of MC-ICP-MS has attracted much attention because it permits the precise measurement of isotope compositions for a wide range of elements combined with excellent detection limits due to high ionisation efficiencies. However, the results are based mainly on measurements using continuous sample introduction. In the present study the determination of isotope ratios on various transient signals with a time duration of 30 to 60 s has been achieved by coupling high-performance liquid chromatography to a multicollector inductively coupled plasma mass spectrometer. In order to investigate the origin of ratio drifts across the transient signals for this hyphenated technique, measurements with the same standard solutions were also carried out using a flow-injection device for sample introduction. As a result of this application it could be concluded that the main source of the bias in the measured isotope ratios is within the ICP-MS instead of fractionation effects on the chromatographic column material. Preliminary studies on short transient signals of gaseous samples (dry plasma) showed a reverse fractionation effect compared with wet plasma conditions (flow injection and HPLC).

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

PubMed

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

2014-07-01

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

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

NASA Astrophysics Data System (ADS)

Makonnen, Yoseif; Beauchemin, Diane

2015-01-01

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

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

PubMed

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

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(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 simultaneous

Specific determination of bromate in bread by ion chromatography with ICP-MS.

PubMed

Akiyama, Takumi; Yamanaka, Michiko; Date, Yukiko; Kubota, Hiroki; Nagaoka, Megumi Hamano; Kawasaki, Yoko; Yamazaki, Takeshi; Yomota, Chikako; Maitani, Tamio

2002-12-01

A sensitive method for detecting bromate in bread by ion chromatography with inductively-coupled plasma mass spectrometry (IC/ICP-MS) was developed. Bromate was extracted from bread with water. The clean-up procedure included a 0.2 micron filter, a C18 cartridge for defatting, a silver cartridge to remove halogen anions, a centrifugal ultrafiltration unit to remove proteins, and a cation-exchange cartridge to remove silver ions. A 500 microL sample solution was applied to IC/ICP-MS. The detection limit and the quantitation limit of bromate in the solution were 0.3 ng/mL and 1.0 ng/mL, expressed as HBrO3, respectively, which corresponded to 2 ng/g and 5 ng/g, respectively, in bread. Recovery of bromate was about 90%, and the CV was about 2%. Based on the detection limit in solution and recovery from bread, the detection limit of bromate in bread was estimated to be 2 ng/g.

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

PubMed

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

2015-07-23

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

Confirmation of Sentinel Lymph Node Identity by Analysis of Fine-Needle Biopsy Samples Using Inductively Coupled Plasma–Mass Spectrometry

PubMed Central

Beavis, Alison; Dawson, Michael; Doble, Philip; Scolyer, Richard A.; Bourne, Roger; Li, Ling-Xi L.; Murali, Rajmohan; Stretch, Jonathan R.; Lean, Cynthia L.; Uren, Roger F.

2008-01-01

Background The sentinel lymph node (SLN) biopsy technique is a reliable means of determining the tumor-harboring status of regional lymph nodes in melanoma patients. When technetium 99 m-labeled antimony trisulfide colloid (99 mTc-Sb2S3) particles are used to perform preoperative lymphoscintigraphy for SLN identification, they are retained in the SLN but are absent or present in only tiny amounts in non-SLNs. The present study investigated the potential for a novel means of assessing the accuracy of surgical identification of SLNs. This involved the use of inductively coupled plasma–mass spectrometry (ICP-MS) to analyze antimony concentrations in fine-needle biopsy (FNB) samples from surgically procured lymph nodes. Methods A total of 47 FNB samples from surgically excised lymph nodes (32 SLNs and 15 non-SLNs) were collected. The SLNs were localized by preoperative lymphoscintigraphy that used 99 mTc-Sb2S3, blue dye, and gamma probe techniques. The concentrations of antimony were measured in the FNB samples by ICP-MS. Results The mean and median antimony concentrations (in parts per billion) were .898 and .451 in the SLNs, and .015 and .068 in the non-SLNs, the differences being highly statistically significant (P < .00005). Conclusions Our results show that ICP-MS analysis of antimony concentrations in FNB specimens from lymph nodes can accurately confirm the identity of SLNs. Used in conjunction with techniques such as proton magnetic resonance spectroscopy for the nonsurgical evaluation of SLNs, ICP-MS analysis of antimony concentrations in FNB samples could potentially serve as a minimally invasive alternative to surgery and histopathologic evaluation to objectively classify a given node as sentinel or nonsentinel and determine its tumor-harboring status. PMID:18172734

Investigation of the RF efficiency of inductively coupled hydrogen plasmas at 1 MHz

NASA Astrophysics Data System (ADS)

Rauner, D.; Mattei, S.; Briefi, S.; Fantz, U.; Hatayama, A.; Lettry, J.; Nishida, K.; Tran, M. Q.

2017-08-01

The power requirements of RF heated sources for negative hydrogen ions in fusion are substantial, which poses strong demands on the generators and components of the RF circuit. Consequently, an increase of the RF coupling efficiency would be highly beneficial. Fundamental investigations of the RF efficiency in inductively coupled hydrogen and deuterium discharges in cylindrical symmetry are conducted at the lab experiment CHARLIE. The experiment is equipped with several diagnostics including optical emission spectroscopy and a movable floating double probe to monitor the plasma parameters. The presented investigations are performed in hydrogen at a varying pressure between 0.3 and 10 Pa, utilizing a conventional helical ICP coil driven at a frequency of 1 MHz and a fixed power of 520 W for plasma generation. The coupling efficiency is strongly affected by the variation in pressure, reaching up to 85 % between 1 and 3 Pa while dropping down to only 50 % at 0.3 Pa, which is the relevant operating pressure for negative hydrogen ion sources for fusion. Due to the lower power coupling, also the measured electron density at 0.3 Pa is only 5 . 1016 m-3, while it reaches up to 2.5 . 1017 m-3 with increasing coupling efficiency. In order to gain information on the spatially resolved aspects of RF coupling and plasma heating which are not diagnostically accessible, first simulations of the discharge by an electromagnetic Particle-In-Cell Monte Carlo collision method have been conducted and are compared to the measurement data. At 1 Pa, the simulated data corresponds well to the results of both axially resolved probe measurements and radially resolved emission profiles obtained via OES. Thereby, information regarding the radial distribution of the electron density and mean energy is provided, revealing a radial distribution of the electron density which is well described by a Bessel profile.

Two-dimensional on-line detection of brominated and iodinated volatile organic compounds by ECD and ICP-MS after GC separation.

PubMed

Schwarz, A; Heumann, K G

2002-09-01

Inductively coupled plasma-mass spectrometry (ICP-MS) was coupled to a gas chromatographic (GC) system with electron capture detector (ECD), which enables relatively easy characterization and quantification of brominated and iodinated (halogenated) volatile organic compounds (HVOCs) in aquatic and air samples. The GC-ECD system is connected in series with an ICP-MS by a directly heated transfer line and an outlet port-hole for elimination of the ECD make-up gas during ignition of the plasma. The hyphenated GC-ECD/ICP-MS system provides high selectivity and sensitivity for monitoring individual HVOCs under fast chromatographic conditions. The ECD is most sensitive for the detection of chlorinated and brominated but the ICP-MS for iodinated compounds. The greatest advantage of the use of an ICP-MS is its element-specific detection, which allows clear identification of compounds in most cases. The absolute detection limits for ICP-MS are 0.5 pg for iodinated, 10 pg for brominated, and 50 pg for chlorinated HVOCs with the additional advantage that calibration is almost independent on different compounds of the same halogen. In contrast to that detection limits for ECD vary for the different halogenated compounds and lie in the range of 0.03-11 pg. The two-dimensional GC-ECD/ICP-MS instrumentation is compared with electron impact mass spectrometry (EI-MS) and microwave induced plasma atomic emission detection (MIP-AED). Even if EI-MS has additional power in identifying unknown peaks by its scan mode, the detection limits are much higher compared with GC-ECD/ICP-MS, whereas the selective ion monitoring mode (SIM) reaches similar detection limits. The MIP-AED detection limits are at the same level as EI-MS in the scan mode.

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

NASA Astrophysics Data System (ADS)

Zhang, Gai; Tian, Min

2015-04-01

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

Selective solid phase extraction of copper using a new Cu(II)-imprinted polymer and determination by inductively coupled plasma optical emission spectroscopy (ICP-OES).

PubMed

Yilmaz, Vedat; Arslan, Zikri; Hazer, Orhan; Yilmaz, Hayriye

2014-05-01

This work reports the preparation of a novel Cu(II)-ion imprinted polymer using 2-thiozylmethacrylamide (TMA) for on-line preconcentration of Cu(II) prior to its determination by inductively coupled optical emission spectroscopy (ICP-OES). Cu(II)-TMA monomer (complex) was synthesized and copolymerized via bulk polymerization method in the presence of ethyleneglycoldimethacrylate cross-linker. The resulting polymer was washed with 5% (v/v) HNO 3 to remove Cu(II) ions and then with water until a neutral pH. The ion imprinted polymer was characterized by FT-IR and scanning electron microscopy. The experimental conditions were optimized for on-line preconcentration of Cu(II) using a minicolumn of ion imprinted polymer (IIP). Quantitative retention was achieved between pH 5.0 and 6.0, whereas the recoveries for the non-imprinted polymer (NIP) were about 61%. The IIP showed about 30 times higher selectivity to Cu(II) in comparison to NIP. The IIP also exhibited excellent selectivity for Cu(II) against the competing transition and heavy metal ions, including Cd, Co, Cr, Fe, Mn, Ni, Pb and Zn. Computational calculations revealed that the selectivity of IIP was mediated by the stability of Cu(II)-TMA complex which was far more stable than those of Co(II), Ni(II) and Zn(II) that have similar charge and ionic radii to Cu(II). A volume of 10 mL sample solution was loaded onto the column at 4.0 mL min -1 by using a sequential injection system (FIALab 3200) followed by elution with 1.0 mL of 2% (v/v) HNO 3 . The relative standard deviation (RSD) and limit of detection (LOD, 3s) of the method were 3.2% and 0.4 μg L -1 , respectively. The method was successfully applied to determination of Cu(II) in fish otoliths (CRM 22), bone ash (SRM 1400) and coastal seawater and estuarine water samples.

Selective solid phase extraction of copper using a new Cu(II)-imprinted polymer and determination by inductively coupled plasma optical emission spectroscopy (ICP-OES)

PubMed Central

Yilmaz, Vedat; Arslan, Zikri; Hazer, Orhan; Yilmaz, Hayriye

2014-01-01

This work reports the preparation of a novel Cu(II)-ion imprinted polymer using 2-thiozylmethacrylamide (TMA) for on-line preconcentration of Cu(II) prior to its determination by inductively coupled optical emission spectroscopy (ICP-OES). Cu(II)-TMA monomer (complex) was synthesized and copolymerized via bulk polymerization method in the presence of ethyleneglycoldimethacrylate cross-linker. The resulting polymer was washed with 5% (v/v) HNO3 to remove Cu(II) ions and then with water until a neutral pH. The ion imprinted polymer was characterized by FT-IR and scanning electron microscopy. The experimental conditions were optimized for on-line preconcentration of Cu(II) using a minicolumn of ion imprinted polymer (IIP). Quantitative retention was achieved between pH 5.0 and 6.0, whereas the recoveries for the non-imprinted polymer (NIP) were about 61%. The IIP showed about 30 times higher selectivity to Cu(II) in comparison to NIP. The IIP also exhibited excellent selectivity for Cu(II) against the competing transition and heavy metal ions, including Cd, Co, Cr, Fe, Mn, Ni, Pb and Zn. Computational calculations revealed that the selectivity of IIP was mediated by the stability of Cu(II)-TMA complex which was far more stable than those of Co(II), Ni(II) and Zn(II) that have similar charge and ionic radii to Cu(II). A volume of 10 mL sample solution was loaded onto the column at 4.0 mL min−1 by using a sequential injection system (FIALab 3200) followed by elution with 1.0 mL of 2% (v/v) HNO3. The relative standard deviation (RSD) and limit of detection (LOD, 3s) of the method were 3.2% and 0.4 μg L−1, respectively. The method was successfully applied to determination of Cu(II) in fish otoliths (CRM 22), bone ash (SRM 1400) and coastal seawater and estuarine water samples. PMID:24511158

Dithizone-functionalized solid phase extraction-displacement elution-high performance liquid chromatography-inductively coupled plasma mass spectrometry for mercury speciation in water samples.

PubMed

Yin, Yong-guang; Chen, Ming; Peng, Jin-feng; Liu, Jing-fu; Jiang, Gui-bin

2010-06-15

A novel and simple solid phase extraction (SPE)-high performance liquid chromatography (HPLC)-inductively coupled plasma mass spectrometry (ICP-MS) method was developed for determination of inorganic mercury (IHg), methylmercury MeHg and ethylmercury (EtHg) in water samples in the present work. The procedure involves pre-functionalization of the commercially available C18 SPE column with dithizone, loading water sample, displacement elution of mercury species by Na(2)S(2)O(3) solution, followed by HPLC-ICP-MS determination. Characterization and optimization of operation parameters of this new SPE procedure were discussed, including eluting reagent selection, concentration of eluting reagent, volume of eluting reagent, effect of NaCl and humic acid in sample matrix. At optimized conditions, the detection limits of mercury species for 100mL water sample were about 3ngL(-1) and the average recoveries were 93.7, 83.4, and 71.7% for MeHg, IHg and EtHg, respectively, by spiking 0.2microgL(-1) mercury species into de-ion water. Stability experiment reveals that both the dithizone-functionalized SPE cartridge and the mercury species incorporated were stable in the storage procedure. These results obtained demonstrate that SPE-HPLC-ICP-MS is a simple and sensitive technique for the determination of mercury species at trace level in water samples with high reproducibility and accuracy.

Quantitative bioimaging of trace elements in the human lens by LA-ICP-MS.

PubMed

Konz, Ioana; Fernández, Beatriz; Fernández, M Luisa; Pereiro, Rosario; González-Iglesias, Héctor; Coca-Prados, Miguel; Sanz-Medel, Alfredo

2014-04-01

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) was used for the quantitative imaging of Fe, Cu and Zn in cryostat sections of human eye lenses and for depth profiling analysis in bovine lenses. To ensure a tight temperature control throughout the experiments, a new Peltier-cooled laser ablation cell was employed. For quantification purposes, matrix-matched laboratory standards were prepared from a pool of human lenses from eye donors and spiked with standard solutions containing different concentrations of natural abundance Fe, Cu and Zn. A normalisation strategy was also carried out to correct matrix effects, lack of tissue homogeneity and/or instrumental drifts using a thin gold film deposited on the sample surface. Quantitative images of cryo-sections of human eye lenses analysed by LA-ICP-MS revealed a homogeneous distribution of Fe, Cu and Zn in the nuclear region and a slight increase in Fe concentration in the outer cell layer (i.e. lens epithelium) at the anterior pole. These results were assessed also by isotope dilution mass spectrometry, and Fe, Cu and Zn concentrations determined by ID-ICP-MS in digested samples of lenses and lens capsules.

High-precision Ru isotopic measurements by multi-collector ICP-MS.

PubMed

Becker, Harry; Dalpe, Claude; Walker, Richard J

2002-06-01

Ruthenium isotopic data for a pure Aldrich ruthenium nitrate solution obtained using a Nu Plasma multi collector inductively coupled plasma-mass spectrometer (MC-ICP-MS) shows excellent agreement (better than 1 epsilon unit = 1 part in 10(4)) with data obtained by other techniques for the mass range between 96 and 101 amu. External precisions are at the 0.5-1.7 epsilon level (2sigma). Higher sensitivity for MC ICP-MS compared to negative thermal ionization mass spectrometry (N-TIMS) is offset by the uncertainties introduced by relatively large mass discrimination and instabilities in the plasma source-ion extraction region that affect the long-term reproducibility. Large mass bias correction in ICP mass spectrometry demands particular attention to be paid to the choice of normalizing isotopes. Because of its position in the mass spectrum and the large mass bias correction, obtaining precise and accurate abundance data for 104Ru by MC-ICP-MS remains difficult. Internal and external mass bias correction schemes in this mass range may show similar shortcomings if the isotope of interest does not lie within the mass range covered by the masses used for normalization. Analyses of meteorite samples show that if isobaric interferences from Mo are sufficiently large (Ru/Mo < 10(4)), uncertainties on the Mo interference correction propagate through the mass bias correction and yield inaccurate results for Ru isotopic compositions. Second-order linear corrections may be used to correct for these inaccuracies, but such results are generally less precise than N-TIMS data.

Chip-based magnetic solid phase microextraction coupled with ICP-MS for the determination of Cd and Se in HepG2 cells incubated with CdSe quantum dots.

PubMed

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

2018-03-01

The quantification of trace Cd and Se in cells incubated with CdSe quantum dots (QDs) is critical to investigate the cytotoxicity of CdSe QDs. In this work, a miniaturized platform, namely chip-based magnetic solid phase microextraction (MSPME) packing with sulfhydryl group functionalized magnetic nanoparticles, was fabricated and combined with inductively coupled plasma mass spectrometry (ICP-MS) for the determination of trace Cd and Se in cells. Under the optimized conditions, the limits of detection (LOD) of the developed chip-based MSPME-ICP-MS system are 2.2 and 21ngL -1 for Cd and Se, respectively. The proposed method is applied successfully to the analysis of total and released small molecular fraction of Cd and Se in Human hepatocellular carcinoma cells (HepG2 cells) incubated with CdSe QDs, and the recoveries for the spiked samples are in the range of 86.0-109%. This method shows great promise to analyze cell samples and the obtained results are instructive to explore the cytotoxicity mechanism of CdSe QDs in cells. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of Plutonium Isotope Ratios at Very Low Levels by ICP-MS using On-Line Electrochemically Modulated Separations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liezers, Martin; Lehn, Scott A; Olsen, Khris B

2009-10-01

Electrochemically modulated separations (EMS) are shown to be a rapid and selective means of extracting and concentrating Pu from complex solutions prior to isotopic analysis by inductively coupled plasma mass spectrometry (ICP-MS). This separation is performed in a flow injection mode, on-line with the ICP-MS. A three-electrode, flow-by electrochemical cell is used to accumulate Pu at an anodized glassy carbon electrode by redox conversion of Pu(III) to Pu (IV&VI). The entire process takes place in 2% v/v (0.46M) HNO 3. No redox chemicals or acid concentration changes are required. Plutonium accumulation and release is redox dependent and controlled by themore » applied cell potential. Thus large transient volumetric concentration enhancements can be achieved. Based on more negative U(IV) potentials relative to Pu(IV), separation of Pu from uranium is efficient, thereby eliminating uranium hydride interferences. EMS-ICP-MS isotope ratio measurement performance will be presented for femtogram to attogram level plutonium concentrations.« less

Arsenic species separation by IELC-ICP/OES: Arsenocholine behavior

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rubio, R.; Peralta, I.; Alberti, J.

1993-01-01

In the literature an increasing interest is observed in developing methods to determine arsenobetaine, arsenocholine and related compounds in sea food and in reference materials. The separation conditions and quantification of As(III), As(V), monomethylarsenate (MMA), dimethylarsinate (DMA), arsenobetaine (AsBet) and arsenocholine (AsChol) are studied by Liquid Chromatography (LC) coupled directly to an Inductively Coupled Plasma Optical Emission Spectroscopy (ICP/OES) system. The separation conditions are optimized to improve the resolution of the six arsenic species. Arsenocholine shows a particular pattern of behavior when phosphate is used as eluent: two peaks are observed in the chromatogram, thus a systematic study assaying differentmore » pH and concentration of phosphate is carried out to improve resolution and analysis time when the six arsenic compounds are analyzed in a mixture. Boric acid as mobile phase avoids the splitting of the arsenocholine peak and leads to a good separation of the six arsenic compounds. Detection limits are established for the six arsenic species.« less

Improvements on high-precision measurement of bromine isotope ratios by multicollector inductively coupled plasma mass spectrometry.

PubMed

Wei, Hai-Zhen; Jiang, Shao-Yong; Zhu, Zhi-Yong; Yang, Tao; Yang, Jing-Hong; Yan, Xiong; Wu, He-Pin; Yang, Tang-Li

2015-10-01

A new, feasible procedure for high-precision bromine isotope analysis using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is described. With a combination of HR mass resolution mode and accurate optimization of the Zoom Optics parameters (Focus Quad: -1.30; Zoom Quad: 0.00), the challenging problem of the isobaric interferences ((40)Ar(38)ArH(+) and (40)Ar(40)ArH(+)) in the measurement of bromine isotopes ((79)Br(+), (81)Br(+)) has been effectively solved. The external reproducibility of the measured (81)Br/(79)Br ratios in the selected standard reference materials ranged from ±0.03‰ to ±0.14‰, which is superior to or equivalent to the best results from previous contributions. The effect of counter cations on the Br(+) signal intensity and the instrumental-induced mass bias was evaluated as the loss of HBr aerosol in nebulizer and potential diffusive isotope fractionations. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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.

Determination of toxic inorganic elements pollution in ground waters of Kahuta Industrial Triangle Islamabad, Pakistan using inductively coupled plasma mass spectrometry.

PubMed

Kausar, Rubina; Ahmad, Zulfiqar

2009-10-01

The present study deals with the ground water quality assessment in Kahuta Industrial Triangle Islamabad, Pakistan. The objective of the study was to assess ground water quality against the drinking water standards for various toxic inorganic elements. Representative groundwater samples were collected and analyzed in the Water Quality Laboratory of Pakistan Council of Research in Water Resources (PCRWR) at Islamabad, Pakistan. The samples were run on ICP-MS (Inductively coupled plasma mass spectrometry), which has the capability to separate and quantify 70 elements at a time. One of the finding of study is that ICP-MS is a very good tool to analyze broad range of toxic inorganic elements to the level of parts per billion (ppb). World Health Organization drinking water standards shows that these toxic inorganic elements such as heavy metals even at this concentration level (ppb) are injurious to human health. This analysis indicated pollution of various toxic elements including Selenium. Vertical leachate through industrial waste septic tanks is identified as major cause of groundwater pollution in the Industrial Triangle. Monitoring of the septic tanks and groundwater quality in study area is suggested along with remedial measures.

Evaluation of microwave and ultrasound extraction procedures for arsenic speciation in bivalve mollusks by liquid chromatography-inductively coupled plasma-mass spectrometry

NASA Astrophysics Data System (ADS)

Santos, Clarissa M. M.; Nunes, Matheus A. G.; Barbosa, Isa S.; Santos, Gabriel L.; Peso-Aguiar, Marlene C.; Korn, Maria G. A.; Flores, Erico M. M.; Dressler, Valderi L.

2013-08-01

Liquid chromatography-inductively coupled plasma-mass spectrometry (LC-ICP-MS) was used for arsenic speciation analysis in tissues of bivalve mollusks (Anomalocardia brasiliana sp. and Macoma constricta sp.). Microwave and ultrasound radiation, combined with different extraction conditions (solvent, sample amount, time, and temperature), were evaluated for As-species extraction from the mollusks' tissues. Accuracy, extraction efficiency, and the stability of As species were evaluated by analyzing certified reference materials (DORM-2, dogfish muscle; BCR-627, tuna fish tissue; and SRM 1566b, oyster tissue) and analyte recovery tests. The best conditions were found to be microwave-assisted extraction using 200 mg of samples and water at 80 °C for 6 min. The agreement of As-species concentration in samples ranged from 97% to 102%. Arsenobetaine (AsB) was the main species present in bivalve mollusk tissues, while monomethylarsonic acid (MMA) and arsenate (As(V)) were below the limit of quantification (0.001 and 0.003 μg g- 1, respectively). Two unidentified As species also were detected and quantified. The sum of the As-species concentration was in agreement (90 to 104%), with the total As content determined by ICP-MS after sample digestion.

A comparison of laser ablation-inductively coupled plasma-mass spectrometry and high-resolution continuum source graphite furnace molecular absorption spectrometry for the direct determination of bromine in polymers

NASA Astrophysics Data System (ADS)

de Gois, Jefferson S.; Van Malderen, Stijn J. M.; Cadorim, Heloisa R.; Welz, Bernhard; Vanhaecke, Frank

2017-06-01

This work describes the development and comparison of two methods for the direct determination of Br in polymer samples via solid sampling, one using laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) and the other using high-resolution continuum source graphite furnace molecular absorption spectrometry with direct solid sample analysis (HR-CS SS-GF MAS). The methods were optimized and their accuracy was evaluated by comparing the results obtained for 6 polymeric certified reference materials (CRMs) with the corresponding certified values. For Br determination with LA-ICP-MS, the 79Br+ signal could be monitored interference-free. For Br determination via HR-CS SS-GF MAS, the CaBr molecule was monitored at 625.315 nm with integration of the central pixel ± 1. Bromine quantification by LA-ICP-MS was performed via external calibration against a single CRM while using the 12C+ signal as an internal standard. With HR-CS SS-GF MAS, Br quantification could be accomplished using external calibration against aqueous standard solutions. Except for one LA-ICP-MS result, the concentrations obtained with both techniques were in agreement with the certified values within the experimental uncertainty as evidenced using a t-test (95% confidence level). The limit of quantification was determined to be 100 μg g- 1 Br for LA-ICP-MS and 10 μg g- 1 Br for HR-CS SS-GF MAS.

Application of SEC-ICP-MS for comparative analyses of metal-containing species in cancerous and healthy human thyroid samples.

PubMed

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.

Using ICP-OES and SEM-EDX in biosorption studies

PubMed Central

Chojnacka, Katarzyna; Marycz, Krzysztof

2010-01-01

We have compared the analytical results obtained by inductively coupled plasma optical emission spectroscopy (ICP-OES) and by scanning electron microscopy with an energy dispersive X-ray analytical system (SEM-EDX) in order to explore the mechanism of metal ions biosorption by biomass using two independent methods. The marine macroalga Enteromorpha sp. was enriched with Cu(II), Mn(II), Zn(II), and Co(II) ions via biosorption, and the biosorption capacity of alga determined from the solution and biomass composition before and after biosorption process was compared. The first technique was used to analyze the composition of the natural and metal-loaded biomass, and additionally the composition of the solution before and after biosorption. The second technique was used to obtain a picture of the surface of natural and metal ion-loaded macroalgae, to map the elements on the cell wall of dry biomass, and to determine their concentration before and after biosorption. ICP-OES showed a better precision and lower detection limit than EDX, but SEM-EDX gave more information regarding the sample composition of Enteromorpha sp. Both techniques confirmed that biosorption is a surface phenomenon, in which alkali and alkaline earth metal ions were exchanged by metal ions from aqueous solution. Figure The advantages and disadvantages of ICP-OES and SEM-EDX techniques Electronic supplementary material The online version of this article (doi:10.1007/s00604-010-0468-0) contains supplementary material, which is available to authorized users. PMID:21423317

Using ICP-OES and SEM-EDX in biosorption studies.

PubMed

Michalak, Izabela; Chojnacka, Katarzyna; Marycz, Krzysztof

2011-02-01

We have compared the analytical results obtained by inductively coupled plasma optical emission spectroscopy (ICP-OES) and by scanning electron microscopy with an energy dispersive X-ray analytical system (SEM-EDX) in order to explore the mechanism of metal ions biosorption by biomass using two independent methods. The marine macroalga Enteromorpha sp. was enriched with Cu(II), Mn(II), Zn(II), and Co(II) ions via biosorption, and the biosorption capacity of alga determined from the solution and biomass composition before and after biosorption process was compared. The first technique was used to analyze the composition of the natural and metal-loaded biomass, and additionally the composition of the solution before and after biosorption. The second technique was used to obtain a picture of the surface of natural and metal ion-loaded macroalgae, to map the elements on the cell wall of dry biomass, and to determine their concentration before and after biosorption. ICP-OES showed a better precision and lower detection limit than EDX, but SEM-EDX gave more information regarding the sample composition of Enteromorpha sp. Both techniques confirmed that biosorption is a surface phenomenon, in which alkali and alkaline earth metal ions were exchanged by metal ions from aqueous solution.FigureThe advantages and disadvantages of ICP-OES and SEM-EDX techniques ELECTRONIC SUPPLEMENTARY MATERIAL: The online version of this article (doi:10.1007/s00604-010-0468-0) contains supplementary material, which is available to authorized users.

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

PubMed

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.

Inductively coupled plasma mass spectrometry with a twin quadrupole instrument using laser ablation sample introduction and monodisperse dried microparticulate injection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Allen, Lloyd A.

1996-10-17

The focus of this dissertation is the use of a twin quadrupole inductively coupled plasma mass spectrometer (ICP-MS) for the simultaneous detection of two m/z values. The twin quadrupole ICP-MS is used with laser ablation sample introduction in both the steady state (10 Hz) and single pulse modes. Steady state signals are highly correlated and the majority of flicker noise cancels when the ratio is calculated. Using a copper sample, the isotope ratio 63Cu +/ 65Cu + is measured with a relative standard deviation (RSD) of 0.26%. Transient signals for single laser pulses are also obtained. Copper isotope ratio measurementsmore » for several laser pulses are measured with an RSD of 0.85%. Laser ablation (LA) is used with steel samples to assess the ability of the twin quadrupole ICP-MS to eliminate flicker noise of minor components of steel samples. Isotopic and internal standard ratios are measured in the first part of this work. The isotope ratio 52Cr +/ 53Cr + (Cr present at 1.31 %) can be measured with an RSD of 0.06 % to 0.1 %. For internal standard elements, RSDs improve from 1.9 % in the Cr + signal to 0.12% for the ratio of 51V + to 52Cr +. In the second part of this work, one mass spectrometer is scanned while the second channel measures an individual m/z value. When the ratio of these two signals is calculated, the peak shapes in the mass spectrum are improved significantly. Pulses of analyte and matrix ions from individual drops are measured simultaneously using the twin quadrupole ICP-MS with monodisperse dried microparticulate injection (MDMI). At modest Pb concentrations (500 ppm), a shoulder on the leading edge of the Li + signal becomes apparent. Space charge effects are consistent with the disturbances seen.« less

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

PubMed

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.

Studies of LA-ICP-MS on quartz glasses at different wavelengths of a Nd:YAG laser.

PubMed

Becker, J S; Tenzler, D

2001-07-01

The capability of LA-ICP-MS for determination of trace impurities in transparent quartz glasses was investigated. Due to low or completely lacking absorption of laser radiation, laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) proves difficult on transparent solids, and in particular the quantification of measurement results is problematic in these circumstances. Quartz glass reference materials of various compositions were studied by using a Nd:YAG laser system with focused laser radiation of wavelengths of 1064 nm, 532 nm and 266 nm, and an ICP-QMS (Elan 6000, Perkin Elmer). The influence of ICP and laser ablation conditions in the analysis of quartz glasses of different compositions was investigated, with the laser power density in the region of interaction between laser radiation and solid surface determining the ablation process. The trace element concentration was determined via calibration curves recorded with the aid of quartz glass reference materials. Under optimized measuring conditions the correlation coefficients of the calibration curves are in the range of 0.9-1. The relative sensitivity factors of the trace elements determined in the quartz glass matrix are 0.1-10 for most of the trace elements studied by LA-ICP-MS. The detection limits of the trace elements in quartz glass are in the low ng/g to pg/g range.

RAPID DETERMINATION OF ACTINIDES IN URINE BY INDUCTIVELY-COUPLED PLASMA MASS SPECTROMETRY AND ALPHA SPECTROMETRY: A HYBRID APPROACH

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, S.; Jones, V.

2009-05-27

A new rapid separation method that allows separation and preconcentration of actinides in urine samples was developed for the measurement of longer lived actinides by inductively coupled plasma mass spectrometry (ICP-MS) and short-lived actinides by alpha spectrometry; a hybrid approach. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration, if required, is performed using a streamlined calcium phosphate precipitation. Similar technology has been applied to separate actinides prior to measurement by alpha spectrometry, but this new method has been developed with elution reagents now compatible with ICP-MS as well. Purified solutions are splitmore » between ICP-MS and alpha spectrometry so that long- and short-lived actinide isotopes can be measured successfully. The method allows for simultaneous extraction of 24 samples (including QC samples) in less than 3 h. Simultaneous sample preparation can offer significant time savings over sequential sample preparation. For example, sequential sample preparation of 24 samples taking just 15 min each requires 6 h to complete. The simplicity and speed of this new method makes it attractive for radiological emergency response. If preconcentration is applied, the method is applicable to larger sample aliquots for occupational exposures as well. The chemical recoveries are typically greater than 90%, in contrast to other reported methods using flow injection separation techniques for urine samples where plutonium yields were 70-80%. This method allows measurement of both long-lived and short-lived actinide isotopes. 239Pu, 242Pu, 237Np, 243Am, 234U, 235U and 238U were measured by ICP-MS, while 236Pu, 238Pu, 239Pu, 241Am, 243Am and 244Cm were measured by alpha spectrometry. The method can also be adapted so that the separation of uranium isotopes for assay is not required, if uranium assay by direct dilution of the urine sample is preferred

Investigating Uranium Concentrations in Groundwaters in the State of Idaho Using Kinetic Phosphorescence Analysis and Inductively Coupled Plasma Mass Spectrometry.

PubMed

Tkavadze, Levan; Dunker, Roy E; Brey, Richard R; Dudgeon, John

2016-11-01

The determination of uranium concentrations in natural water samples is of great interest due to the environmental consequences of this radionuclide. In this study, 380 groundwater samples from various locations within the state of Idaho were analyzed using two different techniques. The first method was Kinetic Phosphorescence Analysis (KPA), which gives the total uranium concentrations in water samples. The second analysis method was inductively coupled plasma mass spectrometry (ICP- MS). This method determines the total uranium concentration as well as the separate isotope concentrations of uranium. The U/U isotopic ratio was also measured for each sample to confirm that there was no depleted or enriched uranium present. The results were compared and mapped separately from each other. The study also found that in some areas of the state, natural uranium concentrations are relatively high.

Comparative evaluation of GFAAS and ICP-MS for analyses of cadmium in blood.

PubMed

Fukui, Yoshinari; Ohashi, Fumiko; Sakuragi, Sonoko; Moriguchi, Jiro; Ikeda, Masayuki

2011-01-01

Cadmium in blood (Cd-B) is an important indicator, next to Cd in urine, in biological monitoring of exposure to Cd. The present study was initiated to examine compatibility in results of analysis for Cd-B between graphite furnace atomic absorption spectrophotometry (GFAAS) and inductively-coupled plasma mass-spectrometry (ICP-MS). For this purpose, 1,159 blood samples were collected from adult women (with no occupational exposure to Cd) in eight prefectures nation-widely in Japan. The samples were analyzed by the two methods; geometric mean (the maximum) concentrations were 1.22 (6.90) μg/l by ICP-MS, and 1.47 (7.40) μg/l by GFAAS. Statistical analyses showed that there was a close correlation between the results by the two methods. The regression line (with ICP-MS and GFAAS results as an independent variable and a dependent variable, respectively) had a slope close to one and an intercept next to zero to suggest that ICP-MS gave values compatible with that of GFAAS. Further analysis with the ratio of Cd-B by GFAAS over that by ICP-MS revealed that the two results were close to each other, and that the agreement was even closer when Cd-B was >2 μg/l. Thus, the two methods can be employed inter-convertibly when Cd-B is relatively high, e.g. >2 μg/l. Care may need to be practiced, however, for possible 'between methods' difference when Cd-B is low, e.g., ≤2 μg/l.

Comparative tissue distribution of metals in birds in Sweden using ICP-MS and laser ablation ICP-MS.

PubMed

Ek, Kristine H; Morrison, Gregory M; Lindberg, Peter; Rauch, Sébastien

2004-08-01

Cadmium, copper, lead, palladium, platinum, rhodium, and zinc profiles were investigated along feather shafts of raptor and other bird species by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). The distribution of external versus internal metal contamination of feathers was investigated. The species examined were peregrine falcon (Falco peregrinus), sparrowhawk ( Accipiter nisus), willow grouse (Lagopus lagopus), and house sparrow (Passer domesticus) in Sweden. For habitat comparisons, total Cu, Pb, Zn, and Cd concentrations were analyzed by ICP-MS in feathers of the examined species as well as captive peregrine falcon. For investigation of metal distribution and correlation in different biological materials of raptors, total concentrations of Cu, Pb, Cd, and Zn were also investigated by ICP-MS in feathers, eggs, blood, feces, liver, and kidney of wild peregrine falcon from southwestern Sweden. Laser ablation of feathers revealed that Pb contamination is both external and internal, Zn contamination is internal, and Cd and Cu contamination is predominantly internal, with a few externally attached particles of high concentration. Pb, Cu, and Cd signal intensities were highest in urban habitats and contamination was mainly external in feathers. The background signal intensity of Zn was also higher in birds from urban habitats. The laser ablation profile of PGE (Pt, Pd, Rh) demonstrated that PGE contamination of feathers consists almost exclusively of externally attached PGE-containing particles, with little evidence of internally deposited PGE.Generally, total metal concentrations in feathers were highest in sparrowhawk and house sparrow due to their urban habitat. Total Cu, Zn, and Cd concentrations were highest in liver and kidney due to binding to metallothionein, while the total Pb concentration was highest in feces due to the high excretion rate of Pb. A decreasing temporal trend for Pb in feathers, showing that Pb levels in feathers have

Interlaboratory evaluation of trace element determination in workplace air filter samples by inductively coupled plasma mass spectrometry†‡

PubMed Central

Shulman, Stanley A.; Brisson, Michael J.; Howe, Alan M.

2015-01-01

Inductively coupled plasma mass spectrometry (ICP-MS) is becoming more widely used for trace elemental analysis in the occupational hygiene field, and consequently new ICP-MS international standard procedures have been promulgated by ASTM International and ISO. However, there is a dearth of interlaboratory performance data for this analytical methodology. In an effort to fill this data void, an interlaboratory evaluation of ICP-MS for determining trace elements in workplace air samples was conducted, towards fulfillment of method validation requirements for international voluntary consensus standard test methods. The study was performed in accordance with applicable statistical procedures for investigating interlaboratory precision. The evaluation was carried out using certified 37-mm diameter mixed-cellulose ester (MCE) filters that were fortified with 21 elements of concern in occupational hygiene. Elements were spiked at levels ranging from 0.025 to 10 μg filter−1, with three different filter loadings denoted “Low”, “Medium” and “High”. Participating laboratories were recruited from a pool of over fifty invitees; ultimately twenty laboratories from Europe, North America and Asia submitted results. Triplicates of each certified filter with elemental contents at three different levels, plus media blanks spiked with reagent, were conveyed to each volunteer laboratory. Each participant was also provided a copy of the test method which each participant was asked to follow; spiking levels were unknown to the participants. The laboratories were requested to prepare the filters by one of three sample preparation procedures, i.e., hotplate digestion, microwave digestion or hot block extraction, which were described in the test method. Participants were then asked to analyze aliquots of the prepared samples by ICP-MS, and to report their data in units of μg filter−1. Most interlaboratory precision estimates were acceptable for medium- and high

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

PubMed Central

Axelsson, Mikael D; Rodushkin, Ilia; Baxter, Douglas C; Ingri, Johan; Öhlander, Björn

2002-01-01

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.

The influence of ns- and fs-LA plume local conditions on the performance of a combined LIBS/LA-ICP-MS sensor

DOE Office of Scientific and Technical Information (OSTI.GOV)

LaHaye, Nicole L.; Phillips, Mark C.; Duffin, Andrew M.

2016-01-01

Both laser-induced breakdown spectroscopy (LIBS) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) are well-established analytical techniques with their own unique advantages and disadvantages. The combination of the two analytical methods is a very promising way to overcome the challenges faced by each method individually. We made a comprehensive comparison of local plasma conditions between nanosecond (ns) and femtosecond (fs) laser ablation (LA) sources in a combined LIBS and LA-ICP-MS system. The optical emission spectra and ICP-MS signal were recorded simultaneously for both ns- and fs-LA and figures of merit of the system were analyzed. Characterization of the plasma was conductedmore » by evaluating temperature and density of the plume under various irradiation conditions using optical emission spectroscopy, and correlations to ns- and fs-LIBS and LA-ICP-MS signal were made. The present study is very useful for providing conditions for a multimodal system as well as giving insight into how laser ablation plume parameters are related to LA-ICP-MS and LIBS results for both ns- and fs-LA.« less

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

PubMed

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.

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

PubMed

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.

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

NASA Astrophysics Data System (ADS)

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

2017-11-01

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

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

NASA Astrophysics Data System (ADS)

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

2000-02-01

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

Influence of instrumental parameters on the kinetic energy of ions and plasma temperature for a hexapole collision/reaction-cell-based inductively coupled plasma quadrupole mass spectrometer.

PubMed

Favre, Georges; Brennetot, René; Chartier, Frédéric; Tortajada, Jeanine

2009-02-01

Inductively coupled plasma mass spectrometry (ICP-MS) is widely used in inorganic analytical chemistry for element and/or isotope ratio measurements. The presence of interferences, which is one of the main limitations of this method, has been addressed in recent years with the introduction of collision/reaction cell devices on ICP-MS apparatus. The study of ion-molecule reactions in the gas phase then became of great importance for the development of new analytical strategies. Knowing the kinetic energy and the electronic states of the ions prior to their entrance into the cell, i.e., just before they react, thereby constitutes crucial information for the interpretation of the observed reactivities. Such studies on an ICP-MS commonly used for routine analyses require the determination of the influence of different instrumental parameters on the energy of the ions and on the plasma temperature from where ions are sampled. The kinetic energy of ions prior to their entrance into the cell has been connected to the voltage applied to the hexapole according to a linear relationship determined from measurements of ion energy losses due to collisions with neutral gas molecules. The effects of the plasma forward power, sampling depth, and the addition of a torch shield to the ICP source were then examined. A decrease of the plasma potential due to the torch shielding, already mentioned in the literature, has been quantified in this study at about 3 V.

Enantioselective determination of the organochlorine pesticide bromocyclen in spiked fish tissue using solid-phase microextraction coupled to gas chromatography with ECD and ICP-MS detection.

PubMed

Fidalgo-Used, Natalia; Montes-Bayón, Maria; Blanco-González, Elisa; Sanz-Medel, Alfredo

2008-05-15

A method for enantioselective determination of bromocyclen enantiomers in fish tissue has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (CP-Chirasil-Dex CB) and a temperature program from 50 degrees C (held for 1 min), raised to 140 degrees C at 40 degrees C min(-1) and then raised at 0.2 degrees C min(-1) to 155 degrees C. This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on solid-phase microextraction (SPME). Under SPME optimized conditions, precision, linearity range and detection limits of the developed SPME-enantioselective GC procedure were evaluated and compared using two different detection systems: a classical electron-capture detection (ECD) and an element specific detection using inductively coupled plasma mass spectrometry (ICP-MS). The SPME-GC-ECD method exhibited an excellent sensitivity, with detection limits of 0.2 ng L(-1) for each enantiomer of bromocyclen. Although ICP-MS offered poorer detection limits (7 ng L(-1) as Br, equivalent to 36 ng L(-1) of each enantiomer) than conventional ECD detector, it proved to be clearly superior in terms of selectivity. The relative potential and performance of the two compared methods for real-life analysis has been illustrated by the determination of enantiomers of bromocyclen in spiked tissue extracts of trout.

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

PubMed

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 (<7.0 μg L -1 ) confirms the official statement that leaded gasoline is no longer used in Cuba.

Isotope ratios of trace elements in samples from human nutrition studies determined by TIMS and ICP-MS: precision and accuracy compared.

PubMed

Turnlund, Judith R; Keyes, William R

2002-09-01

Stable isotopes are used with increasing frequency to trace the metabolic fate of minerals in human nutrition studies. The precision of the analytical methods used must be sufficient to permit reliable measurement of low enrichments and the accuracy should permit comparisons between studies. Two methods most frequently used today are thermal ionization mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICP-MS). This study was conducted to compare the two methods. Multiple natural samples of copper, zinc, molybdenum, and magnesium were analyzed by both methods to compare their internal and external precision. Samples with a range of isotopic enrichments that were collected from human studies or prepared from standards were analyzed to compare their accuracy. TIMS was more precise and accurate than ICP-MS. However, the cost, ease, and speed of analysis were better for ICP-MS. Therefore, for most purposes, ICP-MS is the method of choice, but when the highest degrees of precision and accuracy are required and when enrichments are very low, TIMS is the method of choice.

Comparative analysis of barium titanate thin films dry etching using inductively coupled plasmas by different fluorine-based mixture gas

PubMed Central

2014-01-01

In this work, the inductively coupled plasma etching technique was applied to etch the barium titanate thin film. A comparative study of etch characteristics of the barium titanate thin film has been investigated in fluorine-based (CF4/O2, C4F8/O2 and SF6/O2) plasmas. The etch rates were measured using focused ion beam in order to ensure the accuracy of measurement. The surface morphology of etched barium titanate thin film was characterized by atomic force microscope. The chemical state of the etched surfaces was investigated by X-ray photoelectron spectroscopy. According to the experimental result, we monitored that a higher barium titanate thin film etch rate was achieved with SF6/O2 due to minimum amount of necessary ion energy and its higher volatility of etching byproducts as compared with CF4/O2 and C4F8/O2. Low-volatile C-F compound etching byproducts from C4F8/O2 were observed on the etched surface and resulted in the reduction of etch rate. As a result, the barium titanate films can be effectively etched by the plasma with the composition of SF6/O2, which has an etch rate of over than 46.7 nm/min at RF power/inductively coupled plasma (ICP) power of 150/1,000 W under gas pressure of 7.5 mTorr with a better surface morphology. PMID:25278821

[The matrix effects of organic acid compounds in ICP-MS].

PubMed

Nie, Xi-Du; He, Xiao-Mei; Li, Li-Bo; Xie, Hua-Lin

2007-07-01

The matrix effects arising from oxalic acid, lactic acid, tartaric acid and citric acid in inductively coupled plasma mass spectrometry (ICP-MS) were investigated. It has been proved that the sensitivity of analytes can be significantly enhanced by adding small amounts of organic acid compounds with adjusted nebulizer gas flow-rate, especially for the elements with ionization potential between 9 and 11 eV. The tartaric acid has higher enhancement effect on the signal intensity of the hard-to-ionize elements than oxalic acid, lactic acid and citric acid. The mechanism of the enhancement was investigated. The method has been used to determine Be, Zn, As, Se, Sb and Hg in water standard reference materials (SRM). The analytical results are very close to the certified values.

Microwave-assisted Extraction of Rare Earth Elements from Petroleum Refining Catalysts and Ambient Fine Aerosols Prior to Inductively Coupled Plasma - Mass Spectrometry

NASA Technical Reports Server (NTRS)

Mittlefehldt, David W.; Kulkarni, Pranav; Chellam, Shankar

2006-01-01

In the absence of a certified reference material, a robust microwave-assisted acid digestion procedure followed by inductively coupled plasma - mass spectrometry (ICP-MS) was developed to quantify rare earth elements (REEs) in fluidized-bed catalytic cracking (FCC) catalysts and atmospheric fine particulate matter (PM2.5). High temperature (200 C), high pressure (200 psig), acid digestion (HNO3, HF, and H3BO3) with 20 minute dwell time effectively solubilized REEs from six fresh catalysts, a spent catalyst, and PM2.5. This method was also employed to measure 27 non-REEs including Na, Mg, Al, Si, K, Sc, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Se, Rb, Sr, Zr, Mo, Cd, Cs, Ba, Pb, and U. Complete extraction of several REEs (Y, La, Ce, Pr, Nd, Tb, Dy, and Er) required HF indicating that they were closely associated with the aluminosilicate structure of the zeolite FCC catalysts. Internal standardization using 115In quantitatively corrected non-spectral interferences in the catalyst digestate matrix. Inter-laboratory comparison using ICP-optical emission spectroscopy (ICP-OES) and instrumental neutron activation analysis (INAA) demonstrated the applicability of the newly developed analytical method for accurate analysis of REEs in FCC catalysts. The method developed for FCC catalysts was also successfully implemented to measure trace to ultra-trace concentrations of La, Ce, Pr, Nd, Sm, Gd, Eu, and Dy in ambient PM2.5 in an industrial area of Houston, TX.

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

PubMed

Boulyga, S F; Becker, J S

2001-07-01

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

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

PubMed

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

2014-08-11

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

Chemical vapor generation sample introduction for the determination of As, Cd, Sb, Hg, and Pb in nail polish by inductively coupled plasma mass spectrometry

NASA Astrophysics Data System (ADS)

Huang, Fan-Feng; Jiang, Shiuh-Jen; Chen, Yen-Ling; Sahayam, A. C.

2018-02-01

This paper describes a flow injection vapor generation (VG) method using inductively coupled plasma mass spectrometry (ICP-MS) for determining As, Cd, Sb, Hg, and Pb in nail polish. The samples for VG were prepared as aqueous slurries of a nail polish (0.5% m/v), thiourea (1% m/v), Co(II) (0.75 μg mL- 1), and HCl (1.2% v/v). Chemical VG of As, Cd, Sb, Hg, and Pb ions, by reduction with tetrahydroborate (3% m/v in 0.2% m/v NaOH), enabled their separation from the slurry. With VG sample introduction, As, Cd, Sb and Hg signals were increased by 1-2 orders (except Pb) compared to solution nebulization due to better sample introduction. Quantifications were performed by VG ICP-MS using isotope dilution and standard addition methods as slopes of calibration plots of analytes in the slurries were higher. Using the reported procedure, samples of three nail polishes purchased locally were analyzed for their levels of As, Cd, Sb, Hg, and Pb. The results obtained were in good agreement with those measured using electrothermal vaporization ICP-MS. In the original nail polish sample, the detection limits, calculated as 3σ of blank measurements, for As, Cd, Sb, Hg, and Pb, estimated from standard addition curves, were 0.06, 0.12, 0.14, 0.2, and 12 ng g- 1, respectively.

Addition of Si-Containing Gases for Anisotropic Etching of III-V Materials in Chlorine-Based Inductively Coupled Plasma

NASA Astrophysics Data System (ADS)

Gatilova, Lina; Bouchoule, Sophie; Patriarche, Gilles; Guilet, Stephane

2011-08-01

We discuss the possibility of obtaining high-aspect-ratio etching of InP materials in Cl2- and HBr-based inductively coupled plasmas (ICP) with the addition of Si-containing gases (SiH4 or SiCl4). A vertical and smooth etching profile is demonstrated in SiCl4/H2 plasma. The effect of adding of a small amount of SiH4 to a previously optimised Cl2/H2 chemistry is presented, and new SiH4/Cl2 and SiH4/HBr chemistries are proposed. Ex-situ energy-dispersive X-ray spectroscopy coupled to transmission electron microscopy (EDX-TEM) is used to analyze the composition of the thin passivation layer deposited on the etched sidewalls. We show that it consists of a Si-rich silicon oxide (Si/O˜1) in Cl2/H2/SiH4 chemistry, and is changed to nano-crystalline (nc-) Si in SiH4/Cl2 chemistry depending on the SiH4 percentage. Moreover, we show that deep anisotropic etching of InP independent of the electrode coverplate material can be obtained via a SiOx passivation mechanism with the addition of Si-containing gases.

An interlaboratory comparison of bone lead measurements via K-shell X-ray fluorescence spectrometry: validation against inductively coupled plasma mass spectrometry

PubMed Central

Bellis, David J.; Todd, Andrew C.

2012-01-01

109Cd-based K-shell X-ray fluorescence spectrometry (hereafter, for brevity, XRF) is used, often in epidemiological studies, to perform non-invasive, in vivo measurements of lead in bone. We conducted the first interlaboratory study of XRF via the circulation of nine goat tibiæ in which the mean lead value ranged from 4.0 µg g−1 to 55.3 µg g−1 bone mineral. The test tibiæ were subsequently analyzed via nitric acid digestion followed by lead determination by inductively coupled plasma mass spectrometry (ICP-MS) – along with certified reference materials for bone lead – thus providing measurement traceability to SI units. Analysis of dried bone for lead via nitric acid digestion and ICP-MS yields mass fraction data in units of µg g−1 dry weight. The mean bone lead value based on ICP-MS analysis ranged from 1.8 µg g−1 to 35.8 µg g−1 dry weight. For comparison purposes, XRF-measured Pb values (µg g−1 bone mineral) were converted into the ICP-MS-measured units (µg g−1dry weight bone) by multiplying the former by the average ash fraction from the nine tibiæ. Eight of the XRF systems did not yield a significant bias for any of the nine tibiæ; one system was biased for one of the tibiæ; two systems were biased for two tibiæ; one system was biased for four tibiæ; two systems (813-1 and 804-2) were biased for five tibiæ and one system (801-1) was biased for six of the nine tibiæ. Average bias for the systems (under those particular operating conditions) that were biased for the majority of samples ranged from −2.6 µg g−1 (−15.7%) to 5.1 µg g−1 (30.7%) dry weight bone. All participants now have the ICP-MS data, allowing any corrective actions deemed necessary to be implemented. The ICP-MS data, however, indicated that the lead mass fraction varied considerably with the sampling location within the tibiæ, to the extent of exceeding XRF variability for the higher lead values. Material heterogeneity is an unavoidable reality of

Quantification of immobilized Candida antarctica lipase B (CALB) using ICP-AES combined with Bradford method.

PubMed

Nicolás, Paula; Lassalle, Verónica L; Ferreira, María L

2017-02-01

The aim of this manuscript was to study the application of a new method of protein quantification in Candida antarctica lipase B commercial solutions. Error sources associated to the traditional Bradford technique were demonstrated. Eight biocatalysts based on C. antarctica lipase B (CALB) immobilized onto magnetite nanoparticles were used. Magnetite nanoparticles were coated with chitosan (CHIT) and modified with glutaraldehyde (GLUT) and aminopropyltriethoxysilane (APTS). Later, CALB was adsorbed on the modified support. The proposed novel protein quantification method included the determination of sulfur (from protein in CALB solution) by means of Atomic Emission by Inductive Coupling Plasma (AE-ICP). Four different protocols were applied combining AE-ICP and classical Bradford assays, besides Carbon, Hydrogen and Nitrogen (CHN) analysis. The calculated error in protein content using the "classic" Bradford method with bovine serum albumin as standard ranged from 400 to 1200% when protein in CALB solution was quantified. These errors were calculated considering as "true protein content values" the results of the amount of immobilized protein obtained with the improved method. The optimum quantification procedure involved the combination of Bradford method, ICP and CHN analysis. Copyright © 2016 Elsevier Inc. All rights reserved.

NHEXAS PHASE I ARIZONA STUDY--STANDARD OPERATING PROCEDURE FOR EXTRACTION OF METALS FROM SOIL, DUST, AIR FILTER, AND SURFACE AND DERMAL SAMPLES FOR AA (GRAPHITE FURNACE OR FLAME) OR ICP-AES ANALYSIS (BCO-L-3.1)

EPA Science Inventory

The purpose of this SOP is to describe the acid digestion of soil, house dust, air filter, and surface or dermal wipe samples for analysis using inductively coupled plasma atomic emissions spectrometry (ICP-AES) and/or graphite furnace atomic absorption spectrometry (GFAAS) or fl...

The performance of single and multi-collector ICP-MS instruments for fast and reliable 34S/32S isotope ratio measurements†

PubMed Central

Pröfrock, Daniel; Irrgeher, Johanna; Prohaska, Thomas

2016-01-01

The performance and validation characteristics of different single collector inductively coupled plasma mass spectrometers based on different technical principles (ICP-SFMS, ICP-QMS in reaction and collision modes, and ICP-MS/MS) were evaluated in comparison to the performance of MC ICP-MS for fast and reliable S isotope ratio measurements. The validation included the determination of LOD, BEC, measurement repeatability, within-lab reproducibility and deviation from certified values as well as a study on instrumental isotopic fractionation (IIF) and the calculation of the combined standard measurement uncertainty. Different approaches of correction for IIF applying external intra-elemental IIF correction (aka standard-sample bracketing) using certified S reference materials and internal inter-elemental IIF (aka internal standardization) correction using Si isotope ratios in MC ICP-MS are explained and compared. The resulting combined standard uncertainties of examined ICP-QMS systems were not better than 0.3–0.5% (uc,rel), which is in general insufficient to differentiate natural S isotope variations. Although the performance of the single collector ICP-SFMS is better (single measurement uc,rel = 0.08%), the measurement reproducibility (>0.2%) is the major limit of this system and leaves room for improvement. MC ICP-MS operated in the edge mass resolution mode, applying bracketing for correction of IIF, provided isotope ratio values with the highest quality (relative combined measurement uncertainty: 0.02%; deviation from the certified value: <0.002%). PMID:27812369

The performance of single and multi-collector ICP-MS instruments for fast and reliable 34S/32S isotope ratio measurements.

PubMed

Hanousek, Ondrej; Brunner, Marion; Pröfrock, Daniel; Irrgeher, Johanna; Prohaska, Thomas

2016-11-14

The performance and validation characteristics of different single collector inductively coupled plasma mass spectrometers based on different technical principles (ICP-SFMS, ICP-QMS in reaction and collision modes, and ICP-MS/MS) were evaluated in comparison to the performance of MC ICP-MS for fast and reliable S isotope ratio measurements. The validation included the determination of LOD, BEC, measurement repeatability, within-lab reproducibility and deviation from certified values as well as a study on instrumental isotopic fractionation (IIF) and the calculation of the combined standard measurement uncertainty. Different approaches of correction for IIF applying external intra-elemental IIF correction (aka standard-sample bracketing) using certified S reference materials and internal inter-elemental IIF (aka internal standardization) correction using Si isotope ratios in MC ICP-MS are explained and compared. The resulting combined standard uncertainties of examined ICP-QMS systems were not better than 0.3-0.5% ( u c,rel ), which is in general insufficient to differentiate natural S isotope variations. Although the performance of the single collector ICP-SFMS is better (single measurement u c,rel = 0.08%), the measurement reproducibility (>0.2%) is the major limit of this system and leaves room for improvement. MC ICP-MS operated in the edge mass resolution mode, applying bracketing for correction of IIF, provided isotope ratio values with the highest quality (relative combined measurement uncertainty: 0.02%; deviation from the certified value: <0.002%).

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

NASA Astrophysics Data System (ADS)

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

2014-06-01

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

Isotope-ratio measurements of lead in NIST standard reference materials by multiple-collector inductively coupled plasma mass spectrometry.

PubMed

Platzner, I; Ehrlich, S; Halicz, L

2001-07-01

The capability of a second-generation Nu Instruments multiple collector inductively coupled plasma mass spectrometer (MC-ICP-MS) has been evaluated for precise and accurate isotope-ratio determinations of lead. Essentially the mass spectrometer is a double-focusing instrument of Nier-Johnson analyzer geometry equipped with a newly designed variable-dispersion ion optical device, enabling the measured ion beams to be focused into a fixed array of Faraday collectors and an ion-counting assembly. NIST SRM Pb 981, 982, and 983 isotopic standards were used. Addition of thallium to the lead standards and subsequent simultaneous measurement of the thallium and lead isotopes enabled correction for mass discrimination, by use of the exponential correction law and 205Tl/203Tl = 2.3875. Six measurements of SRM Pb-982 furnished the results 206Pb/204Pb = 36.7326(68), 207Pb/204Pb = 17.1543(30), 208Pb/204Pb = 36.7249(69), 207Pb/206Pb = 0.46700(1), and 208Pb/206Pb = 0.99979(2); the NIST-certified values were 36.738(37), 17.159(25), 36.744(50), 0.46707(20), and 1.00016(36), respectively. Direct isotope lead analysis in silicates can be performed without any chemical separation. NIST SRM 610 glass was dissolved and introduced into the MC-ICP-MS by means of a micro concentric nebulizer. The ratios observed were in excellent agreement with previously reported data obtained by TIMS and laser ablation MC-ICP-MS, despite the high Ca/Pb concentration ratio (200/1) and the presence of many other elements at levels comparable with that of lead. Approximately 0.2 microg lead are sufficient for isotope analysis with ratio uncertainties between 240 and 530 ppm.

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

NASA Astrophysics Data System (ADS)

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

2004-12-01

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

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

PubMed

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.

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

PubMed Central

Gulson, Brian; Manton, William; Rabinowitz, Michael

2018-01-01

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. PMID:29641487

High precision isotope ratio measurements of mercury isotopes in cinnabar ores using multi-collector inductively coupled plasma mass spectrometry.

PubMed

Hintelmann, Holger; Lu, ShengYong

2003-06-01

Variations in Hg isotope ratios in cinnabar ores obtained from different countries were detected by high precision isotope ratio measurements using multi-collector inductively coupled mass spectrometry (MC-ICP-MS). Values of delta198/202Hg varied from 0.0-1.3 percent per thousand relative to a NIST SRM 1641d Hg solution. The typical external uncertainty of the delta values was 0.06 to 0.26 percent per thousand. Hg was introduced into the plasma as elemental Hg after reduction by sodium borohydride. A significant fractionation of lead isotopes was observed during the simultaneous generation of lead hydride, preventing normalization of the Hg isotope ratios using the measured 208/206Pb ratio. Hg ratios were instead corrected employing the simultaneously measured 205/203T1 ratio. Using a 10 ng ml(-1) Hg solution and 10 min of sampling, introducing 60 ng of Hg, the internal precision of the isotope ratio measurements was as low as 14 ppm. Absolute Hg ratios deviated from the representative IUPAC values by approximately 0.2% per u. This observation is explained by the inadequacy of the exponential law to correct for mass bias in MC-ICP-MS measurements. In the absence of a precisely characterized Hg isotope ratio standard, we were not able to determine unambiguously the absolute Hg ratios of the ore samples, highlighting the urgent need for certified standard materials.

Simultaneous in situ determination of both U-Th-Pb and Sm-Nd isotopes in monazite by laser ablation using a magnetic sector ICP-MS and a multicollector ICP-MS

NASA Astrophysics Data System (ADS)

Goudie, D. J.; Fisher, C. M.; Hanchar, J. M.; Davis, W. J.; Crowley, J. L.; Ayers, J. C.

2012-12-01

We present a method for the simultaneous in situ determination of U-Th-Pb and Sm-Nd isotopes in monazite, using a laser ablation (LA) system coupled to both a magnetic sector inductively coupled plasma mass spectrometer (HR) ICP-MS and a multicollector (MC) ICP-MS. The ablated material is split using a glass Y-connector and transported simultaneously to both mass spectrometers via helium carrier gas. The MC-ICP-MS is configured to provide relative Ce, Gd, and Eu contents, in addition to Sm and Nd. This approach obtains both age (U-Pb), tracer isotope (Sm-Nd), and REE element data (Ce, Gd, and Eu), in the same ablation volume, thus reducing sampling problems associated with fine-scale zoning and other internal structures. The accuracy and precision of the U-Pb data are demonstrated using six well characterized monazite reference materials from the Geological Survey of Canada (three of which are currently used as SHRIMP standards) and agree well with previously determined ID-TIMS ages. The accuracy of the Sm-Nd isotopic data was assessed by comparison to TIMS measurements on a well-characterized in-house monazite standard. The dual LA-ICP-MS method was applied to the Birch Creek Pluton (BCP) in the White Mountains, California in a case study to test the utility of U-Th-Pb dating coupled with Sm-Nd (and Ce, Gd, Eu) isotopic data for solving geologic problems. Previous work on the Cretaceous BCP [1] used Th-Pb ages coupled with O isotopic data to constrain hydrothermal fluid events, as recorded in monazite. The original study suggested that the high delta 18O monazite in Paleozoic country rocks adjacent to the BCP grew in response to fluid alternation associated with the intrusion of the BCP, based on overlapping age with the BCP. New monazite split-stream U-Pb and Sm-Nd data show that monazite from the BCP pluton and monazite from altered country rock have homogenous and overlapping initial Nd isotopic composition, further strengthening the proposal that monazite in

Electrothermal vaporization of mineral acid solutions in inductively coupled plasma mass spectrometry: comparison with sample nebulization

NASA Astrophysics Data System (ADS)

Mora, Juan; Gras, Luis; van Veen, Eric H.; de Loos-Vollebregt, Margaretha T. C.

1999-06-01

The analytical behaviour of an electrothermal vaporization (ETV) device for the introduction of mineral acid solutions in inductively coupled plasma mass spectrometry (ICP-MS) was evaluated. Water, nitric acid, hydrochloric acid, perchloric acid and sulphuric acid in concentrations within the 0.05-1.0 mol l-1 range were studied. For all the acids tested, increasing the acid concentration increases the ion signal and deteriorates the precision. The magnitude of the signal enhancement depends on the analyte and on the acid considered. Acid solutions give rise to ion signals that are between 2 and 10 times higher than those with water. Among the acids tested, sulphuric acid provides the highest signals. The addition of palladium reduces matrix effects due to the acids and increases the signal in ETV ICP-MS. In comparison with conventional sample nebulization (CS), the ETV sample introduction system provides higher sensitivities (between 2 and 20 times higher) at the same acid concentration. The magnitude of this improvement is similar to that obtained with a microwave desolvation system (MWDS). The ETV sample introduction system gives rise to the lowest background signals from matrix-induced species. Due to this fact, the limits of detection (LODs) obtained for the isotopes affected by any interference are lower for ETV sample introduction than those obtained with the CS and the MWDS. For the isotopes that do not suffer from matrix-induced spectral interferences, the ETV gives rise to LODs higher than those obtained with the CS. For these isotopes the lowest LODs are obtained with MWDS.

Collisionless electron heating in inductively coupled discharges

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shaing, K.C.; Aydemir, A.Y.

1996-07-01

A kinetic theory of collisionless electron heating is developed for inductively coupled discharges with a finite height L. The novel effect associated with the finite-length system is the resonance between the bounce motion of the electrons and the wave frequency, leading to enhanced heating. The theory is in agreement with results of particle simulations.

MRI surface-coil pair with strong inductive coupling.

PubMed

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

2016-12-01

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

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

NASA Astrophysics Data System (ADS)

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

2018-05-01

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

Determination of Os by isotope dilution-inductively coupled plasma-mass spectrometry with the combination of laser ablation to introduce chemically separated geological samples

NASA Astrophysics Data System (ADS)

Sun, Yali; Ren, Minghao; Xia, Xiaoping; Li, Congying; Sun, Weidong

2015-11-01

A method was developed for the determination of trace Os in geological samples by laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) with the combination of chemical separation and preconcentration. Samples are digested using aqua regia in Carius tubes, and the Os analyte is converted into volatile OsO4, which is distilled and absorbed with HBr. The HBr solution is concentrated for further Os purification using the microdistillation technique. The purified Os is dissolved in 10 μl of 0.02% sucrose-0.005% H3PO4 solution and then evaporated on pieces of perfluoroalkoxy (PFA) film, resulting in the formation of a tiny object (< 3 × 104 μm2 superficial area). Using LA-ICP-MS measurements, the object can give Os signals at least 100 times higher than those provided by routine solution-ICP-MS while successfully avoiding the memory effect. The procedural blank and detection limit in the developed technique are 3.0 pg and 1.8 pg for Os, respectively when 1 g of samples is taken. Reference materials (RM) are analyzed, and their Os concentrations obtained by isotope dilution are comparable to reference or literature values. Based on the individual RM results, the precision is estimated within the range of 0.6 to 9.4% relative standard deviation (RSD), revealing that this method is applicable to the determination of trace Os in geological samples.

Ultrasound-assisted enzymatic hydrolysis for iodinated amino acid extraction from edible seaweed before reversed-phase high performance liquid chromatography-inductively coupled plasma-mass spectrometry.

PubMed

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

2013-09-27

The combination of reverse phase high performance liquid chromatography (RP-HPLC) with inductively coupled plasma mass spectrometry (ICP-MS) was used for the determination of monoiodotyrosine (MIT) and diiodotyrosine (DIT) in edible seaweed. A sample pre-treatment based on ultrasound assisted enzymatic hydrolysis was optimized for the extraction of these iodinated amino acids. Pancreatin was selected as the most adequate type of enzyme, and parameters affecting the extraction efficiency (pH, temperature, mass of enzyme and extraction time) were evaluated by univariate approaches. In addition, extractable inorganic iodine (iodide) was also quantified by anion exchange high performance liquid chromatography (AE-HPLC) coupled with ICP-MS. The proposed procedure offered limits of detection of 1.1 and 4.3ngg(-1) for MIT and DIT, respectively. Total iodine contents in seaweed, as well as total iodine in enzymatic digests were measured by ICP-MS after microwave assisted alkaline digestion with tetramethylamonium hydroxide (TMAH) for total iodine assessment, and also by treating the pancreatin extracts (extractable total iodine assessment). The optimized procedure was successfully applied to five different types of edible seaweed. The highest total iodine content, and also the highest iodide levels, was found in the brown seaweed Kombu (6646±45μgg(-1)). Regarding iodinated amino acids, Nori (a red seaweed) was by far the one with the highest amount of both species (42±3 and 0.41±0.024μgg(-1) for MIT and DIT, respectively). In general, MIT concentrations were much higher than the amounts of DIT, which suggests that iodine from iodinated proteins in seaweed is most likely bound in the form of MIT residues. Copyright © 2013 Elsevier B.V. All rights reserved.

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

PubMed

Arslan, Zikri; Oymak, Tulay; White, Jeremy

2018-05-30

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

Measurement of plutonium isotope ratios in nuclear fuel samples by HPLC-MC-ICP-MS

NASA Astrophysics Data System (ADS)

Günther-Leopold, I.; Waldis, J. Kobler; Wernli, B.; Kopajtic, Z.

2005-04-01

Radioactive isotopes are traditionally quantified by means of radioactivity counting techniques ([alpha], [beta], [gamma]). However, these methods often require extensive matrix separation and sample purification before the identification of specific isotopes and their relative abundance is possible as it is necessary in the frame of post-irradiation examinations on nuclear fuel samples. The technique of multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) is attracting much attention because it permits the precise measurement of the isotope compositions for a wide range of elements combined with excellent limits of detection due to high ionization efficiencies. The present paper describes one of the first applications of an online high-performance liquid chromatographic separation system coupled to a MC-ICP-MS in order to overcome isobaric interferences for the determination of the plutonium isotope composition and concentrations in irradiated nuclear fuels. The described chromatographic separation is sufficient to prevent any isobaric interference between 238Pu present at trace concentrations and 238U present as the main component of the fuel samples. The external reproducibility of the uncorrected plutonium isotope ratios was determined to be between 0.04 and 0.2% (2 s) resulting in a precision in the [per mille sign] range for the isotopic vectors of the irradiated fuel samples.

Reference measurements for total mercury and methyl mercury content in marine biota samples using direct or species-specific isotope dilution inductively coupled plasma mass spectrometry.

PubMed

Krata, Agnieszka; Vassileva, Emilia; Bulska, Ewa

2016-11-01

The analytical procedures for reference measurements of the total Hg and methyl mercury (MeHg) mass fractions at various concentration levels in marine biota samples, candidates for certified reference materials (oyster and clam Gafrarium tumidum), were evaluated. Two modes of application of isotope dilution inductively coupled plasma mass spectrometry method (ID ICP-MS), namely direct isotope dilution and species-specific isotope dilution analysis with the use of two different quantification mass spectrometry techniques were compared. The entire ID ICP-MS measurement procedure was described by mathematical modelling and the combined uncertainty of measurement results was estimated. All factors influencing the final results as well as isotopic equilibrium were systematically investigated. This included the procedural blank, the moisture content in the biota samples and all factors affecting the blend ratio measurements (instrumental background, spectral interferences, dead time and mass discrimination effects as well as the repeatability of measured isotopic ratios). Modelling of the entire measurement procedures and the use of appropriate certified reference materials enable to assure the traceability of obtained values to the International System of Units (SI): the mole or the kilogram. The total mass fraction of mercury in oyster and clam biota samples, after correction for moisture contents, was found to be: 21.1 (1.1) 10(-9) kg kg(-1) (U =5.1% relative, k=2) and 390.0 (9.4) 10(-9) kg kg(-1) (U=2.4% relative, k=2), respectively. For the determination of mercury being present as methyl mercury, the non-chromatographic separation on anion-exchange resin AG1-X8 of the blended samples was applied. The content of MeHg (as Hg) in oyster sample was found: 4.81 (24) 10(-9)kgkg(-1) (U=5.0%, k=2) and 4.84 (21) 10(-9)kgkg(-1) (U=4.3%, k=2) with the use of quadrupole (ICP QMS) or sector field (ICP SFMS) inductively coupled plasma mass spectrometers, respectively. In the

Microfluidic high performance liquid chromatography-chip hyphenation to inductively coupled plasma-mass spectrometry.

PubMed

Bishop, David P; Blanes, Lucas; Wilson, Alexander B; Wilbanks, Thor; Killeen, Kevin; Grimm, Rudolf; Wenzel, Ross; Major, Derek; Macka, Mirek; Clarke, David; Schmid, Robin; Cole, Nerida; Doble, Philip A

2017-05-12

The Agilent Chip Cube Interface is a microfluidic chip-based technology originally designed for nanospray molecular mass spectrometry in which the sample enrichment, nano-column, tubing, connectors and spray tip were integrated into a single biocompatible chip. Here we describe the hyphenation of the Chip Cube Interface to ICP-MS via modification of the standard HPLC chip design and a new total consumption nebuliser suitable for flow rates as low as 300nLmin -1 . The potential of the instrument to eliminate common nanoLC - ICP-MS shortcomings such as leaks, blockages and band-broadening was demonstrated via analysis of cyanocobalamin in equine plasma. The method was linear over three orders of magnitude with an r 2 of 0.9999, the peak area repeatability was 1.9% (n=7), and the detection limit was 14ngmL -1 . This novel configuration of the Chip Cube Interface coupled to ICP-MS is a suitable platform for the analysis of biomolecules associated with trace metals and speciation applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Documenting utility of paddlefish otoliths for quantification of metals using inductively coupled plasma mass spectrometry

USGS Publications Warehouse

Long, James M.; Schaffler, James J.

2013-01-01

RATIONALE The otoliths of the inner ear of fishes record the environment of their surrounding water throughout their life. For paddlefish (Polyodon spathula), otoliths have not been routinely used by scientists since their detriments were outlined in the early 1940s. We sought to determine if paddlefish otoliths were useful for resolving elemental information contained within. METHODS Adult paddlefish were collected from two wild, self-sustaining populations in Oklahoma reservoirs in the Arkansas River basin. Juveniles were obtained from a hatchery in the Red River basin of Oklahoma. Otoliths were removed and laser ablation, inductively coupled plasma mass spectrometry (ICP-MS) was used to quantify eight elements (Li, Mg, Mn, Rb, Sr, Y, Ba, and Pb) along the core and edge portions, which were analyzed for differences between otolith regions and among paddlefish sources. RESULTS Differences were found among samples for six of the eight elements examined. Otoliths from Red River basin paddlefish born in a hatchery had significantly lower amounts of Mg and Mn, but higher levels of Rb than otoliths from wild paddlefish in the Arkansas River basin. Concentrations of Y, Sr, and Ba were reduced on the edges of adult paddlefish from both reservoirs compared with the cores. CONCLUSIONS This research shows the utility of using an ICP-MS analysis of paddlefish otoliths. Future research that seeks to determine sources of paddlefish production, such as which reservoir tributaries are most important for reproduction or what proportion of the population is composed of wild versus hatchery-produced individuals, appears promising. Published in 2013. This article is a U.S. Government work and is in the public domain in the USA.

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

PubMed

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.

Determination of As, Cd, Hg and Pb in herbs using slurry sampling electrothermal vaporisation inductively coupled plasma mass spectrometry.

PubMed

Lin, Mei-Ling; Jiang, Shiuh-Jen

2013-12-01

Inductively coupled plasma mass spectrometry coupled with ultrasonic slurry sampling electrothermal vaporisation (USS-ETV-ICP-MS) has been applied to determine As, Cd, Hg and Pb in 0.5% m/v slurries of several herb samples. 1% m/v 8-Hydroxyquinoline was used as the modifier to enhance the ion signals. The influences of instrument operating conditions, slurry preparation and interferences on the ion signals were reported. This method has been applied to the determination of As, Cd, Hg and Pb in NIST SRM 1547 peach leaves and SRM 1573a tomato leaves reference materials and three herb samples purchased from the local market and ground to 150 μm. The analysis results of the standard reference materials agreed with the certified values which are at sub μg g(-1) levels. Precision between sample replicates was better than 4% for all the determinations. The method detection limits estimated from standard addition curves were about 0.3, 0.1, 0.1 and 0.2 ng g(-1) for As, Cd, Hg and Pb, respectively, in original herb samples. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

PubMed

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.

Vaporization and atomization of uranium in a graphite tube electrothermal vaporizer: a mechanistic study using electrothermal vaporization inductively coupled plasma mass spectrometry and graphite furnace atomic absorption spectrometry

NASA Astrophysics Data System (ADS)

Goltz, D. M.; Grégoire, D. C.; Byrne, J. P.; Chakrabarti, C. L.

1995-07-01

The mechanism of vaporization and atomization of U in a graphite tube electrothermal vaporizer was studied using graphite furnace atomic absorption spectrometry (GFAAS) and electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS). Graphite furnace AAS studies indicate U atoms are formed at temperatures above 2400°C. Using ETV-ICP-MS, an appearance temperature of 1100°C was obtained indicating that some U vaporizes as U oxide. Although U carbides form at temperatures above 2000°C, ETV-ICP-MS studies show that they do not vaporize until 2600°C. In the temperature range between 2200°C and 2600°C, U atoms in GFAAS are likely formed by thermal dissociation of U oxide, whereas at higher temperatures, U atoms are formed via thermal dissociation of U carbide. The origin of U signal suppression in ETV-ICP-MS by NaCl was also investigated. At temperatures above 2000°C, signal suppression may be caused by the accelerated rate of formation of carbide species while at temperatures below 2000°C, the presence of NaCl may cause intercalation of the U in the graphite layers resulting in partial retention of U during the vaporization step. The use of 0.3% freon-23 (CHF 3) mixed with the argon carrier gas was effective in preventing the intercalation of U in graphite and U carbide formation at 2700°C.